JP2000274598A - Improved multipurpose production device and multipurpose production method using thereof - Google Patents

Abstract

PROBLEM TO BE SOLVED: To produce the same product with high efficiency and perform a small not multi-variety production with high efficiency by use of the same device by connecting the outlet piping from the bottom of the tower tank of a tower tank group and the inlet piping from the tower top part of the tower tank group to a piping automatic connection device, and connecting the outlet piping of the piping automatic connection device. SOLUTION: A piping group Lx and a piping are connected to the inlet and outlet of an L:1 piping automatic connection device 1. Pipings are connected to the inlet and outlet of an M:K piping automatic connection device 2. The outlet piping of the L:1 piping automatic connection device is connected to the inlet piping of the M:K piping automatic connection device 2 through a piping 10. The liquid supplied form the piping group Lx to the L:1 piping automatic connection device 1 is supplied to the inlet piping of the M:K piping automatic connection device 2 through the piping 10, and supplied to the tower top of an optional tower of tower tanks A-D from the outlet piping of the M:K piping automatic connection device 2. According to this, a small lot multi-variety production can be placed, and a production plan for performing the same lot production in the shortest time can be formed.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an improved multipurpose production apparatus and a multipurpose production method using the same.

[0002]

2. Description of the Related Art In the field of manufacturing pharmaceuticals, fine chemicals, etc. (hereinafter referred to as "pharmaceuticals, etc."), when producing intermediates such as pharmaceuticals or drug substances in a batch system, a dedicated reaction tank fixed for each brand to be manufactured. , An extraction tank, a distillation tower, a crystallization tank, and the like, and fixed piping for it. In such a batch-type production system, the transfer of fluids such as raw materials and products has been mainly performed by a valve switching operation using fixed piping. However, as the number of reactors and the like increased, the number of valves also increased, and the control system had to be complicated.

[0003] In addition, when it becomes necessary to switch types due to an increase in brands, the existing manufacturing equipment is remodeled to provide a pipe for it, a control system is examined, and mixing of different types of fluids is prevented. And so on.

Against this background, the applicant has previously disclosed in Japanese Patent Publication No. 8-12000 a combination of a plurality of hose groups used in a batch-type production system instead of fixed pipes, and A flexible automatic connection device at a ho station for transferring intermediate products and the like and a management system thereof have been proposed. In this publication, the connection device includes a unit in which a plurality of cells are vertically arranged in a line, a unit in which a plurality of cells are arranged in a line, and a moving body that moves in the cell. Two hose groups, one end of each hose connected to a board and the other end connected to a connection joint in the moving body so that the hoses do not get caught, and the moving body provided in both units is moved in the cell. And a device for moving both units or joints to connect the ends of the hoses and releasing the connection after the fluid transfer operation is completed.

Further, in Japanese Patent Publication No. Hei 8-25600, a switching station pipe automatic connection device which can use a pipe represented by stainless steel or the like in place of the hose disclosed in Japanese Patent Publication No. Hei 8-12000 and A management system was proposed. In the above two proposals, it is natural that the inside of the pipe can be cleaned.

Further, in the above two proposals, there is a possibility that the excess length of a hose or the like may be bent and a liquid pool may be generated in a vertically provided switching station. As means for preventing contamination, Japanese Patent Laid-Open Publication No. 7-71699 has proposed an automatic pipe connection apparatus for a switching station that does not cause the liquid pool. These squid automatic connection devices having M inlet piping connections and K outlet piping connections are collectively referred to as M: K automatic piping connections.

As described above, the present invention is not limited to this, but columns and tanks having different unit operation functions such as a reaction tank, an extraction tank, a distillation column, and crystallization are used according to their functions. When the piping automatic connection device proposed by the applicant is applied to a plant in which the order is determined, by installing a hose or piping switching station instead of fixed piping, complicated piping group is entangled, reduction of manual work, Dangerous work by humans has been drastically reduced, and the incorporation of fluids of different types at the time of switching pipe connections has become possible.

By the way, there has been a demand from the development of the above-mentioned automatic piping connection apparatus that it is desired to use an existing plant or a new plant for multiple purposes. One example of such a demand is so-called multi-product small-quantity production in which different products are simultaneously manufactured using the same plant. As another example, when manufacturing the same product, it is necessary to minimize the downtime of the work of the towers and the like installed in the same plant, so-called full operation, increase the production volume per operation time, or One example is to reduce the operation time required for production.

Although the details of the present invention will be described later, the above-mentioned demands cannot be simultaneously achieved only by the proposals of the applicant and the like.

[0010]

SUMMARY OF THE INVENTION The present invention proposes a multi-purpose production apparatus and a multi-purpose production method using the same apparatus, which enables high-efficiency production of the same product, high-mix low-volume production with the same apparatus. The purpose is to:

[0011]

Means for Solving the Problems In view of the above circumstances, the present inventors have diligently studied means for simultaneously achieving the above demands.
As a result, the number of pipes at the inlet of the fluid for the purpose of supplying the raw material is L and the number of pipes at the outlet is one. An M: K pipe automatic connection device having K outlet pipes, and at least a plurality of N outlet pipes having one fluid inlet pipe and one outlet pipe having the same function. A tower group consisting of batch towers or a group of N batch tanks having a plurality of different functions, or a group of N batch tanks having different functions. An improved multi-purpose device comprising: N pipes at the outlet from the bottom of each of the tower groups and M inlet pipes from the top of the tower group. ： Connect with K automatic pipe connection device,
Further, they have come to the knowledge that this can be achieved by connecting one of the inlet pipes of the M: K automatic pipe connection apparatus to the outlet pipe of the L: 1 automatic pipe connection apparatus. Here, L, K and M are arbitrary integers indicating the number of pipes, N
Is the number of tower tanks, M ≧ N + 1, and K ≧ N.

That is, the present invention provides (1) N batch-type column tanks each having one outlet pipe from the bottom of the tower and one inlet pipe from the top of the tower; Automatic M: K pipe connection device with one inlet pipe and K outlet pipes, and L: 1 pipe automatic connection for raw material supply with L inlet pipes and one outlet pipe And an apparatus for connecting the N outlet pipes of each of the tower tanks of the tower tank group and the N inlet pipes of the tower tank group to an M: K automatic pipe connection device. An improved multi-purpose production apparatus (where L, K and M are:
An arbitrary integer indicating the number of pipes, N is the number of tanks, M ≧ N +
1, K ≧ N), and the present invention also includes (2) a plurality of towers in the tower group having the same function, and (3) a plurality of towers in the tower group. And (4) each of the plurality of towers in the tower group has a single different function. Further, the present invention provides (5) using the multipurpose production apparatus according to any one of the above (1) to (4), wherein one unit reaction is performed in one of the tower tanks,
Includes an improved multi-purpose production method characterized by transferring the contents of the tower tank to another tower tank by switching the M: K automatic pipe connection device and performing another unit operation there.

[0013]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described with reference to FIG. FIG. 1 is a flow sheet showing an embodiment of the present invention, but it goes without saying that the present invention is not limited to this.

A description will be given of an automatic pipe connection apparatus 1 of L: 1 and an automatic pipe connection apparatus 2 of M: K having a plurality of pipes for supplying water, solvent and the like for supplying raw materials and washing.

In the L: 1 automatic pipe connection apparatus 1, a pipe group Lx composed of n pipes is connected to the inlet, and one pipe is connected to the outlet. Here, x = 1 to n, and n is an arbitrary integer of 1 or more. Different fluids are supplied to the group of pipes as described above. In addition,
L is an integer equal to x.

It goes without saying that control can be performed such that different fluids can be supplied to the pipes L1 to Ln of the pipe group at any time in any time.

In the M: K automatic pipe connection device 2, M pipes are connected to the inlet and K pipes are connected to the outlet.

In the automatic pipe connection apparatus 1 of L: 1 and the automatic pipe connection apparatus 2 of M: K, a unit in which a plurality of cells are vertically arranged in a line and a plurality of cells are horizontally arranged in a line. Although the unit has units arranged in a plane, it goes without saying that it is possible to arbitrarily select which unit is used as the inlet pipe or the outlet pipe.

The connection between the L: 1 automatic pipe connection apparatus 1 and the M: K automatic pipe connection apparatus 2 will be described.
The necessary control valves and the like are installed in the pipes L1 to Ln at the inlet of the L: 1 automatic pipe connection device 1, respectively.

The pipe at the outlet of the L: 1 automatic pipe connection apparatus 1 is connected to an M: K automatic pipe connection apparatus 2 by a pipe 10.
It can be connected to the inlet piping. Therefore, the fluid is supplied from the piping group Lx to the automatic piping connection device 1 of L: 1, the fluid is supplied to the inlet piping of the automatic piping connection device 2 of M: K through the piping 10, and the piping of M: K is supplied. It can be supplied from the pipe at the outlet of the automatic connection device to the tower top of any of the tower tanks A to D described in detail later.

Here, M is usually an integer equal to or greater than N + 1. As described above, the outlet pipe of the L: 1 automatic pipe connection apparatus 1 is connected as the inlet pipe of the M: K automatic pipe connection apparatus 2. Therefore, in FIG. 1, N is 4 and M is 5. However, usually, although not shown in this figure, one of the inlet pipes of the M: K automatic pipe connection apparatus 2 requires a pipe such as a cleaning liquid input pipe and a pipe used for other purposes. Sometimes. In short, M is the number of pipes that are at least N + 1 or more that can be arbitrarily set as needed.

K is usually any integer greater than or equal to N.
In some cases, a pipe such as a cleaning liquid discharge pipe may be required as a pipe at an outlet of the automatic M: K pipe connection device 2. In short, K
Indicates the number of pipes that are at least N and can be set arbitrarily as needed.

The tower tanks A to D will be described. In the present invention, it goes without saying that the number of towers is not limited to this, and may be increased or decreased.

The tower tanks A to D are of a batch type, and the tower tanks are provided with one outlet pipe from the bottom of the tower and one tower inlet pipe is installed at the top. . Here, N is an integer at least equal to the number of the towers A to D, and usually the same number of pipes as the number of towers is sufficient. Therefore, N is 4 in the example of FIG.

Conventionally, a plurality of pipes and control valves and the like are provided at the inlet pipes of the tower tanks A to D. However, in the present invention, as described above, an L: 1 automatic pipe is provided. Since the outlet pipe of the connecting device 1 is connected to the inlet pipe of the M: K pipe automatic connecting device 2 and supplied to an arbitrary tower tank, the inlet pipe to the tower tanks A to D is 1 each
A book is sufficient, and a piping at the entrance to the tower tanks A to D does not require a control valve.

The pipes 20, 22, 24 and 26 which are the pipes at the outlets of the tower tanks A to D are the same as those of the M:
The pipe 21, the pipe 23, the pipe 25, and the pipe 27 which are connected to the inlet pipe of the automatic pipe connection apparatus 2 of K and are the inlet pipes of the tower tanks A to D are connected to the automatic pipe of M: K. It is connected to the outlet pipe of the connection device 2.

As described above, since the M: K automatic pipe connection device 2 is connected to the towers A to D through arbitrary pipes and to arbitrary towers, the L: 1 pipe is connected. When the outlet pipe of the automatic connection apparatus 1 is connected to one of the inlet pipe groups of the M: K automatic pipe connection apparatus 2, the L: 1 automatic pipe connection apparatus 1 is connected to the M: K automatic pipe connection apparatus 2. It will be connected to arbitrary towers via the system. As a result, a desired fluid from any pipe selected from the pipes L1 to Ln to any desired column or tank, for example, a raw material, a solvent,
A cleaning liquid, cleaning water and the like can be supplied. Therefore, as will be described in detail later, the reactant a reacted in a certain tower tank is transferred to any other tower tank via the M: K automatic pipe connection device 2 and is transferred to the above-mentioned certain tower tank. In order to obtain another reactant b or perform another unit operation, the inside of a certain column tank is washed from the L: 1 automatic pipe connection apparatus 1 through the M: K automatic pipe connection apparatus 2. And the like can be performed very easily.

The functions of the tower group will be described below.

First, the case where at least a plurality of towers A to D have the same function will be described. Needless to say, having the same function means having at least a plurality of the same functions. Hereinafter, the towers A to C have the same function, and the tower D has different functions. The towers D are not limited to so-called towers, and unit operations can be performed. Anything that has a function is sufficient.

Since the towers A to C are of a batch type,
Although not limited to this, it is possible to have the same volume and the same shape, or to provide a plurality of the same functions such as the same auxiliary equipment such as a stirrer and a distillation equipment.
Therefore, the same or different unit operations can be performed in each of the tower tanks.

Secondly, a case where at least a plurality of the towers A to C have a plurality of different functions will be described.

It is possible to have a plurality of different functions for the same reasons as described above. Therefore, the same or different unit operations can be performed in each of the tower tanks.

Finally, usually, in the example where the towers A to D have one different function, completely different unit operations are performed in the respective towers.

The fact that so-called multi-product small-quantity production can be efficiently performed will be described below. Here, an example in which a reactant a as a medicine and a reactant b as a medicine will be described.

In this production method, each of the reactant a and the reactant b is reacted in the reaction step, crystallized in the crystallization step through the extraction step, and separated into the product by the centrifugal separator. .

As for the raw materials, reagents, solvents, washing liquids, washing water, etc. of the reactants a and b, those in the form of a solution are connected to the pipes L1 to Ln of the pipe group. Solid substances may be connected so as to be directly supplied to the towers A to D, respectively. In the example described below, in the pipes L1 to Ln of the pipe group, the pipe L1
And the pipe L2 are connected to the raw material a1 and the raw material a2 of the reactant a, respectively, and the pipe L3 and the pipe L4 are connected to the reactant b.
Are connected to the raw materials b1 and b2 of
5 and pipe L6 are reactant a and reactant b, respectively.
Cleaning liquid a and the cleaning liquid a.

First, the tower tanks A to C have the same functions of the reaction function, the extraction function and the crystallization function, and have the same functions.
An example in which has a centrifugal separation function will be described. The same applies to the examples described below.

In this example, the raw materials are sent to each of the towers A to C arbitrarily selected and independently reacted, extracted and crystallized in the towers A to C, respectively. By repeating the precipitation and separating the reactant a or the reactant b obtained in each column by a centrifugal separator, a desired product is selected.
Needless to say, it is preferable to prepare a centrifuge dedicated to the reactant a and a centrifuge dedicated to the reactant b in order to avoid mixing of other reactants.

Next, when the towers A to C have a plurality of different functions, the tower A has a reaction function and an extraction function, the tower B has an extraction function and a crystallization function, and the tower A has a plurality of functions. C will be described as an example having a crystallization function and a reaction function.

<Reaction in Tower A: Reactant a> In the tower A, the raw materials for obtaining the reactant a are the pipe L1, the pipe L2, and the pipe automatic connection apparatus 1, the pipe 10, and the pipe M. :
K is supplied to the tower tank A via the automatic pipe connection device 2 and the pipe 21, and a reaction for obtaining a reactant a is performed.

Next, the pipe 10 is washed with the cleaning liquid b supplied through the pipe automatic connection apparatus 1 of pipes L6 and L: 1. The cleaning waste liquid is discharged from a waste liquid discharge pipe (not shown) provided separately from the M: K automatic pipe connection device 2 and is separately processed.

<Reaction in Tower C: Reactant b> After washing the pipe 10, the raw materials for obtaining the reactant b are the pipe L3, the pipe L4, and the pipe automatic connection apparatus 1, the pipe 10,
M: K is supplied to the tower tank C via the pipe automatic connection device 2 and the pipe 25, and the reaction for obtaining the reactant b is performed.

<Reaction in Column A and Transition to Extraction in Column A: Reactant a> When the reaction is completed in Column A, the extraction operation in Column A is started.

<The reaction is completed in the column C, and the column B is
And extraction: Reactant b> On the other hand, pipe 2 from tower tank C
4. M: K is transferred to the tower tank B via the pipe automatic connection device 2 and the pipe 23, and the extraction operation is performed in the tank B. When the transfer from the tower tank C to the tower tank B is completed, the tower tank C and the pipe 24 used for the transfer, the M: K automatic pipe connection apparatus 2, the pipe 10, the L: 1 automatic pipe connection apparatus 1 and The cleaning is performed with the cleaning liquid b of the pipe L5 or the pipe L6 supplied through the pipe 25. The waste liquid after washing is M: K
Is discharged through a pipe (not shown) discharged from the automatic pipe connection device 2 of FIG.

<Extraction is completed in the tower tank B, and is transferred from the tower tank B to the tower tank C for crystallization: Reactant b> The entire contents of the tower tank B after the completion of the extraction operation are piped from the tower tank B. 22, M: K is transferred to the tower tank C via the pipe automatic connection device 2 and the pipe 25 to be crystallized.

When the transfer from the tower tank B to the tower tank C is completed, the tower tank B and the pipe 22, the M: K automatic pipe connection device 2 used for the transfer are automatically connected to the pipe 10, L: 1 pipe. The cleaning is performed with the cleaning liquid a of the pipe L5 supplied through the apparatus 1 and the pipe 23. The waste liquid after washing is discharged from the M: K pipe automatic connection device 2 (not shown).
And is processed separately.

<Extraction is completed in tower tank A, transferred from tower tank A to tower tank B and crystallized: reactant a> The contents of tower tank A after the completion of the extraction operation are pipe 20, M: K Is transferred to the tower tank B through the pipe automatic connection device 2 and the pipe 23, and is crystallized.

When the transfer from the tower tank A to the tower tank B is completed, the tower tank A and the pipe 20, the M: K automatic pipe connection device 2 used for the transfer are automatically connected to the pipe 10, L: 1 pipe. The cleaning is performed with the cleaning liquid a of the pipe L5 supplied through the apparatus 1 and the pipe 21. The waste liquid after washing is discharged from the M: K pipe automatic connection device 2 (not shown).
And is processed separately.

<Crystallization is completed in the tower C, and from the tower C to the centrifugal separator: the reactant b>
It is transferred to the centrifugal separator via the pipe automatic connection device 2 and the pipe 27 of M: K. Here, the reactant a is connected to the pipe L5,
Washing is performed with the cleaning liquid b supplied through the automatic pipe connection apparatus 1 of L: 1, the pipe 10, the automatic pipe connection apparatus 2 of M: K, and the pipe 27, and is subjected to a predetermined treatment except for the cleaning liquid b in the centrifuge. The product (reactant b). On the other hand, the waste liquid after the washing is supplied to the M: K automatic pipe connection apparatus 2 through the pipe 26, discharged through the pipe (not shown) discharged from the M: K automatic pipe connection apparatus 2, and treated separately. Is done.

<End of crystallization in tower tank B, from tower tank B to centrifuge: Reactant a> All the crystallized contents are transferred from tower tank B to pipe 22, M: K automatic pipe connection device 2. It is transferred to the centrifuge via the pipe 27. Here, the reactant a is connected to the pipe L6, the pipe automatic connection device 1 of L: 1, the pipe 10,
In order to avoid contamination with the reactant b, the washing liquid a is washed with another centrifugal separator not used for the reactant b in order to avoid contamination with the reactant b. Except for the above, it is separately processed to obtain a product (reactant a). On the other hand, the waste liquid after the washing is supplied to the M: K automatic pipe connection device 2 through the pipe 26,
It is discharged through a pipe (not shown) discharged from the M: K automatic pipe connection device 2 and is separately processed.

As described above, the reactant a was supplied to the column A (reaction).
→ Tower tank A (extraction) → Tower tank B (crystallization), reaction product b
After passing through the tower tank C (reaction) → the tower tank B (extraction) → the tower tank C (crystallization), they are separated into products by a centrifugal separator. During this time, any one of the tower tanks A to C becomes empty,
In order to fill the empty space, for example, when the tower A (extraction) and the tower B (extraction) are used, if the tower C is used for the reaction, the empty space can always be used.

By repeating these steps, the reactants a and b can be produced so that the tower tanks A to C always have no space.

Lastly, an example will be described in which, when the towers A to D usually have different functions, they are obtained in the order of a reactant a, a reactant b, a reactant a, and a reactant b. . Here, the column A has a function of a reaction, the column B has an extraction function, and the column C has a function of crystallization. Needless to say, the pipes and the like that have been used once are washed with the washing liquid as necessary as described above, and the waste liquid after the washing is separately treated.

When either one of the reactants a and b is selectively obtained, it goes without saying that washing can be omitted.

The raw material for obtaining the reactant a was supplied to the column A as described above, and the reaction was started. After the completion of the reaction, the entire contents were transferred from the tower A to the tower B. Then, tower tank A
And the transfer pipe including the pipe 10 was washed with the washing liquid b for the reactant b as described above.

The raw material for obtaining the reactant b was supplied to the tower A after the washing, and the reaction was started.

Extraction is performed in the tower B, and after completion of the extraction operation, all the contents are transferred to the tower C, and the tower B and the pipe 1
The transfer piping and the like including 0 were washed with the washing liquid b for the reactant b.

In the column B after the washing, the entire contents from the column A were transferred and extracted. Here, the column A, the transfer pipe including the pipe 10, and the like were washed with the washing liquid a for the reactant a, the raw material for obtaining the reactant a was supplied, and the reaction was started.

The reaction product a was crystallized in the tower C, and after the crystallization operation was completed, the entire contents were transferred to a centrifuge to obtain a product (reaction product a). The transfer piping including the tower tank C and the piping 10 was washed with the washing liquid for the reactant b.

In the column C after washing, the entire contents from the column B are transferred to crystallize the reactant b. After the crystallization operation is completed, the entire contents are transferred to the centrifugal separator and the product ( Reactant b)
I got The transfer piping and the like including the tower tank C and the piping 10 were washed with the washing liquid a for the reactant a. Here, the tower tank B is
The transfer pipe including the pipe 10 and the like were washed with the cleaning liquid b for the reactant b, the entire contents from the tower B were transferred, and the reactant b was extracted.

By repeating the above, reactants a,
It can be seen that products are obtained in the order of the reactants b, and that a high-mix low-volume production can be performed efficiently. Also, reactant a is replaced with reactant b
It can be seen that the same product can be efficiently produced by replacing

As described above, the so-called multi-product small-quantity production can be efficiently performed, and the production time of the same product can be minimized by stopping the operation of the towers installed in the same plant as much as possible. Put into operation,
It was found that the production amount per operation time can be increased or the operation time for the same production amount can be shortened.

[0063]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention has been described above, and the present invention will be further described in detail with reference to embodiments. It goes without saying that the present invention is not limited only to the embodiments described below. Example 1 Normally, methyl salicylate is prepared by charging salicylic acid, methanol, and sulfuric acid into a reactor equipped with a reflux condenser,
React at 90 ° C for 5-6 hours.

After completion of the reaction, unreacted methanol is recovered, cooled, and water is added to remove sulfuric acid. The reaction is transferred to a washing tank, washed with sodium carbonate solution and deacidified.
It is well known that this is sent to a dehydration tank, a desiccant is added to dehydrate it, and distillation in a distillation column yields ethyl salicylate.

In the example in which methyl salicylate was produced according to FIG. 1, when producing the same product, the time for stopping the work of the towers installed in the same plant was minimized, so-called full operation was performed, and The fact that the production volume can be increased or the operation time required for the same production volume can be reduced will be described.

In FIG. 1, column tanks A to D will be described in the order of reference numbers as examples having functions as a reaction tank, a washing tank, a dehydration tank and a distillation tower. However, it goes without saying that the present invention is not limited to this.

In the present invention, the L: 1 automatic piping connection device 1
Are connected to a methanol tank (not shown), a sulfuric acid tank (not shown), a sodium carbonate aqueous solution tank (not shown), and a water tank (not shown) as L1 to L4, respectively. Further, the system is such that salicylic acid (not shown) and a desiccant (not shown) can be separately supplied to the towers A to C.

A predetermined amount of salicylic acid is supplied to the column A, and further from the L1 and L2 via the automatic piping connection device 1 of L: 1, the piping 10, the automatic piping connection device 2 of M: K and the piping 21. A predetermined amount of methanol and a predetermined amount of sulfuric acid were supplied to the column A to start the reaction in the column A, and the reaction was carried out at 90 ° C. for 5 hours.

After 5 hours from the start of the reaction in the tower A, the reaction was stopped. Methanol was recovered by a cooling device not shown in this figure. The recovered methanol was separately purified and returned to the methanol tank.

On the other hand, water is supplied from the pipe L4 to the tower A, and the entire contents are stored in the pipe 20, the M: K automatic pipe connection device 2
And transferred to the tower tank B via the pipe 23.

The above-mentioned predetermined amount of salicylic acid is supplied to the emptied column A, and the above L1 and L2 are added to L: 1.
A predetermined amount of methanol and a predetermined amount of sulfuric acid are supplied to the column A via the automatic line connection device 1, the line 10, the automatic line connection device 2 for M: K and the line 21, and the reaction starts in the column A. And reacted at 90 ° C. for 5 hours.

On the other hand, in the tower tank B, the sodium carbonate solution was sent to neutralize the sulfuric acid, and water was supplied for washing. The neutralized solution and the like were sent to the pipe 20 and the M: K automatic pipe connection device 2, discharged through a pipe (not shown) discharged from the M: K automatic pipe connection device 2, and separately processed.

The contents from which the sulfuric acid had been removed were transferred from the tower tank B to the tower tank C through the pipe 22, the M: K automatic pipe connection device 2 and the pipe 25, and dehydrated.

In the column B, the same operation as described above was repeated.

The reaction product transferred to the column C and dehydrated was transferred to the column D and distilled to obtain methyl salicylate.

In the tower tank B, the same operation as described above was repeated.

The above operations were repeated to obtain methyl salicylate efficiently.

[0078]

According to the present invention, the following effects can be obtained. (1) By connecting one of the outlet pipes of the L: 1 automatic pipe connection device to the inlet pipe of the M: K automatic pipe connection device, through the M: K automatic pipe connection device Raw materials from any L: 1 automatic piping connection device
Solvents, cleaning liquids, etc. can be supplied. For this reason, control valves and the like, which are conventionally required for all piping at the inlet of tower tanks, are omitted, and it is sufficient to install only at the piping at the inlet of the L: 1 automatic piping connection device. (2) By connecting one of the outlet pipes of the L: 1 automatic pipe connection device to the inlet pipe of the M: K automatic pipe connection device, through the M: K automatic pipe connection device, Raw materials, solvents, cleaning liquids, etc. can be supplied from the L: 1 automatic piping connection device to the tower tanks. Therefore, high-mix low-volume production can be planned regardless of the number and function of the towers. (3) For the same reason, it is possible to formulate a production plan that minimizes idle time in the production of the same product type.

[Brief description of the drawings]

FIG. 1 is an explanatory diagram showing an embodiment of the present invention.

[Explanation of symbols]

 1 L: Automatic piping connection device for 1: 2 M: Automatic piping connection device for K A to D Tower tanks Lx Piping group L1 to Ln Piping 10, 20 to 29 Piping

────────────────────────────────────────────────── ───

[Procedure amendment]

[Submission date] March 22, 2000 (200.3.2)
2)

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0004

[Correction method] Change

[Correction contents]

Against this background, the applicant has previously disclosed in Japanese Patent Publication No. 8-12000 a combination of a plurality of hose groups used in a batch-type production system instead of fixed pipes, and It proposed a flexible automatic connection apparatus and management system hose stations for transferring and intermediate products. In this publication, the connection device includes a unit in which a plurality of cells are vertically arranged in a line, a unit in which a plurality of cells are arranged in a line, and a moving body that moves in the cell. Two hose groups, one end of each hose connected to a board and the other end connected to a connection joint in the moving body so that the hoses do not get caught, and the moving body provided in both units is moved in the cell. And a device for moving both units or joints to connect the ends of the hoses and releasing the connection after the fluid transfer operation is completed.

[Procedure amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0006

[Correction method] Change

[Correction contents]

Further, in the above two proposals, there is a possibility that the excess length of a hose or the like may be bent and a liquid pool may be generated in a vertically provided switching station. As means for preventing contamination, Japanese Patent Laid-Open Publication No. 7-71699 has proposed an automatic pipe connection apparatus for a switching station that does not cause the liquid pool. Squid, are collectively these pipes automatic connection apparatus having a pipe connection portion of the inlet pipe connecting portion and K present at the outlet of the M M: that K piping automatic connection device.

[Procedure amendment 3]

[Document name to be amended] Statement

[Correction target item name] 0025

[Correction method] Change

[Correction contents]

Conventionally, a plurality of pipes and control valves have been provided at the inlet pipes of the towers A to D. However, in the present invention, as described above, the L: 1 pipe automatic connection is provided. Since the outlet pipe of the apparatus 1 is connected to the inlet pipe of the M: K pipe automatic connection apparatus 2 and supplied to an arbitrary tower, the inlet pipes to the tower tanks A to D are respectively provided. A single pipe is sufficient, and a piping at the inlet to the tower tanks A to D does not require a control valve.

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0036

[Correction method] Change

[Correction contents]

As for the raw materials, reagents, solvents, washing liquids, washing water, etc. of the reactants a and b, those in the form of a solution are connected to the pipes L1 to Ln of the pipe group. Solid substances may be connected so as to be directly supplied to the towers A to D, respectively. In the example described below, in the pipes L1 to Ln of the pipe group, the pipe L1
And the pipe L2 are connected to the raw material a1 and the raw material a2 of the reactant a, respectively, and the pipe L3 and the pipe L4 are connected to the reactant b.
Are connected to the raw materials b1 and b2 of
5 and pipe L6 are reactant a and reactant b, respectively.
Are connected to the cleaning liquid a and the cleaning liquid b .

[Procedure amendment 5]

[Document name to be amended] Statement

[Correction target item name] 0038

[Correction method] Change

[Correction contents]

In this example, the raw materials are sent to each of the towers A to C arbitrarily selected and independently reacted, extracted and crystallized in the towers A to C, respectively. The desired product can be obtained by repeating the precipitation and separating the reactant a or the reactant b obtained in each column tank by a centrifuge.
Needless to say, it is preferable to prepare a centrifuge dedicated to the reactant a and a centrifuge dedicated to the reactant b in order to avoid mixing of other reactants.

[Procedure amendment 6]

[Document name to be amended] Statement

[Correction target item name] 0044

[Correction method] Change

[Correction contents]

<The reaction is completed in the column C, and the column B is
And extraction: Reactant b> On the other hand, pipe 24 from tower tank C
M: Tower tank B via pipe automatic connection device 2 and pipe 23 of K
And the extraction operation is performed in the tank B. Tower tank C
When the transfer from the vessel to the tower tank B is completed, the tower tank C and the pipe 24 used for the transfer, the M: K pipe automatic connection device 2
Is cleaned with the cleaning liquid b of the pipe L5 or the pipe L6 supplied through the pipe 10, L: 1 automatic pipe connection device 1 and the pipe 25. The waste liquid after washing is discharged from the M: K pipe automatic connection device 2 (not shown).
And is processed separately.

[Procedure amendment 7]

[Document name to be amended] Statement

[Correction target item name] 0051

[Correction method] Change

[Correction contents]

As described above, the reactant a was supplied to the column A (reaction).
→ tower tank A (extraction) → via column tank B (crystallization), the reaction product b
Means tower tank C (reaction) → tower tank B (extraction) → tower tank C (crystallization)
After that , the product is separated by a centrifuge to obtain a product. During this time,
Any one of the tower tanks A to C becomes empty. For example, the tower tank A (extraction) is filled so as to fill the empty space.
When the tower tank B (extraction) is used, if the tower tank C is used for the reaction, it can be used without any empty space.

[Procedure amendment 8]

[Document name to be amended] Statement

[Correction target item name] 0064

[Correction method] Change

[Correction contents]

After completion of the reaction, unreacted methanol is recovered, cooled, and water is added to remove sulfuric acid. The reaction is transferred to a washing tank, washed with sodium carbonate solution and deacidified.
This was dehydrated by adding the feed desiccant dehydration tub, salicylic methylation is well known to be obtained when distilling in a distillation column.

[Procedure amendment 9]

[Document name to be amended] Statement

[Correction target item name] 0071

[Correction method] Change

[Correction contents]

The above-mentioned predetermined amount of salicylic acid is supplied to the emptied column A, and the above L1 and L2 are added to L: 1.
A predetermined amount of methanol and a predetermined amount of sulfuric acid are supplied to the tower tank A via the automatic pipe connection apparatus 1, the pipe 10, the M: K automatic pipe connection apparatus 2 and the pipe 21, and the reaction is started in the tower tank A. At 90 ° C. for 5 hours.

[Procedure amendment 10]

[Document name to be amended] Statement

[Correction target item name] 0073

[Correction method] Change

[Correction contents]

The contents from which the sulfuric acid had been removed were transferred from the tower tank B to the tower tank C through the pipe 22, the M: K automatic pipe connection device 2 and the pipe 25, and dehydrated.

Claims (5)

[Claims] 1. An N tube having one outlet pipe from the bottom of the tower and one inlet pipe from the top of the tower.
A batch-type tower tank group, an M: K pipe automatic connection device having M inlet pipes and K outlet pipes, and L inlet pipes and one outlet pipe L for raw material supply:
1 automatic pipe connection device, and connects the N outlet pipes of each tower in the tower group and the N inlet pipes of the tower group to an M: K automatic pipe connection device. An improved multi-purpose production apparatus (here, L, K) wherein one of the inlet pipes of the M: K automatic pipe connection apparatus is connected to the outlet pipe of the L: 1 automatic pipe connection apparatus. K and M are arbitrary integers indicating the number of pipes, N is the number of tanks, M ≧ N + 1, K
≧ N). 2. The improved multipurpose production apparatus according to claim 1, wherein a plurality of towers in the tower group have the same function. 3. The improved multipurpose production apparatus according to claim 1, wherein a plurality of towers in the tower group have a plurality of different functions. 4. The improved multipurpose production apparatus according to claim 1, wherein a plurality of towers in the tower group have a single different function. 5. A multi-purpose production apparatus according to claim 1, wherein one unit reaction is performed in one of the tower tanks, and the contents of the tower tank are automatically adjusted to M: K piping. An improved multi-purpose production method, characterized in that the connection device is switched and transferred to another tower, where another unit operation is performed.