JP7199993B2 - Polymer production system and production method - Google Patents

Description

The present invention relates to a polymer production system and production method. Specifically, the present invention relates to a polymer production system and production method capable of continuously producing a polymer.

BACKGROUND ART Conventionally, as a method for producing a polymer such as polyamic acid, a batch production method using a stirring tank has been known. Batch manufacturing methods are relatively superior in terms of quality control, but may not be suitable for mass production.

On the other hand, for example, a method of continuously producing polyamic acid (polyamic acid) in a tube has been proposed (see, for example, Patent Document 1).

Japanese Patent Application Laid-Open No. 2006-249380

However, in the method disclosed in Patent Document 1, it is said that it is difficult to stably obtain the desired polymer due to the large influence of the compositional difference in the raw material solution caused by the difference between raw material lots and the error in the charging amount. I had a problem.

In addition, management based on ex post facto analysis results takes time to adjust the supply conditions of the raw material solution, etc., which may result in the production of many out-of-specification waste products. In order to reduce the out-of-specification rate, it is conceivable to constantly assign experienced workers to perform monitoring and management, but this causes an increase in work load and manufacturing costs.

Under such circumstances, there is a demand for a polymer production system and production method that can stably obtain a desired polymer.

An object of the present invention is to provide a polymer production system and a production method capable of continuously and stably obtaining a desired polymer. Another object of the present invention is to provide a polymer production system and production method capable of reducing the speck out rate in continuous polymer production.

Specific means for solving the above problems include the following embodiments.
<1> A polymer is prepared from a first solution containing a first polyaddition polymerizable compound and a second solution containing a second polyaddition polymerizable compound that polyadditions with the first polymerizable compound as raw materials. A polymer manufacturing system for manufacturing,
a first supply unit that supplies the first solution;
a second supply unit that supplies the second solution;
a first mixing unit that mixes the first solution and the second solution to generate a first mixed solution;
It is arranged continuously downstream of the first mixing section, and includes a first polymer by advancing a polymerization reaction between the first polymerizable compound and the second polymerizable compound contained in the first mixed solution. a first reaction section that produces a first polymerization solution;
a first measurement unit that acquires first reaction information related to the viscosity of the first polymerization solution, the absorbance of the first polymerization solution, or the pressure difference between two points in the flow direction in the flow path of the first polymerization solution ;
a first control unit that controls supply in the first supply unit and/or the second supply unit based on the first reaction information acquired by the first measurement unit ;
Among the first polymerizable compound and the second polymerizable compound, one is a tetracarboxylic dianhydride and the other is a diamine, or one is an acid anhydride group-terminated or amino group-terminated polyamic acid, and the other is A diamine or a tetracarboxylic dianhydride,
A polymer production system for producing polyamic acid as the first polymer .

< 2 > The first measuring unit has a viscometer, acquires first viscosity information about the viscosity of the first polymerization solution as the first reaction information,
The weight according to < 1 >, wherein the first control unit controls supply in the first supply unit and/or the second supply unit based on the first viscosity information acquired by the first measurement unit. Combined manufacturing system.

< 3 > The first polymer is a polyaddition polymer,
a third supply unit that supplies a third solution containing a polyadditive third polymerizable compound that polyadditions to the first polymer;
a second mixing unit that mixes the first polymerization solution and the third solution to generate a second mixed solution;
The first polymer from the first polymerization solution and the third polymerizable compound from the third solution, which are arranged continuously downstream of the second mixing section and are contained in the second mixed solution a second reaction part that advances the polymerization reaction of to generate a second polymerization solution containing the second polymer;
a second measurement unit that acquires second reaction information related to the viscosity of the second polymerization solution, the absorbance of the second polymerization solution, or the pressure difference between two points in the flow direction of the flow path of the second polymerization solution ;
a second control unit that controls supply in the third supply unit based on the second reaction information acquired by the second measurement unit ;
The first polymer is an acid anhydride group-terminated or amino group-terminated polyamic acid,
the third polymerizable compound is a diamine or a tetracarboxylic dianhydride,
The polymer production system according to <1> or <2> , which produces polyamic acid as the second polymer .

< 4 > The second measurement unit has a viscometer, acquires second viscosity information about the viscosity of the second polymerization solution as the second reaction information,
The polymer production system according to < 3 >, wherein the second control unit controls supply in the third supply unit based on the second viscosity information acquired by the second measurement unit.

< 5 > The polymer production system according to any one of < 1 > to < 4 >, further comprising an imidization unit that imidizes the produced polyamic acid.

< 6 > A polymer is prepared from a first solution containing a first polyaddition polymerizable compound and a second solution containing a second polyaddition polymerizable compound that polyadditions with the first polymerizable compound as raw materials. A method for producing a polymer to be produced,
a first supply step of supplying the first solution;
a second supply step of supplying the second solution;
a first mixing step of mixing the first solution and the second solution to generate a first mixed solution;
a first reaction step of allowing a polymerization reaction between the first polymerizable compound and the second polymerizable compound contained in the first mixed solution to generate a first polymerization solution containing the first polymer;
a first measuring step of acquiring first reaction information related to the viscosity of the first polymerization solution, the absorbance of the first polymerization solution, or the pressure difference between two points in the flow direction in the flow path of the first polymerization solution ;
a first control step of controlling supply in the first supply step and/or the second supply step based on the first reaction information acquired in the first measurement step ;
Among the first polymerizable compound and the second polymerizable compound, one is a tetracarboxylic dianhydride and the other is a diamine, or one is an acid anhydride group-terminated or amino group-terminated polyamic acid, and the other is A diamine or a tetracarboxylic dianhydride,
A method for producing a polymer in which polyamic acid is produced as the first polymer .

< 7 > In the first measurement step, the viscometer acquires first viscosity information about the viscosity of the first polymerization solution as the first reaction information,
< 6 >, wherein in the first control step, supply in the first supply step and/or the second supply step is controlled based on the first viscosity information acquired in the first measurement step A method for producing a polymer.

< 8 > The first polymer is a polyaddition polymer,
a third supplying step of supplying a third solution containing a polyadditional third polymerizable compound that polyadditions to the first polymer;
a second mixing step of mixing the first polymerization solution and the third solution to generate a second mixed solution;
The polymerization reaction between the first polymer from the first polymerization solution contained in the second mixed solution and the third polymerizable compound from the third solution is allowed to proceed to produce a second polymer containing the second polymer. a second reaction step of producing a polymerization solution;
a second measuring step of acquiring second reaction information related to the viscosity of the second polymerization solution, the absorbance of the second polymerization solution, or the pressure difference between two points in the flow direction in the flow path of the second polymerization solution ;
a second control step of controlling supply in the third supply step based on the second reaction information acquired in the second measurement step ;
The first polymer is an acid anhydride group-terminated or amino group-terminated polyamic acid,
the third polymerizable compound is a diamine or a tetracarboxylic dianhydride,
The method for producing a polymer according to <6> or <7>, wherein a polyamic acid is produced as the second polymer .

< 9 > In the second measurement step, the viscometer acquires second viscosity information about the viscosity of the second polymerization solution as the second reaction information,
The method for producing a polymer according to < 8 >, wherein in the second control step, supply in the third supply step is controlled based on the second viscosity information acquired in the second measurement step.

< 10 > The method for producing the polymer according to any one of < 6 > to < 9 >, further comprising imidizing the produced polyamic acid.

ADVANTAGE OF THE INVENTION According to this invention, the polymer manufacturing system and manufacturing method which can obtain a desired polymer continuously and stably can be provided. Moreover, according to the present invention, it is possible to provide a polymer production system and a production method capable of reducing the speck out rate in continuous polymer production.

It is a figure which shows the polymer manufacturing system in 1st Embodiment. 1 is a block diagram of a polymer production system in a first embodiment; FIG. It is a flowchart explaining operation|movement of the polymer manufacturing system in 1st Embodiment. FIG. 4 is a flow chart explaining another operation of the polymer production system in the first embodiment; It is a figure which shows the polymer manufacturing system in 2nd Embodiment. It is a block diagram of a polymer production system in a second embodiment. It is a flowchart explaining operation|movement of the polymer manufacturing system in 2nd Embodiment. It is a flowchart explaining other operation|movement of the polymer manufacturing system in 2nd Embodiment.

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
The first embodiment is an example of a polymer production system having a single-stage reaction section, and is an example of a system capable of adjusting the supply amount of the raw material solution based on the measurement information from the measurement section. The second embodiment is an example of a polymer manufacturing system having a two-stage reaction section, and is an example of a system capable of adjusting the supply amount of the raw material solution based on the measurement information from the measurement section.

<First Embodiment>
A polymer manufacturing system according to the first embodiment will be described with reference to FIGS. 1 to 4. FIG. FIG. 1 is a diagram showing a polymer production system according to the first embodiment. FIG. 2 is a block diagram of the polymer production system in the first embodiment. FIG. 3 is a flowchart explaining the operation of the polymer production system in the first embodiment. FIG. 4 is a flowchart explaining another operation of the polymer production system in the first embodiment.

First, an overview of the polymer production system 1 in the first embodiment will be described.
The polymer production system 1 comprises a first solution A1 in which a first polyaddition polymerizable compound is dissolved, and a second solution A2 in which a second polyaddition polymerizable compound that polyadditions with the first polymerizable compound is dissolved. It is a production system for producing the first polymer using as a raw material. The first embodiment is an example of a polymer production system having a single reaction section.

As an example, the case where one of the first polymerizable compound and the second polymerizable compound is a tetracarboxylic dianhydride and the other is a diamine, and a polyamic acid is produced as the first polymer will be described below. More specifically, the first polymerizable compound contained in the first solution A1 is a tetracarboxylic dianhydride, the second polymerizable compound contained in the second solution A2 is a diamine, and the first polymer A case of producing a polyamic acid will be described.

The tetracarboxylic dianhydride is not particularly limited, and those similar to those used in conventional polyimide synthesis can be used. Specific examples of tetracarboxylic dianhydrides include 3,3′,4,4′-benzophenonetetracarboxylic dianhydride, 3,3′,4,4′-biphenyltetracarboxylic dianhydride, 2, 3,3′,4′-biphenyltetracarboxylic dianhydride, pyromellitic dianhydride, 1,3-bis(2,3-dicarboxyphenoxy)benzene dianhydride, 1,4-bis(2, 3-dicarboxyphenoxy)benzene dianhydride, 2,3,3′,4′-benzophenonetetracarboxylic dianhydride, 2,2′,3,3′-benzophenonetetracarboxylic dianhydride, 2,2 ',3,3'-biphenyltetracarboxylic dianhydride, 2,2',6,6'-biphenyltetracarboxylic dianhydride, naphthalene-1,2,4,5-tetracarboxylic dianhydride, anthracene-2,3,6,7-tetracarboxylic dianhydride, phenanthrene-1,8,9,10-tetracarboxylic dianhydride, 2,2-bis(4-hydroxyphenyl)propane dibenzoate-3 ,3′,4,4′-tetracarboxylic dianhydride and other aromatic tetracarboxylic dianhydrides; butane-1,2,3,4-tetracarboxylic dianhydride and other aliphatic tetracarboxylic dianhydrides; anhydride; alicyclic tetracarboxylic dianhydride such as cyclobutane-1,2,3,4-tetracarboxylic dianhydride; thiophene-2,3,4,5-tetracarboxylic dianhydride, pyridine- heterocyclic tetracarboxylic dianhydrides such as 2,3,5,6-tetracarboxylic dianhydride; Tetracarboxylic dianhydrides may be used alone or in combination of two or more.

As a solvent for the first solution A1, a solvent in which tetracarboxylic dianhydride and polyamic acid are dissolved is used. Specific examples of solvents include amide solvents such as N,N-dimethylformamide, N,N-dimethylacetamide, N-methyl-2-pyrrolidone, 1,3-dimethyl-2-imidazolidinone, and acetanilide; Cyclic ester solvents such as butyrolactone; chain ester solvents such as ethyl acetate; ketone solvents such as 2-propanone, 3-pentanone, acetone and methyl ethyl ketone; ether solvents such as tetrahydrofuran and dioxolane; and aromatic hydrocarbon solvents such as toluene and xylene; and the like. Among these, amide-based solvents, cyclic ester-based solvents, and ether-based solvents in which the polyamic acid is highly soluble are preferred. A solvent may be used individually by 1 type, and may mix 2 or more types. For example, by mixing a highly polar alcoholic solvent with a solvent in which polyamic acid has relatively low solubility, such as acetone, ethyl acetate, methyl ethyl ketone, toluene, and xylene, the solubility of polyamic acid can be improved. is also possible.

The first solution A1 may contain a small amount of a tertiary amine such as trimethylamine or triethylamine in order to increase the solubility of the tetracarboxylic dianhydride or increase the reactivity with the diamine.

The diamine is not particularly limited, and the same diamines as those used in conventional polyimide synthesis can be used. Specific examples of diamines include 4,4′-diaminodiphenylmethane, 4,4′-diaminodiphenyl ether, 2,2-bis[4-(4-aminophenoxy)phenyl]propane, 4,4′-bis(4- aminophenoxy)biphenyl, 1,4'-bis(4-aminophenoxy)benzene, 1,3'-bis(4-aminophenoxy)benzene, o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, 3, 4'-diaminodiphenyl ether, 4,4'-diaminodiphenylsulfone, 3,4'-diaminodiphenylsulfone, 3,3'-diaminodiphenylsulfone, 4,4'-methylene-bis(2-chloroaniline), 3, 3'-dimethyl-4,4'-diaminobiphenyl, 4,4'-diaminodiphenyl sulfide, 2,6-diaminotoluene, 2,4-diaminochlorobenzene, 1,2-diaminoanthraquinone, 1,4-diaminoanthraquinone, Aromatic diamines such as 3,3′-diaminobenzophenone, 3,4′-diaminobenzophenone, 4,4′-diaminobenzophenone, 4,4′-diaminobibenzyl; 1,2-diaminoethane, 1,4-diamino Aliphatic diamines such as butane, tetramethylenediamine, and 1,10-diaminododecane; heterocyclic diamines such as 3,4-diaminopyridine; and the like. A diamine may be used individually by 1 type, and may use 2 or more types together.

As a solvent for the second solution A2, a solvent in which diamine and polyamic acid are dissolved is used. Specific examples of solvents include amide solvents such as N,N-dimethylformamide, N,N-dimethylacetamide, N-methyl-2-pyrrolidone, 1,3-dimethyl-2-imidazolidinone, and acetanilide; Cyclic ester solvents such as butyrolactone; chain ester solvents such as ethyl acetate; ketone solvents such as 2-propanone, 3-pentanone, acetone and methyl ethyl ketone; ether solvents such as tetrahydrofuran and dioxolane; and aromatic hydrocarbon solvents such as toluene and xylene; and the like. Among these, amide-based solvents, cyclic ester-based solvents, and ether-based solvents in which the polyamic acid is highly soluble are preferred. A solvent may be used individually by 1 type, and may mix 2 or more types. For example, by mixing a highly polar alcoholic solvent with a solvent in which polyamic acid has relatively low solubility, such as acetone, ethyl acetate, methyl ethyl ketone, toluene, and xylene, the solubility of polyamic acid can be improved. is also possible.

As shown in FIG. 1, the polymer production system 1 mixes a first solution A1 and a second solution A2, which are raw materials, in a first mixing section 20 to generate a first mixed solution B, and a first reaction section 30 , the polymerization reaction proceeds to generate the first polymerization solution C, thereby producing a polyamic acid (first polymer).

Here, the polymer production system 1 has a tubular liquid-feeding line L that connects the first and second tanks 11 and 12 described later to the first cushion tank 40 in a sealed state. As a result, the polymer production system 1 can continuously produce a polymer without generating air bubbles in the first mixed solution B or the first polymerization solution C.

Next, a specific configuration of the polymer production system 1 will be described.
As shown in FIG. 1, the polymer production system 1 includes a first tank 11, a second tank 12, a first supply pump 15 (first supply section), and a second supply pump 16 (second supply section). , a first mixing section 20 , a first reaction section 30 , a first cushion tank 40 , and a liquid feeding line L. The liquid feeding line L described above has a first liquid feeding section L1, a second liquid feeding section L2, a third liquid feeding section L3, a fourth liquid feeding section L4, and a fifth liquid feeding section L5. . Here, the third liquid feeding section L3 constitutes the first mixing section 20 . Further, the fourth liquid feeding section L4 constitutes the first reaction section 30. As shown in FIG.

The first tank 11 contains a first solution A1 containing a first polyaddition polymerizable compound. In this embodiment, the first tank 11 contains a first solution A1 containing tetracarboxylic dianhydride.

The second tank 12 contains a second solution A2 containing a second polyaddition polymerizable compound that polyadditions with the first polymerizable compound. In this embodiment, the second tank 12 contains a second solution A2 containing diamine.

The first supply pump 15 (first supply section) supplies the first solution A1 contained in the first tank 11 to the first mixing section 20 . The first supply pump 15 supplies the first solution A1 at a predetermined amount. For example, the first supply pump 15 is adjusted so as to supply the first solution A1 under the conditions under which polyamic acid (first polymer) having desired properties is obtained.

The second supply pump 16 (second supply section) supplies the second solution A2 contained in the second tank 12 to the first mixing section 20 . The second supply pump 16 supplies the second solution A2 at a predetermined amount. For example, the second supply pump 16 is adjusted so as to supply the second solution A2 under conditions under which polyamic acid (first polymer) having desired properties is obtained.

The first mixing section 20 generates a first mixed solution B by mixing the first solution A1 and the second solution A2. The first mixing section 20 is arranged downstream of the first supply pump 15 and the second supply pump 16 . The first mixing section 20 has a first confluence valve 21 and a first mixing stirring section 25 . Further, the first mixing section 20 has a third liquid feeding section L3.

The first merging valve 21 joins the first solution A1 supplied by the first supply pump 15 and the second solution A2 supplied by the second supply pump 16 . The first confluence valve 21 mixes the first solution A1 and the second solution A2.

The first mixing/stirring unit 25 stirs the first mixed solution B in which the first solution A1 and the second solution A2 are mixed without coming into contact with gas. The first mixing/stirring unit 25 is arranged inside the pipe that constitutes the third liquid feeding unit L3, or is configured to constitute the third liquid feeding unit L3.

The first mixing and stirring unit 25 includes, for example, static mixers, nozzles, orifices, and other static mixers, centrifugal pumps, volute pumps, and driven mixers, such as inline mixers having stirring blades, preferably It comprises a static mixer, more preferably a static mixer. In addition, a pipe with a twist tape inserted (see [Fig. 19] of Japanese Patent Application Laid-Open No. 2003-314982, etc.) can also provide the same agitation promotion effect as a static mixer, but the static mixer has a better agitation promotion effect. is obtained.

The static mixer is not particularly limited, and examples thereof include static mixers such as Kenics mixer type, Sulzer SMV type, Sulzer SMX type, Tray Hi-mixer type, Komax mixer type, Lightnin mixer type, Ross ISG type, and Bran & Lube mixer type. mentioned. Among these, the Kenics mixer type static mixer is more preferable since it has a simple structure and has no dead space.

Although the position of the first mixing/stirring section 25 is not particularly limited, it is preferably arranged on the first merging valve 21 side (for example, near) in the first mixing section 20, for example.

The first reaction section 30 is arranged continuously downstream of the first mixing section 20 . The first reaction section 30 is a section where the polymerization reaction between the first polymerizable compound and the second polymerizable compound contained in the first mixed solution B proceeds. In the first reaction section 30, the polymerization reaction between the first polymerizable compound and the second polymerizable compound contained in the first mixed solution B progresses gradually, and the first polymerized solution C is obtained.

The first reaction section 30 has a fourth liquid feeding section L4, a first reaction stirring section 35, and a first temperature control tank 39.

The fourth liquid feeding portion L4 is a portion from one end portion L4a to the other end portion L4b in the present embodiment. The hollow part of the pipe that constitutes the fourth liquid feeding part L4 has, for example, a cross-sectional area of 1 mm ² or more and 400 cm ² or less, but is not limited to this. The fourth liquid sending section L4 has a first reaction adjustment section 32 and a second reaction adjustment section 37 .

The first reaction adjustment section 32 is a piping section arranged upstream of the first reaction stirring section 35 . The first reaction adjusting section 32 is formed so that the first mixed solution B flows for a desired residence time. The first reaction adjustment section 32 is arranged in the first temperature control tank 39 and is temperature-controlled (for example, cooled) to a desired temperature condition. In the first reaction adjusting section 32 , the first mixed solution B is adjusted to a temperature suitable for the polymerization reaction and sent to the first reaction stirring section 35 .

The second reaction adjustment section 37 is a piping section arranged downstream of the first reaction stirring section 35 . The second reaction adjusting section 37 is formed so that the first mixed solution B flows for a desired residence time. The second reaction adjustment section 37 is arranged in the first temperature control tank 39 and is temperature-controlled (for example, cooled) to a desired temperature condition. In the second reaction adjusting section 37, the first mixed solution B stirred by the first reaction stirring section 35, which will be described later, is adjusted to a temperature suitable for the polymerization reaction and fed.

In FIG. 1, the structures of the first reaction adjustment section 32 and the second reaction adjustment section 37 are shown as helical tubes, but as long as a sufficient residence time is ensured, any structure such as a straight tube or a curved tube may be used. can do.

The first reaction stirring section 35 stirs the first mixed solution B sent from the first reaction adjusting section 32 without contacting gas. In the present embodiment, the first reaction-stirring unit 35 stirs the first mixed solution B, which has been adjusted to a temperature suitable for the polymerization reaction by the first reaction adjustment unit 32, without coming into contact with gas.

As described above, the first reaction-stirring unit 35 includes, for example, static mixers such as static mixers, nozzles, and orifices, and drive-type mixers such as centrifugal pumps, vortex pumps, and in-line mixers having stirring blades. preferably includes a static mixer, more preferably includes a static mixer. As described above, a pipe with a twist tape inserted therein can also provide a stirring promotion effect in the same manner as a static mixer.

The static mixer is not particularly limited, and examples thereof include static mixers such as Kenics mixer type, Sulzer SMV type, Sulzer SMX type, Tray Hi-mixer type, Komax mixer type, Lightnin mixer type, Ross ISG type, and Bran & Lube mixer type. mentioned. Among these, the Kenics mixer type static mixer is more preferable since it has a simple structure and has no dead space.

Although the position of the first reaction/stirring section 35 is not particularly limited, it is preferably arranged in the middle of the first reaction section 30, for example.

The first cushion tank 40 accommodates the first polymerization solution C from the first reaction section 30 . The first cushion tank 40 serves as a tank for containing a raw material solution, for example, when polyimide is produced by imidating polyamic acid, which is the first polymer.

When the polymer production system 1 according to the present embodiment produces polyimide, the polymer production system 1 further includes an imidization unit that imidizes the polyamic acid. The imidization unit (not shown) imidizes the polyamic acid by, for example, a thermal imidization method of thermal dehydration ring closure, a chemical imidization method using a dehydrating agent and an imidization accelerator, or the like.

When the polymer manufacturing system 1 manufactures polyimide, the first cushion tank 40 may be omitted, and the liquid may be fed from the fifth liquid feeding section L5 to the imidization section. However, as described above, it is preferable to temporarily store the polyamic acid in the first cushion tank 40 .

In addition, the polymer production system 1 may be any one or more of the first solution A1, the second solution A2, the first mixed solution B, and the first polymerization solution C (hereinafter referred to as "first measurement object"). and/or a first measuring unit that acquires one or more first reaction information regarding the composition. In this embodiment, the polymer production system 1 has a plurality of first measurement units. More specifically, the polymer production system 1 includes a pump pressure measurement unit 81, first differential pressure measurement units 91 and 92, second differential pressure measurement units 93 and 94, a first viscosity measurement unit 111, have

The pump pressure measurement unit 81 acquires information on the pump pressure of the first supply pump 15 as first reaction information. The pump pressure measurement unit 81 acquires, for example, numerical information on the pump pressure and information on voltage and current values as the first reaction information.

The first differential pressure measurement units 91 and 92 acquire information on the input/output differential pressure (differential pressure between the upstream side and the downstream side) in the first mixing/stirring unit 25 as first reaction information.
The second differential pressure measurement units 93, 93 acquire information on the input/output differential pressure (differential pressure between upstream and downstream sides) in the first reaction unit 30 as first reaction information.

The first viscosity measurement unit 111 acquires viscosity information of the first polymerization solution C as first reaction information. Viscosity information is effective information as the first reaction information because the viscosity increases as the polymerization reaction progresses.

The first measurement unit is not limited to the measurement unit (type of physical quantity and/or composition, measurement method) of this embodiment. The first measurement unit includes, for example, a viscometer, a pressure gauge, a pump pressure gauge, an absorbance meter, an infrared spectrometer, a near-infrared spectrometer, a density meter, a color difference meter, a refractometer, a spectrophotometer, a conductivity meter, a turbidity It comprises one or more selected from the group consisting of a photometer and a fluorescent X-ray spectrometer.

The first measurement unit acquires one or more pieces of first reaction information relating to the physical quantity and/or composition of the first measurement object, and outputs the acquired first reaction information to the first control unit 200, which will be described later.

Next, a block diagram of the polymer production system 1 according to the first embodiment will be described with reference to FIG.
As shown in FIG. 2, the polymer production system 1 includes a plurality of first measurement units (first measurement unit group), a first control unit 200, a first storage unit 300, and a first supply unit to be controlled. and a pump 15 and a second supply pump 16 .

The first measurement unit acquires one or more pieces of first reaction information regarding the physical quantity and/or composition of the first measurement object, as described above. The polymer production system 1 has a plurality of first measurement units. More specifically, the polymer production system 1 includes a pump pressure measurement unit 81, first differential pressure measurement units 91 and 92, second differential pressure measurement units 93 and 94, a first viscosity measurement unit 111, have
Here, the first reaction information includes numerical information such as measured values of physical quantity and/or composition, as well as electrical signals that change corresponding to physical quantity and/or composition.

The first control unit 200 controls supply by the first supply pump 15 and/or the second supply pump 16 based on the first reaction information acquired by the first measurement unit.
First control unit 200 has determination unit 210 , selection unit 220 , and instruction unit 230 .

Based on the first reaction information from the first measurement unit, the determination unit 210 determines whether the physical quantity and/or the measured value of the composition of the first measurement object is within a predetermined allowable range. The determination unit 210 acquires the first reaction information from the first measurement unit based on the measurement interval stored in the measurement interval information storage unit 310, which will be described later, and the allowable range stored in the allowable range information storage unit 320, which will be described later Based on the information, it is determined whether the obtained first reaction information is within a predetermined allowable range.

If there is a plurality of pieces of first reaction information determined by the determination unit 210 to be out of the allowable range, the selection unit 220 selects the first reaction to be prioritized in control based on the priority information from the priority information storage unit 340, which will be described later. Select information.
Further, when the first reaction information determined by the determination unit 210 to be out of the allowable range is specific information, for example, when the first reaction information is viscosity information, the selection unit 220 stores complementary information, which will be described later. Based on the complementary information from the section 330, other first reaction information to be complemented is selected in order to determine the control content. For example, when the first reaction information is viscosity information, even if it is found from the viscosity measurement value that the polymerization reaction is insufficient, it is not known which of the first solution A1 and the second solution A2 should be increased. In some cases. The selection unit 220 selects other first reaction information to be complemented with the viscosity information based on the complementary information.

The instruction unit 230 controls the supply of the first supply pump 15 and/or the second supply pump 16 based on control information from the control information storage unit 350, which will be described later. The instruction unit 230 acquires control information, which is the control content stored in the control information storage unit 350 based on the information from the determination unit 210 and the selection unit 220 . Then, the instruction unit 230 controls the first supply pump 15 and/or the second supply pump 16 based on the acquired control information.

Subsequently, the first storage unit 300 has a measurement interval information storage unit 310, an allowable range information storage unit 320, a complementary information storage unit 330, a priority information storage unit 340, and a control information storage unit 350. .

The measurement interval information storage unit 310 stores measurement interval information regarding intervals at which the first control unit 200 (determination unit 210) acquires the first reaction information from the first measurement unit. The measurement interval is set for each first measurement section (first reaction information). Moreover, the measurement interval is set according to the position where the first measurement unit is arranged (positions relating to upstream and downstream in the liquid feeding line L).

The allowable range information storage unit 320 stores the allowable range (for example, the range of measured values, the signal strength, etc.).

Complementary information storage unit 330 can specify first reaction information to be selected as complementary information when various first reaction information (various first measurement units) is specific first reaction information (specific measurement unit). information. Complementary information storage unit 330 associates and stores specific first reaction information and first reaction information to be complemented. The complementary information storage unit 330 stores, for example, information for complementing predetermined first reaction information with respect to viscosity information.

When the determination unit 210 determines that a plurality of pieces of first reaction information (first measurement units) are outside the allowable range, the priority information storage unit 340 stores information about the first reaction information to be prioritized (for example, priority ranking information). The priority information storage unit 340 stores, for example, information indicating that the viscosity information is given priority.

The control information storage unit 350 stores information about the control content corresponding to the content of the first reaction information determined to be out of the allowable range. The control information storage unit 350 stores, for example, control information for increasing/decreasing the supply amount of the first supply pump 15 and/or the second supply pump 16 .

Next, operation of the polymer manufacturing system 1 in the first embodiment will be described with reference to FIG. Here, control using viscosity information as the first reaction information is described.
As shown in FIG. 3, in step ST201, determination section 210 acquires viscosity information, which is first reaction information, from first viscosity measurement section 111, which is the first measurement section.

Next, in step ST202, determination section 210 determines whether or not the obtained viscosity information is within a predetermined allowable range based on the allowable range information stored in allowable range information storage section 320. FIG.
Then, when determining that the viscosity information (viscosity value) is within the predetermined range (YES), the determination section 210 does not change the supply amount of the second supply pump 16 (step ST203).
If determination section 210 determines that the viscosity information (viscosity value) is not within the predetermined range (NO), the process proceeds to step ST204.

Next, in step ST204, the selection section 220 acquires complementary information, which is information related to the first reaction information (type) that complements the viscosity information, from the complementary information storage section 330. FIG.

Next, in step ST205, instruction section 230 acquires control information such as control conditions from control information storage section 350 based on the content of the viscosity information and the content of the first reaction information specified by the complementary information.
The instruction unit 230 then controls the second supply pump 16 based on the acquired control information. If the content of the control is to increase (increase) the supply amount of the second supply pump 16, the instruction unit 230 controls the second supply pump 16 to increase the supply amount (step ST206).
If the content of the control is to decrease the supply amount of the second supply pump 16 (decrease), the instruction section 230 controls the second supply pump 16 to decrease the supply amount (step ST207).

Next, first control section 200 enters a standby state (step ST208). Here, based on the measurement interval information stored in the measurement interval information storage unit 310, the first control unit 200 acquires viscosity information from the first viscosity measurement unit 111 at predetermined intervals.

Next, another operation of the polymer production system 1 in the first embodiment will be described with reference to FIG. Here, control using a plurality of pieces of first reaction information is described.
As shown in FIG. 4, in step ST251, determination section 210 acquires first reaction information from each measurement section of the first measurement section group.

Next, in step ST252, determination section 210 determines whether or not all acquired first reaction information is within a predetermined tolerance range based on the tolerance information stored in tolerance information storage section 320. .
Then, when determining that all the first reaction information are within the predetermined range (YES), the determination section 210 does not change the supply amount of the second supply pump 16 (step ST253).
If determining section 210 determines that not all of the first reaction information is within the predetermined range (one or more first reaction information is outside the predetermined range) (NO), the process proceeds to step ST254. .

Next, in step ST254, when there is a plurality of pieces of first reaction information outside the predetermined range (YES), determination section 210 advances the process to step ST255. If there is not a plurality of pieces of first reaction information outside the predetermined range (NO), determination unit 210 advances the process to step 256 .

Next, in step ST255, the selection section 220 selects first reaction information (type) with high priority based on the priority information recorded in the priority information storage section 340. FIG.

Next, in step ST256, instruction section 230 acquires control information such as control conditions from control information storage section 350 based on the content of the first reaction information that is outside the predetermined range.
The instruction unit 230 then controls the second supply pump 16 based on the acquired control information. If the content of the control is to increase (increase) the supply amount of the second supply pump 16, the instruction unit 230 controls the second supply pump 16 to increase the supply amount (step ST257).
If the content of control is to decrease the supply amount of the second supply pump 16 (decrease), the instruction section 230 controls the second supply pump 16 to decrease the supply amount (step ST258).

Next, first control section 200 enters a standby state (step ST259). Here, based on the measurement interval information stored in the measurement interval information storage unit 310, the first control unit 200 acquires first reaction information from each measurement unit of the first measurement unit group at predetermined intervals.

According to the polymer production system 1 of this embodiment, the following effects are obtained.
The polymer production system 1 includes a first measurement unit that acquires one or more first reaction information related to the physical quantity and / or composition of the first measurement object, and the first reaction information acquired by the first measurement unit. and a first control unit 200 that controls supply in the first supply pump 15 and/or the second supply pump 16 . Then, the polymer production system 1 causes the first supply pump 15 and/or the second supply pump 16 to supply the desired polymer based on the first reaction information acquired by the first measurement unit. controlling.

According to such a polymer production system 1, it is possible to obtain a desired polymer continuously and stably. Moreover, according to the polymer production system 1, the spec out rate can be reduced in the continuous polymer production.

Further, in the polymer production system 1, the first measurement unit includes a viscometer, a pressure gauge, a pump pressure gauge, an absorbance meter, an infrared spectrometer, a near-infrared spectrometer, a density meter, a color difference meter, a refractometer, and a spectrophotometer. meter, conductivity meter, turbidimeter, and fluorescent X-ray analyzer. Thereby, the polymer production system 1 can control the supply in the first supply pump 15 and/or the second supply pump 16 based on the plurality of types of first reaction information acquired by the plurality of types of first measurement units. Therefore, the polymerization reaction can be adjusted more appropriately.

In this embodiment, one of the first polymerizable compound and the second polymerizable compound is a tetracarboxylic dianhydride and the other is a diamine, and the case of producing a polyamic acid as the first polymer has been described. However, it is not limited to this. For example, among the first polymerizable compound and the second polymerizable compound, one is an acid anhydride group-terminated or amino group-terminated polyamic acid (prepolymer), the other is a diamine or tetracarboxylic dianhydride, and the first polymer A polyamic acid may be produced as a coalescence. In this case, one of the first polymerizable compound and the second polymerizable compound is an acid anhydride group-terminated polyamic acid, and the other is a diamine. Further, when one of the first polymerizable compound and the second polymerizable compound is an amino group-terminated polyamic acid, the other is a tetracarboxylic dianhydride.

Further, in the present embodiment, the case where the fourth liquid feeding part L4 is arranged in the first temperature control tank 39 in order to control the temperature of the first mixed solution B to the desired temperature condition has been described, but the present invention is not limited to this. not something. For example, the fourth liquid feeding part L4 may be configured with a double pipe.

In addition, in the present embodiment, the case where the first tank 11 and the second tank 12 to the first cushion tank 40 are connected in a sealed state by the tubular liquid feeding line L has been described, but it is not limited to this. Absent. For example, in order to suppress the generation of air bubbles in the first polymerization solution C, at least the first mixing stirring unit 25 and the first reaction stirring unit 35 should be able to stir the solution without contacting gas. good. However, it is preferable that the solution does not contact the gas in the entirety of the first mixing section 20 and the first reaction section 30, and it is more preferable that the solution does not contact the gas in the entire liquid feeding line L as described above.

<Second embodiment>
Next, a polymer manufacturing system according to a second embodiment will be described with reference to FIGS. 5 to 8. FIG. FIG. 5 is a diagram showing a polymer production system in the second embodiment. FIG. 6 is a block diagram of a polymer production system in the second embodiment. FIG. 7 is a flowchart explaining the operation of the polymer production system in the second embodiment. FIG. 8 is a flowchart explaining another operation of the polymer production system in the second embodiment. The second embodiment is an example of a polymer production system having two stages of processing sections (reaction sections).

First, a polymer production system 1A in the second embodiment will be described with reference to FIG.
As shown in FIG. 5, the polymer manufacturing system 1A has a first processing section K1 and a second processing section K2.

Since the first processing unit K1 has the same configuration as the polymer production system 1 in the first embodiment, detailed description in this embodiment is omitted. The description in the first embodiment can be used for the configuration requirements, operation, and the like in the first processing unit K1. However, the first polymerization solution C produced in the first processing section K1 contains an acid anhydride group-terminated or amino group-terminated polyamic acid (prepolymer) as the first polymer.

The second processing section K2 uses the first polymerization solution C produced by the first processing section K1 (the polymer production system 1 in the first embodiment) and the third solution A3 as raw materials to further progress the polymerization reaction, A polyamic acid (second polymer) is produced. The second processing section K2 has the same basic configuration as the first processing section K1, but uses the first polymerization solution C produced by the first processing section K1 as a raw material to produce polyamic acid (second polymer). It is different from the first processing unit K1 in that

The second processing section K2 includes a third tank 13, a third supply pump 17 (third supply section), a second mixing section 50, a second reaction section 60, a second cushion tank 70, and a liquid feeding line. and a portion of L. A part of the liquid feeding line L described above has a sixth liquid feeding section L6, a seventh liquid feeding section L7, an eighth liquid feeding section L8, and a ninth liquid feeding section L9. Here, the seventh liquid feeding section L7 constitutes the second mixing section 50. As shown in FIG. In addition, the eighth liquid feeding section L8 constitutes the second reaction section 60 .

The third tank 13 contains a third solution A3 containing a polyaddition third polymerizable compound that polyadditions to the first polymer contained in the first polymerization solution C. As shown in FIG. In the case of the present embodiment, the third tank 13 is a third solution in which a diamine or a tetracarboxylic dianhydride that polyadds to an acid anhydride group-terminated or amino group-terminated polyamic acid contained in the first polymerization solution C is dissolved. Accommodates A3.

As an example, the case where the first polymerization solution C contains an acid anhydride group-terminated polyamic acid and the third solution A3 contains a diamine will be described below.

The third supply pump 17 (third supply section) supplies the third solution A3 contained in the third tank 13 to the second mixing section 50 . The third supply pump 17 supplies a predetermined amount of the third solution A3. For example, the third supply pump 17 is adjusted so as to supply the third solution A3 under conditions under which polyamic acid (second polymer) with desired properties is obtained. The amount supplied by the third supply pump 17 can be set according to the properties and composition of the first polymerization solution C. Further, the supply amount of the third supply pump 17 can be set according to the reaction rate of the first polymerization solution C and the like. In other words, the supply amount of the third supply pump 17 can be adjusted to a supply amount that achieves the target properties, composition and reaction rate.

The second mixing section 50 mixes the first polymerization solution C from the first reaction section 30 and the third solution A3 from the third supply pump 17 to generate the second mixed solution D. The second mixing section 50 is arranged downstream of the third supply pump 17 . The second mixing section 50 has a second confluence valve 51 and a second mixing stirring section 55 . The second mixing section 50 also has a seventh liquid feeding section L7.

The second confluence valve 51 merges the first polymerization solution C from the first reaction section 30 and the third solution A3 from the third supply pump 17 . The second confluence valve 51 mixes the first polymerization solution C and the third solution A3.

The second mixing/stirring unit 55 stirs the second mixed solution D in which the first polymerization solution C and the third solution A3 are mixed without coming into contact with gas. The second mixing/stirring unit 55 is arranged inside the pipe that constitutes the seventh liquid feeding unit L7, or is configured to constitute the seventh liquid feeding unit L7.

The second mixing and stirring unit 55 includes, for example, a stationary mixer such as a static mixer, a nozzle, orifice, a centrifugal pump, a centrifugal pump, a driven mixer such as an inline mixer having stirring blades, preferably It comprises a static mixer, more preferably a static mixer. As described above, a pipe with a twist tape inserted therein can also provide a stirring promotion effect in the same manner as a static mixer.

The static mixer is not particularly limited, and examples thereof include static mixers such as Kenics mixer type, Sulzer SMV type, Sulzer SMX type, Tray Hi-mixer type, Komax mixer type, Lightnin mixer type, Ross ISG type, and Bran & Lube mixer type. mentioned. Among these, the Kenics mixer type static mixer is more preferable since it has a simple structure and has no dead space.

Although the position of the second mixing/stirring section 55 is not particularly limited, it is preferably arranged on the second merging valve 51 side (for example, near) in the second mixing section 50, for example.

The second reaction section 60 is arranged continuously downstream of the second mixing section 50 . In the present embodiment, the second reaction section 60 comprises an acid anhydride group-terminated polyamic acid (first polymer) from the first polymerization solution C contained in the second mixed solution D, and a diamine from the third solution A3. It is a portion that advances the polymerization reaction with (the third polymerizable compound). In the second reaction section 60, the acid anhydride group-terminated polyamic acid (first polymer) from the first polymerization solution C contained in the second mixed solution D and the diamine (third polymerizable compound) proceeds gradually, and a second polymerization solution E is obtained.

The second reaction section 60 has an eighth liquid feeding section L8, a second reaction stirring section 65, and a second temperature control tank 69.

The eighth liquid feeding part L8 is a part from one end L8a to the other end L8b in the present embodiment. The hollow part of the pipe that constitutes the eighth liquid feeding part L8 has, for example, a cross-sectional area of 1 mm ² or more and 400 cm ² or less, but is not limited to this. The eighth liquid feeding section L8 has a third reaction adjustment section 62 and a fourth reaction adjustment section 67 .

The third reaction adjustment section 62 is a piping section arranged upstream of the second reaction stirring section 65 . The third reaction adjusting section 62 is formed so that the second mixed solution D flows for a desired residence time. The third reaction adjustment section 62 is arranged in the second temperature control tank 69 and is temperature-controlled (for example, cooled) to a desired temperature condition. In the third reaction adjusting section 62 , the second mixed solution D is adjusted to a temperature suitable for the polymerization reaction and sent to the second reaction stirring section 65 .

The fourth reaction adjustment section 67 is a piping section arranged downstream of the second reaction stirring section 65 . The fourth reaction adjusting section 67 is formed so that the second mixed solution D flows for a desired residence time. The fourth reaction adjustment section 67 is arranged in the second temperature control tank 69 and is temperature-controlled (for example, cooled) to a desired temperature condition. In the fourth reaction adjusting section 67, the second mixed solution D stirred by the second reaction stirring section 65, which will be described later, is adjusted to a temperature suitable for the polymerization reaction and fed.

In FIG. 5, the structure of the third reaction adjustment section 62 and the fourth reaction adjustment section 67 is shown as a helical tube, but as long as a sufficient residence time is ensured, any structure such as a straight tube or a curved tube may be used. can do.

The second reaction stirring section 65 stirs the second mixed solution D sent from the third reaction adjusting section 62 without contacting the gas. In the present embodiment, the second reaction stirring section 65 stirs the second mixed solution D adjusted to a temperature suitable for the polymerization reaction by the third reaction adjusting section 62 without coming into contact with gas.

As described above, the second reaction-stirring unit 65 includes, for example, static mixers such as static mixers, nozzles, and orifices, and drive-type mixers such as centrifugal pumps, vortex pumps, and in-line mixers having stirring blades. preferably includes a static mixer, more preferably includes a static mixer. As described above, a pipe with a twist tape inserted therein can also provide a stirring promotion effect in the same manner as a static mixer.

The static mixer is not particularly limited, and examples thereof include static mixers such as Kenics mixer type, Sulzer SMV type, Sulzer SMX type, Tray Hi-mixer type, Komax mixer type, Lightnin mixer type, Ross ISG type, and Bran & Lube mixer type. mentioned. Among these, the Kenics mixer type static mixer is more preferable since it has a simple structure and has no dead space.

Although the position of the second reaction stirring section 65 is not particularly limited, it is preferably arranged in the middle of the second reaction section 60, for example.

The second cushion tank 70 accommodates the second polymerization solution E from the second reaction section 60 . The second cushion tank 70 serves as a tank for containing a raw material solution, for example, when polyimide is produced by imidating polyamic acid, which is the second polymer.

When the polymer manufacturing system 1A according to the present embodiment manufactures polyimide, the polymer manufacturing system 1A further includes an imidization unit that imidizes the polyamic acid. The imidization unit (not shown) imidizes the polyamic acid by, for example, a thermal imidization method of thermal dehydration ring closure, a chemical imidization method using a dehydrating agent and an imidization accelerator, or the like.

When the polymer manufacturing system 1A manufactures polyimide, the second cushion tank 70 may be omitted and the liquid may be fed from the ninth liquid feeder L9 to the imidization section. However, as described above, it is preferable to temporarily store the polyamic acid in the second cushion tank 70 .

In addition to the above-described first measurement unit, the polymer production system 1A includes any one or more of the first polymerization solution C, the third solution A3, the second mixed solution D, and the second polymerization solution E (hereinafter, " a second measurement unit that acquires one or more second reaction information relating to the physical quantity and/or the composition of the second measurement object"). In this embodiment, the polymer production system 1A has a plurality of second measurement units. More specifically, the polymer production system 1A includes third differential pressure measurement units 95 and 96, fourth differential pressure measurement units 97 and 98, a second viscosity measurement unit 112, and a first absorbance measurement unit 101. , and a second absorbance measuring unit 102 .

The third differential pressure measurement units 95 and 96 acquire information on the input/output differential pressure (the differential pressure between the upstream side and the downstream side) in the second mixing/stirring unit 55 as second reaction information.
The fourth differential pressure measurement units 97 and 98 acquire information on the input/output differential pressure (differential pressure between upstream and downstream sides) in the second reaction unit 60 as second reaction information.

The second viscosity measurement unit 112 acquires viscosity information of the second polymerization solution E as second reaction information. Viscosity information is effective information as the second reaction information because the viscosity increases as the polymerization reaction progresses.

The first absorbance measuring unit 101 acquires information about the absorbance of the first polymerization solution C at a specific wavelength as second reaction information.
The second absorbance measuring unit 102 acquires information about the absorbance of the second polymerization solution E at a specific wavelength as second reaction information.
Here, the absorbance difference can be calculated from the absorbance information acquired by the first absorbance measurement unit 101 and the absorbance information acquired by the second absorbance measurement unit 102 .

The second measurement unit is not limited to the measurement unit (type of physical quantity and/or composition, measurement method) of this embodiment. The second measurement unit includes, for example, a viscometer, a pressure gauge, a pump pressure gauge, an absorbance meter, an infrared spectrometer, a near-infrared spectrometer, a density meter, a color difference meter, a refractometer, a spectrophotometer, a conductivity meter, a turbidity It comprises one or more selected from the group consisting of a photometer and a fluorescent X-ray spectrometer.

The second measurement unit acquires one or more pieces of second reaction information relating to the physical quantity and/or composition of the second measurement object, and outputs the acquired second reaction information to the second control unit 200A, which will be described later.

Next, a block diagram of the polymer production system 1A in the second embodiment will be described with reference to FIG. Here, configurations different from those of the first embodiment will be mainly described, and descriptions of configurations similar to those of the first embodiment will be omitted.

As shown in FIG. 6, the polymer production system 1A includes a plurality of first measurement units (first measurement unit group), a plurality of second measurement units (second measurement unit group), and a second control unit 200A. , a second storage unit 300A, and the first supply pump 15, the second supply pump 16, and the third supply pump 17, which are the objects to be controlled.

The second measurement unit acquires one or more pieces of second reaction information regarding the physical quantity and/or composition of the second measurement object, as described above. The polymer production system 1A has a plurality of second measurement units. More specifically, the polymer production system 1A includes third differential pressure measurement units 95 and 96, fourth differential pressure measurement units 97 and 98, a second viscosity measurement unit 112, and a first absorbance measurement unit 101. , and a second absorbance measuring unit 102 .
Here, the second reaction information includes numerical information such as measured values of physical quantity and/or composition, as well as electrical signals that change corresponding to physical quantity and/or composition.

The second control section 200A controls the supply of the third supply pump 17 based on the first reaction information acquired by the first measurement section and/or the second reaction information acquired by the second measurement section. Here, since the second control unit 200A also has the function of the first control unit, based on the first reaction information acquired by the first measurement unit, the first supply pump 15 and/or the second supply pump 16 The supply is configured to be controllable. Hereinafter, components having the same names as in the first embodiment have the functions described in the first embodiment in addition to the functions described below in the present embodiment.

The second control unit 200A has a determination unit 210A, a selection unit 220A, and an instruction unit 230A.

Based on the first reaction information and/or the second reaction information, the determination unit 210A determines whether the physical quantity and/or the composition of the first measurement object and/or the second measurement object are within a predetermined allowable range. determine whether or not The determination unit 210A acquires the first reaction information and/or the second reaction information from the first measurement unit and/or the second measurement unit based on the measurement interval stored in the measurement interval information storage unit 310A, which will be described later, and Based on the allowable range information stored in the allowable range information storage unit 320A, which will be described later, it is determined whether or not the obtained first reaction information and/or the second reaction information are within a predetermined allowable range.

If there are a plurality of pieces of first reaction information and/or second reaction information determined by the determination unit 210A to be outside the allowable range, the selection unit 220A, based on the priority information from the priority information storage unit 340A, which will be described later, Select the first reaction information and/or the second reaction information with priority in control.

Further, when the first reaction information and/or the second reaction information determined by the determination unit 210A to be out of the allowable range are specific information, the selection unit 220A selects, for example, the first reaction information and/or the second reaction information When the reaction information is viscosity information, other first reaction information and/or second reaction information to be complemented to determine the control content is selected based on the complementary information from the complementary information storage unit 330A, which will be described later. . For example, when the first reaction information and/or the second reaction information is viscosity information, even if it is found that the polymerization reaction is insufficient from the viscosity measurement value, either the first polymerization solution C or the third solution A3 In some cases, it may not be known whether to increase The selection unit 220A selects other first reaction information and/or second reaction information to be complemented with the viscosity information based on the complementary information.

The instruction unit 230A controls the supply of the third supply pump 17 based on control information from a control information storage unit 350A, which will be described later. The instruction unit 230A acquires control information, which is the control content stored in the control information storage unit 350A, based on the information from the determination unit 210A and the selection unit 220A. The instruction unit 230A then controls the third supply pump 17 based on the acquired control information.

Subsequently, the second storage unit 300A has a measurement interval information storage unit 310A, an allowable range information storage unit 320A, a complementary information storage unit 330A, a priority information storage unit 340A, and a control information storage unit 350A. . Hereinafter, components having the same names as in the first embodiment have the functions described in the first embodiment in addition to the functions described below in the present embodiment.

The measurement interval information storage unit 310A stores measurement intervals related to the interval at which the second control unit 200A (determination unit 210A) acquires the first reaction information from the first measurement unit and the interval at which the second reaction information is acquired from the second measurement unit. Store information. The measurement interval is set for each first measurement section (first reaction information). Moreover, the measurement interval is set according to the position where the first measurement unit is arranged (positions relating to upstream and downstream in the liquid feeding line L). Similarly, the measurement interval is set for each second measurement section (second reaction information). Also, the measurement interval is set according to the position where the second measurement unit is arranged (positions relating to upstream and downstream in the liquid feeding line L).

The allowable range information storage unit 320A stores the allowable range (for example, the range of measured values, the signal strength, etc.) is stored. In addition, the allowable range information storage unit 320A stores the allowable range (for example, the range of measured values , signal strength, etc.).

Complementary information storage unit 330A stores various first reaction information (various first measurement units) and/or various second reaction information (various second measurement units) as specific first reaction information (specific measurement units) and/or In the case of specific second reaction information (specific measurement part), information that can specify the first reaction information and/or the second reaction information to be selected as complementary information is stored. The complementary information storage unit 330A associates and stores specific first reaction information and/or second reaction information with first reaction information and/or second reaction information to be complemented. The complementary information storage unit 330A stores, for example, information for complementing viscosity information with predetermined first reaction information and/or second reaction information.

When the determination unit 210A determines that a plurality of pieces of first reaction information (first measurement unit) and/or second reaction information (second measurement unit) are outside the allowable range, the priority information storage unit 340A It stores information (for example, priority order information) regarding the first reaction information and/or the second reaction information to be prioritized. The priority information storage unit 340A stores, for example, information indicating that the viscosity information is given priority.

The control information storage unit 350A stores information about the control content corresponding to the content of the first reaction information and/or the second reaction information determined to be out of the allowable range. The control information storage unit 350A stores, for example, control information for increasing/decreasing the supply amount of the third supply pump 17 .

Next, operation of the polymer production system 1A in the second embodiment will be described with reference to FIG. Here, control using viscosity information as the second reaction information is described.
As shown in FIG. 7, in step ST301, determination section 210A acquires viscosity information, which is the second reaction information, from second viscosity measurement section 112, which is the second measurement section.

Next, in step ST302, determination section 210A determines whether the acquired viscosity information is within a predetermined allowable range based on the allowable range information stored in allowable range information storage section 320A.
Then, if the determining section 210A determines that the viscosity information (viscosity value) is within the predetermined range (YES), it does not change the supply amount of the third supply pump 17 (step ST303).
If determination section 210A determines that the viscosity information (viscosity value) is not within the predetermined range (NO), the process proceeds to step ST304.

Subsequently, in step ST304, the selection section 220A acquires complementary information, which is information related to the first reaction information (type) and/or the second reaction information (type) that complements the viscosity information, from the complementary information storage section 330A.

Subsequently, in step ST305, the instruction unit 230A selects the control conditions from the control information storage unit 350A based on the content of the viscosity information and the content of the first reaction information and/or the second reaction information specified by the complementary information. Acquire control information such as
The instruction unit 230A then controls the third supply pump 17 based on the acquired control information. If the content of the control is to increase (increase) the supply amount of the third supply pump 17, the instruction section 230A controls the third supply pump 17 to increase the supply amount (step ST306).
If the content of control is to decrease the supply amount of the third supply pump 17 (decrease), the instruction section 230A controls the third supply pump 17 to decrease the supply amount (step ST307).

Subsequently, second control section 200A enters a standby state (step ST308). Here, the second control unit 200A acquires viscosity information from the second viscosity measuring unit 112 at predetermined intervals based on the measurement interval information stored in the measurement interval information storage unit 310A.

Next, another operation of the polymer production system 1A in the second embodiment will be described with reference to FIG. Here, control using a plurality of pieces of first reaction information and second reaction information is described.
As shown in FIG. 8, in step ST351, determination section 210A acquires the first reaction information from each measurement section of the first measurement section group, and obtains the second reaction information from each measurement section of the second measurement section group. Get information.

Next, in step ST352, determination section 210A determines whether all of the obtained first reaction information and second reaction information are within a predetermined allowable range based on the allowable range information stored in allowable range information storage section 320. determine whether or not
Then, when determining that all the first reaction information and the second reaction information are within the predetermined range (YES), the determining section 210A does not change the supply amount of the third supply pump 17 (step ST353).
Further, if the determination unit 210A determines that all the first reaction information and the second reaction information are not within the predetermined range (one or more reaction information is outside the predetermined range) (NO), the process is stepped. Proceed to ST354.

Next, in step ST354, determination section 210A advances the process to step ST355 when there is a plurality of pieces of reaction information outside the predetermined range (YES). If there is not a plurality of pieces of reaction information outside the predetermined range (NO), determination unit 210A advances the process to step 356 .

Next, in step ST355, the selection section 220A selects the first reaction information (type) and/or the second reaction information (type) with high priority based on the priority information.

Next, in step ST356, the instruction section 230A acquires control information such as control conditions from the control information storage section 350A based on the content of the reaction information outside the predetermined range.
The instruction unit 230A then controls the third supply pump 17 based on the acquired control information. If the content of the control is to increase (increase) the supply amount of the third supply pump 17, the instruction unit 230A controls the third supply pump 17 to increase the supply amount (step ST357).
If the content of the control is to decrease the supply amount of the third supply pump 17 (decrease), the instruction section 230A controls the third supply pump 17 to decrease the supply amount (step ST358).

Next, second control section 200A enters a standby state (step ST359). Here, based on the measurement interval information stored in the measurement interval information storage unit 310A, the second control unit 200A outputs the first reaction information from each first measurement unit and the second reaction information from each second measurement unit at predetermined intervals. 2 Get reaction information.

According to the polymer production system 1A of the present embodiment, the following effects are obtained in addition to the effects of the above-described first embodiment.
The polymer production system 1A includes a second measurement unit that acquires one or more second reaction information related to the physical quantity and / or composition of the second measurement object, and the first reaction information acquired by the first measurement unit and / Alternatively, a second control section for controlling supply by the third supply pump 17 based on the second reaction information acquired by the second measurement section is further provided.

According to such a polymer production system 1A, it is possible to obtain a desired polymer continuously and stably. Moreover, according to the polymer production system 1A, the spec out rate can be reduced in continuous polymer production.

Further, in the polymer production system 1A, the second measurement unit includes a viscometer, a pressure gauge, a pump pressure gauge, an absorbance meter, an infrared spectrometer, a near-infrared spectrometer, a density meter, a color difference meter, a refractometer, and a spectrophotometer. meter, conductivity meter, turbidimeter, and fluorescent X-ray analyzer. As a result, the polymer production system 1A can obtain multiple types of first reaction information acquired by multiple types of first measurement units and/or multiple types of second reaction information acquired by multiple types of second measurement units. Based on this, the supply from the third supply pump 17 can be controlled, so that the polymerization reaction can be adjusted more appropriately.

In the present embodiment, the case where the eighth liquid feeding part L8 is arranged in the second temperature control tank 69 in order to control the temperature of the second mixed solution D to the desired temperature condition has been described, but the present invention is not limited to this. not something. For example, the eighth liquid feeding part L8 may be configured with a double pipe.

Further, in the present embodiment, the case where the first tank 11 and the second tank 12 to the second cushion tank 70 are connected in a sealed state by the tubular liquid feeding line L has been described, but it is not limited to this. Absent. For example, in order to suppress the generation of bubbles in the second polymerization solution E, at least the first mixing/stirring unit 25, the first reaction/stirring unit 35, the second mixing/stirring unit 55, and the second reaction/stirring unit 65 are Anything that can stir the solution without coming into contact with gas may be used. However, it is preferable that the solution does not come into contact with the gas in the entirety of the first mixing section 20, the first reaction section 30, the second mixing section 50, and the second reaction section 60. More preferably, the solution does not come into contact with gas.

<Specific example of control>
Specific examples of control in the polymer production system 1 and the polymer production system 1A will be described below. However, it is not limited to the following specific examples.

(1) Example 1
Assume that the viscosity of the first polymerization solution C at the outlet of the first reaction section 30 is lower than the set value. An in-line viscometer is installed at the outlet of the first reaction section 30 to acquire viscosity information of the first polymerization solution C over time. In order to increase the viscosity, the flow ratio should be controlled so that the tetracarboxylic dianhydride/diamine ratio approaches the equivalence ratio.

(2) Example 2
Assume that the viscosity of the first polymerization solution C at the outlet of the first reaction section 30 is lower than the set value. Two pressure gauges are installed near the outlet of the first reaction section 30, and the viscosity information of the first polymerization solution C is acquired over time using the differential pressure. In order to increase the viscosity, the flow ratio should be controlled so that the tetracarboxylic dianhydride/diamine ratio approaches the equivalence ratio.

(3) Example 3
Assume that the viscosity of the first polymerization solution C at the outlet of the first reaction section 30 is lower than the set value. An in-line viscometer is installed at the outlet of the first reaction section 30 to acquire viscosity information of the first polymerization solution C over time. Further, an in-line absorbance meter is installed at the outlet of the first reaction section 30 to acquire absorbance information of the first polymerization solution C over time. Based on the absorbance information detected when there is an excess monomer, it is determined which of the tetracarboxylic dianhydride and the diamine is excess. In order to increase the viscosity, the flow ratio should be controlled so that the tetracarboxylic dianhydride/diamine ratio approaches the equivalence ratio.

(4) Example 4
Assume that the viscosity of the first polymerization solution C at the outlet of the first reaction section 30 is lower than the set value. An in-line viscometer is installed at the outlet of the first reaction section 30 to acquire viscosity information of the first polymerization solution C over time. Furthermore, an in-line infrared spectrometer is installed at the outlet of the first reaction section 30 to obtain infrared spectral information of the first polymerization solution C over time. Based on the infrared spectroscopy information detected when there is an excess monomer, it is determined which of the tetracarboxylic dianhydride and the diamine is excess. In order to increase the viscosity, the flow ratio should be controlled so that the tetracarboxylic dianhydride/diamine ratio approaches the equivalence ratio.

(5) Example 5
Assume that the viscosity of the first polymerization solution C at the outlet of the first reaction section 30 is lower than the set value. Two pressure gauges are installed near the outlet of the first reaction section 30, and the viscosity information of the first polymerization solution C is acquired over time using the differential pressure. Further, an in-line absorbance meter is installed at the outlet of the first reaction section 30 to acquire absorbance information of the first polymerization solution C over time. Based on the absorbance information detected when there is an excess monomer, it is determined which of the tetracarboxylic dianhydride and the diamine is excess. In order to increase the viscosity, the flow ratio should be controlled so that the tetracarboxylic dianhydride/diamine ratio approaches the equivalence ratio.

(6) Example 6
Assume that the viscosity of the first polymerization solution C at the outlet of the first reaction section 30 is lower than the set value. Two pressure gauges are installed near the outlet of the first reaction section 30, and the viscosity information of the first polymerization solution C is acquired over time using the differential pressure. Furthermore, an in-line infrared spectrometer is installed at the outlet of the first reaction section 30 to obtain infrared spectral information of the first polymerization solution C over time. Based on the absorbance information detected when there is an excess monomer, it is determined which of the tetracarboxylic dianhydride and the diamine is excess. In order to increase the viscosity, the flow ratio should be controlled so that the tetracarboxylic dianhydride/diamine ratio approaches the equivalence ratio.

(7) Example 7
Assume that the viscosity of the first polymerization solution C at the outlet of the first reaction section 30 is lower than the set value. An in-line viscometer is installed at the outlet of the first reaction section 30 to acquire viscosity information of the first polymerization solution C over time. Next, decrease the flow rate of either the first solution A1 or the second solution A2, and check whether the viscosity increases or decreases. Then, the correlation between increase/decrease in flow rate and increase/decrease in viscosity is confirmed, and the flow ratio is controlled in the direction of increasing viscosity.

(8) Example 8
A calibration curve is prepared for the viscosity of the polyamic acid solution as the first solution A1 and the tetracarboxylic dianhydride/diamine ratio in the first solution A1. If the tetracarboxylic dianhydride/diamine ratio that provides the desired viscosity is obtained in advance, the amount of the second solution A2 to be added to the first solution A1 can be calculated. An in-line viscometer is installed at the outlet of the first supply pump 15 to obtain viscosity information of the first solution A1 over time. Using the obtained viscosity information of the first solution A1, the addition amount of the second solution A2 necessary for the viscosity at the outlet of the first reaction unit 30 to reach the set viscosity is calculated, and to control the supply amount of the second solution A2.

(9) Example 9
Assume that the viscosity of the second polymerization solution E at the outlet of the second reaction section 60 is lower than the set value. An in-line viscometer is installed at the outlet of the second reaction section 40 to acquire viscosity information of the second polymerization solution E over time. Further, an in-line absorbance meter is installed at the outlet of the second reaction section 60 to obtain absorbance information of the second polymerization solution E over time. Further, an in-line viscometer is installed at the outlet of the first reaction section 30 to acquire viscosity information of the first polymerization solution C over time. Further, an in-line absorbance meter is installed at the outlet of the first reaction section 30 to acquire absorbance information of the first polymerization solution C over time.

When the viscosity of the first polymerization solution C at the outlet of the first reaction unit 30 deviates from the set value, based on the absorbance information detected when there is an excess monomer, tetracarboxylic dianhydride and Determine which is excess with the diamine. Then, the flow rate of the second solution A2 may be controlled so as to approach the tetracarboxylic dianhydride/diamine ratio at which the viscosity of the first polymerization solution C reaches a set value.
On the other hand, when the viscosity of the first polymerization solution C at the outlet of the first reaction unit 30 indicates the set value, based on the absorbance information detected when there is an excess monomer, tetracarboxylic dianhydride and diamine is excessive. Then, the flow rate of the third solution A3 may be controlled so that the viscosity of the second polymerization solution E approaches the tetracarboxylic dianhydride/diamine ratio at the set value.

<Modification>
Although the two embodiments have been described above, the present invention is not limited to the above embodiments, and includes modifications, improvements, etc. within the scope of achieving the object of the present invention.

For example, in the above-described embodiments, the polymer production system is configured to have one or two reaction units (treatment units), but is not limited to this, and may include three or more reaction units (treatment units). part). That is, the polymer production system is not limited to one that performs one-stage or two-stage reactions, and may be one that performs three or more stages of reactions. For example, the polymer production system may be configured to have three or more sets of a mixing section having a mixing stirring section and a reaction section having a reaction stirring section. The polymer production system can adjust the amount of supply and the like in a multi-step manner so as to approach the target reaction rate and quality each time it passes through each reaction section (treatment section).

Also, in the above-described embodiments, the polymer production system for producing polyamic acid or polyimide was described, but the polymer to be produced is not limited to these. For example, the polymer production system may produce polymers using polyaddition monomers such as urethane monomers and epoxy monomers.

Further, in the polymer production system, the first solution A1 and/or the second solution A2 may contain a filler. By adding a filler to the first solution A1 and/or the second solution A2, it is possible to easily introduce the filler into the produced polymer.

EXAMPLES The present invention will be specifically described below with reference to Examples, but the present invention is not limited to these Examples.

<Example 1>
In Example 1, polyamic acid was produced using the polymer production system 1 having the structure as shown in FIG. In the first tank 11, a first solution of acid anhydride group-terminated polyamic acid obtained by the reaction of 4,4′-diaminodiphenyl ether and pyromellitic dianhydride dissolved in N,N-dimethylformamide. Housed A1. Further, the second tank 12 contained a second solution A2 in which p-phenylenediamine was dissolved in N,N-dimethylformamide. An in-line absorbance meter was installed as the first viscosity measurement unit 111 .

First, in the first mixing section 20, the first solution A1 supplied by the first supply pump 15 and the second solution A2 supplied by the second supply pump 16 were mixed to generate the first mixed solution B. . Next, in the first reaction section 30, the first mixed solution B was stirred by a Kenics mixer type static mixer without coming into contact with gas, thereby generating the first polymerization solution C in which the polyamic acid was dissolved.

The absorbance A of the solution is represented by the following formula (1) according to the Lambert-Beer law.
A=εcl (1)
where ε is the molar extinction coefficient, c is the molar concentration of the sample, and l is the optical path length. As a result of previously measuring the absorbance of a polymerization solution obtained from a predetermined polymerization recipe off-line, it was found that there is a predetermined relationship between absorbance and viscosity. Specifically, the viscosity increases as the absorbance at a wavelength of 490 nm decreases. When the target viscosity is 3200 poise, the absorbance should be 0.178. Since measurement information with an absorbance of 0.199 (converted viscosity: 2100 poise) was obtained during the feeding of the first solution A1 and the second solution A2, the flow ratio was changed so that the second solution A2 increased, Absorbance was adjusted to 0.178. As a result, the viscosity of the first polymerization solution C was 3200 poise. No air bubbles were observed in the first polymerization solution C obtained.

<Example 2>
In Example 2, polyamic acid was produced using the polymer production system 1 having the structure as shown in FIG. In the first tank 11, a first solution of acid anhydride group-terminated polyamic acid obtained by the reaction of 4,4′-diaminodiphenyl ether and pyromellitic dianhydride dissolved in N,N-dimethylformamide. Housed A1. Further, the second tank 12 contained a second solution A2 in which p-phenylenediamine was dissolved in N,N-dimethylformamide. Also, two pressure gauges were installed as the second differential pressure measuring units 93 and 94 .

First, in the first mixing section 20, the first solution A1 supplied by the first supply pump 15 and the second solution A2 supplied by the second supply pump 16 were mixed to generate the first mixed solution B. . Next, in the first reaction section 30, the first mixed solution B was stirred by a Kenics mixer type static mixer without coming into contact with gas, thereby generating the first polymerization solution C in which the polyamic acid was dissolved.

The pressure loss ΔP in a circular tube of a solution flowing in a laminar flow can be obtained from the Hagen-Poiseuille formula shown in the following formula (2).
ΔP=32 μLu/D ² (2)
Here, μ is the viscosity of the solution, L is the tube length (distance between two pressure gauges), u is the tube cross-sectional average flow velocity of the solution, and D is the tube diameter. Since the values of ΔP, L, u, and D can be obtained, the relationship between the differential pressure and the viscosity of the solution can be obtained using the above equation (2). At this time, the distance between the two points at which the differential pressure is measured should be determined in consideration of the pressure measurement accuracy. As a result of confirming the relationship between differential pressure and viscosity in advance, it was found that viscosity increases linearly as the measured value of differential pressure decreases. When the target viscosity is 1500 poise, the differential pressure should be 0.6 MPa. Since the measurement information that the differential pressure was 0.4 MPa (converted viscosity: 600 poise) was obtained during the feeding of the first solution A1 and the second solution A2, the flow ratio was changed so that the second solution A2 increased. , the differential pressure was adjusted to 0.6 MPa. As a result, the viscosity of the first polymerization solution C was 1500 poise. No air bubbles were observed in the first polymerization solution C obtained.

Reference Signs List 1, 1A polymer manufacturing system 11 first tank 12 second tank 13 third tank 15 first supply pump (first supply section)
16 second supply pump (second supply unit)
17 Third supply pump (third supply unit)
20 first mixing section 30 first reaction section 40 first cushion tank 50 second mixing section 60 second reaction section 70 second cushion tank 81 pump pressure measurement section (first measurement section)
91, 92 first differential pressure measurement unit (first measurement unit)
93, 94 second differential pressure measurement unit (first measurement unit)
95, 96 third differential pressure measurement unit (second measurement unit)
97, 98 fourth differential pressure measurement unit (second measurement unit)
111 first viscosity measurement unit (first measurement unit)
112 second viscosity measurement unit (second measurement unit)
101 first absorbance measurement unit (second measurement unit)
102 second absorbance measurement unit (second measurement unit)
200 first control unit 200A second control unit 300 first storage unit 300A second storage unit A1 first solution A2 second solution A3 third solution B first mixed solution C first polymerization solution D second mixed solution E second Polymerization solution L Liquid transfer line

Claims (10)

a first solution containing a first polyaddition polymerizable compound and a second solution containing a second polyaddition polymerizable compound that polyadditions with the first polymerizable compound as raw materials to produce a polymer; A combined manufacturing system,
a first supply unit that supplies the first solution;
a second supply unit that supplies the second solution;
a first mixing unit that mixes the first solution and the second solution to generate a first mixed solution;
It is arranged continuously downstream of the first mixing section, and includes a first polymer by advancing a polymerization reaction between the first polymerizable compound and the second polymerizable compound contained in the first mixed solution. a first reaction section that produces a first polymerization solution;
a first measurement unit that acquires first reaction information related to the viscosity of the first polymerization solution, the absorbance of the first polymerization solution, or the pressure difference between two points in the flow direction in the flow path of the first polymerization solution ;
a first control unit that controls supply in the first supply unit and/or the second supply unit based on the first reaction information acquired by the first measurement unit ;
Among the first polymerizable compound and the second polymerizable compound, one is a tetracarboxylic dianhydride and the other is a diamine, or one is an acid anhydride group-terminated or amino group-terminated polyamic acid, and the other is A diamine or a tetracarboxylic dianhydride,
A polymer production system for producing polyamic acid as the first polymer . The first measurement unit has a viscometer, acquires first viscosity information regarding the viscosity of the first polymerization solution as the first reaction information,
The weight according to claim 1 , wherein the first control unit controls supply in the first supply unit and/or the second supply unit based on the first viscosity information acquired by the first measurement unit. Combined manufacturing system. The first polymer is a polyaddition polymer,
a third supply unit that supplies a third solution containing a polyadditive third polymerizable compound that polyadditions to the first polymer;
a second mixing unit that mixes the first polymerization solution and the third solution to generate a second mixed solution;
The first polymer from the first polymerization solution and the third polymerizable compound from the third solution, which are arranged continuously downstream of the second mixing section and are contained in the second mixed solution a second reaction part that advances the polymerization reaction of to generate a second polymerization solution containing the second polymer;
a second measurement unit that acquires second reaction information related to the viscosity of the second polymerization solution, the absorbance of the second polymerization solution, or the pressure difference between two points in the flow direction of the flow path of the second polymerization solution ;
a second control unit that controls supply in the third supply unit based on the second reaction information acquired by the second measurement unit ;
The first polymer is an acid anhydride group-terminated or amino group-terminated polyamic acid,
the third polymerizable compound is a diamine or a tetracarboxylic dianhydride,
3. The polymer production system according to claim 1, wherein polyamic acid is produced as the second polymer . The second measurement unit has a viscometer, acquires second viscosity information regarding the viscosity of the second polymerization solution as the second reaction information,
The polymer production system according to claim 3 , wherein the second control section controls supply in the third supply section based on the second viscosity information acquired by the second measurement section. The polymer production system according to any one of claims 1 to 4 , further comprising an imidization unit that imidizes the produced polyamic acid. a first solution containing a first polyaddition polymerizable compound and a second solution containing a second polyaddition polymerizable compound that polyadditions with the first polymerizable compound as raw materials to produce a polymer; A method of manufacturing a coalescence,
a first supply step of supplying the first solution;
a second supply step of supplying the second solution;
a first mixing step of mixing the first solution and the second solution to generate a first mixed solution;
a first reaction step of allowing a polymerization reaction between the first polymerizable compound and the second polymerizable compound contained in the first mixed solution to generate a first polymerization solution containing the first polymer;
a first measuring step of acquiring first reaction information related to the viscosity of the first polymerization solution, the absorbance of the first polymerization solution, or the pressure difference between two points in the flow direction in the flow path of the first polymerization solution ;
a first control step of controlling supply in the first supply step and/or the second supply step based on the first reaction information acquired in the first measurement step ;
Among the first polymerizable compound and the second polymerizable compound, one is a tetracarboxylic dianhydride and the other is a diamine, or one is an acid anhydride group-terminated or amino group-terminated polyamic acid, and the other is A diamine or a tetracarboxylic dianhydride,
A method for producing a polymer in which polyamic acid is produced as the first polymer . In the first measurement step, the viscometer acquires first viscosity information about the viscosity of the first polymerization solution as the first reaction information,
7. The supply according to claim 6 , wherein in the first control step, supply in the first supply step and/or the second supply step is controlled based on the first viscosity information acquired in the first measurement step. A method for producing a polymer. The first polymer is a polyaddition polymer,
a third supplying step of supplying a third solution containing a polyadditional third polymerizable compound that polyadditions to the first polymer;
a second mixing step of mixing the first polymerization solution and the third solution to generate a second mixed solution;
The polymerization reaction between the first polymer from the first polymerization solution contained in the second mixed solution and the third polymerizable compound from the third solution is allowed to proceed to produce a second polymer containing the second polymer. a second reaction step of producing a polymerization solution;
a second measuring step of acquiring second reaction information related to the viscosity of the second polymerization solution, the absorbance of the second polymerization solution, or the pressure difference between two points in the flow direction in the flow path of the second polymerization solution ;
a second control step of controlling supply in the third supply step based on the second reaction information acquired in the second measurement step ;
The first polymer is an acid anhydride group-terminated or amino group-terminated polyamic acid,
the third polymerizable compound is a diamine or a tetracarboxylic dianhydride,
8. The method for producing a polymer according to claim 6 , wherein polyamic acid is produced as the second polymer . In the second measurement step, the viscometer acquires second viscosity information about the viscosity of the second polymerization solution as the second reaction information,
9. The method for producing a polymer according to claim 8 , wherein in the second control step, supply in the third supply step is controlled based on the second viscosity information obtained in the second measurement step. 10. The method for producing the polymer according to any one of claims 6 to 9 , further comprising an imidization step of imidizing the produced polyamic acid.

Images