JP3729834B2 - Polymer compound solution manufacturing equipment - Google Patents

Description

  The present invention relates to an apparatus for producing a polymer compound solution.

High molecular compounds are used in various fields. A polymer material such as a plastic film is produced from a solution obtained by melting a polymer compound by heating or a solution obtained by dissolving a polymer compound in a solvent. In the method using a solution, the solvent is evaporated after the polymer material is formed.
The solvent used for the polymer compound solution is a liquid that can dissolve the polymer compound at a required concentration. The solvent to be used is required to have an appropriate boiling point for safety and evaporation. In recent years, in particular, safety regarding the human body and the environment is strongly required for the solvent. For this reason, even if an attempt is made to select a solvent satisfying these requirements from a liquid capable of dissolving the polymer compound, there is a situation in which no suitable solvent is found.

For example, for cellulose triacetate, methylene chloride has been conventionally used as a solvent. However, the use of methylene chloride is greatly regulated due to problems with the human body and the global environment. Besides methylene chloride, liquids capable of dissolving cellulose triacetate (eg, epichlorohydrin, N-methylpyrrolidone, tetrahydrofuran, 1,4-dioxane, 1,3-dioxolane, nitromethane) are known. Has a high boiling point and is difficult to remove by evaporation, and there is a risk of explosion.
Acetone, which is a general-purpose organic solvent, has an appropriate boiling point (boiling point: 56 ° C.), and has less problems with respect to the human body and the global environment than other organic solvents. However, although cellulose triacetate swells with acetone, it could not be dissolved in acetone by a normal method.

For example, after cooling a cellulose acetate having a substitution degree of 2.80 (acetylation degree of 60.1%) to a substitution degree of 2.90 (acetylation degree of 61.3%) in acetone from −80 ° C. to −70 ° C. It has been reported that a dilute solution in which cellulose acetate is dissolved in acetone at 0.5 to 5% by weight by heating is obtained (for example, see Non-Patent Document 1). Hereinafter, a method for obtaining a solution by cooling a mixture of a polymer compound and a solvent and heating the mixture is referred to as a “cooling dissolution method”.
There is another paper on dissolution of cellulose acetate in acetone (see, for example, Non-Patent Document 2). This title, as its title, applies the cooling dissolution method to the technical field of spinning method. In this paper, the cooling dissolution method is examined while paying attention to the mechanical properties, dyeability and cross-sectional shape of the fibers obtained. In the method described in this article, a solution of cellulose acetate having a concentration of 10 to 25% by weight is obtained.

J. et al. M.M. G. Cowie et al., Makromol, Chem. 143, 105 (1971) Kenji Kamide et al., Dry spinning from acetone solution of cellulose triacetate, Journal of Textile Machinery Society, 34, 57-61 (1981)

In the present invention, the cooling dissolution method is improved, and a method capable of producing a polymer compound solution is realized even with a combination of a polymer compound and a solvent that swells but does not dissolve in a normal method.
And the objective of this invention is providing the manufacturing apparatus of the high molecular compound solution which can be preferably used for the cooling dissolution method.

When the manufacturing apparatus of the present invention is used, the following method (1) or (4) can be easily realized.
(1) A step of mixing a polymer compound and a solvent at −10 to 55 ° C. and swelling the polymer compound with the solvent; a step of cooling the swelling mixture to −100 to −10 ° C .; A method for producing a polymer compound solution comprising a step of heating to 0 to 55 ° C. and dissolving the polymer compound in a solvent,
In the cooling step, the swelling mixture is cooled at a rate of 1 to 40 ° C./min.
The method (1) can be carried out in the following aspects (2) or (3).
(2) The method for producing a polymer compound solution according to (1), wherein in the cooling step, the swollen mixture is stirred and conveyed in a cylindrical container, and the swollen mixture is cooled from around the container.
(3) The method for producing a polymer compound solution according to (1), wherein a solvent cooled to −105 to −15 ° C. is added to the swollen mixture in the cooling step.

(4) A step of mixing the polymer compound and the solvent at −10 to 55 ° C. and swelling the polymer compound with the solvent; a step of cooling the swelling mixture to −100 to −10 ° C .; and the cooled swelling mixture A method for producing a polymer compound solution comprising a step of heating to 0 to 55 ° C. and dissolving the polymer compound in a solvent,
In the heating step, the swelling mixture is heated at a rate of 1 to 40 ° C./min.
The method (4) can be carried out in the following mode (5).
(5) The method for producing a polymer compound solution according to (4), wherein in the heating step, the swollen mixture is stirred and conveyed in a cylindrical container, and the swollen mixture is heated from around the container.

The object of the present invention has been achieved by the following apparatuses (1) to (9).
(1) A device for producing a polymer compound solution in which a stirring device, a cooling device, and a heating device are connected in this order,
An apparatus for producing a polymer compound solution, wherein the cooling device comprises a cylindrical container, a helical transport mechanism provided in the container, and a cooling mechanism provided around the container.
(2) The apparatus for producing a polymer compound solution according to (1), wherein the stirrer is an apparatus for mixing the polymer compound and the solvent at −10 to 55 ° C. to swell the polymer compound with the solvent.
(3) The apparatus for producing a polymer compound solution according to (2), wherein the cooling device is a device for cooling the swelling mixture to −100 to −10 ° C.
(4) The apparatus for producing a polymer compound solution according to (3), wherein the cooling device further has a mechanism for replenishing the container with a solvent cooled to −105 to −15 ° C.
(5) The apparatus for producing a polymer compound solution according to (4), wherein the heating device is a device for heating the cooled swollen mixture to 0 to 55 ° C.

(6) A polymer compound solution production apparatus in which a stirring device, a cooling device, and a heating device are connected in this order,
The apparatus for producing a polymer compound solution, wherein the heating device includes a cylindrical container, a spiral conveyance mechanism provided in the container, and a heating mechanism provided around the container .
(7) The apparatus for producing a polymer compound solution according to (6), wherein the stirrer is an apparatus that mixes a polymer compound and a solvent at −10 to 55 ° C. and swells the polymer compound with the solvent.
(8) The apparatus for producing a polymer compound solution according to (7), wherein the cooling device is a device for cooling the swelling mixture to −100 to −10 ° C.
(9) The apparatus for producing a polymer compound solution according to (8), wherein the heating device is a device for heating the cooled swelling mixture to 0 to 55 ° C.

When the cooling dissolution method is used, the polymer compound can be dissolved in the solvent even if it is a combination of the polymer compound and the solvent that does not dissolve at a normal temperature. The reason for this is thought to be that a change (such as destruction of a regular structure) occurs in the molecular arrangement of the polymer compound by cooling and heating.
When the present inventor further researched the cooling dissolution method, after the polymer compound was swollen with a solvent and then rapidly cooled or warmed in the cooling dissolution method, the polymer compound dissolved in the solvent. It was found that the sex was further improved. The reason for this is considered to be that when the cooling or heating (preferably both) is rapid, the molecular arrangement of the polymer compound changes significantly.
J. M.M. G. The Cowie et al paper does not describe the cooling rate and the heating rate. In addition, Kenji Kamide et al. Do not describe the cooling rate, and can calculate only the heating rate. The heating rate requires 5 hours (0.4 ° C./min) from −70 ° C. to 50 ° C. It is estimated that the cooling rate which is not described is also a similar rate.
According to the inventor's research, the swollen mixture is rapidly cooled in the cooling step at a rate of 1 ° C./min or more, or the swollen mixture is rapidly heated in the heating step at a rate of 1 ° C./min or more. It turned out to be preferable. As a result, it has become possible to produce polymer solutions from combinations of various polymer substances and solvents. That is, by adopting rapid cooling or rapid heating, the range of selection of the solvent type for a certain polymer substance is expanded.
The rapid cooling or heating described above can be easily achieved by using the manufacturing apparatus of the present invention. Moreover, the manufacturing apparatus of this invention can cool or heat a swelling mixture uniformly, without unevenness. Furthermore, the production apparatus of the present invention has an advantage that heat efficiency is good and rapid cooling or heating is possible with a small amount of energy used.

[Polymer compound and solvent]
As the polymer compound and the solvent, a combination of a polymer compound and a solvent in which the polymer compound swells with the solvent at a temperature in the range of 0 to 55 ° C. (temperature that is expected to be used as a solution) is used. If the polymer compound does not swell with a solvent, it is almost impossible to dissolve the polymer compound using a cooling dissolution method. Even when the polymer compound is dissolved in the solvent at the above temperature, using the cooling dissolution method of the present invention, a uniform solution can be obtained more rapidly than the conventional method of stirring at ordinary temperature or high temperature.
Examples of polymer compounds include polyamides, polyolefins (eg, norbornene), polystyrenes, polycarbonates, polysulfones, polyacrylic acids, polymethacrylic acids, polyether ether ketones, polyvinyl alcohols, polyvinyl acetates, and cellulose derivatives. (E.g., a lower fatty acid ester of cellulose) is used. A lower fatty acid ester of cellulose is particularly preferred.

The lower fatty acid ester of cellulose, which is a preferred polymer compound, will be further described.
Lower fatty acid means a fatty acid having 6 or less carbon atoms. The number of carbon atoms is preferably 2 (cellulose acetate), 3 (cellulose propionate) or 4 (cellulose butyrate). Cellulose acetate is more preferable, and cellulose triacetate (degree of acetylation: 58.0 to 62.5%) is particularly preferable. A mixed fatty acid ester of cellulose such as cellulose acetate propionate or cellulose acetate butyrate may be used.

As described above, the solvent used is a liquid that swells the polymer compound. Therefore, the specific type of solvent is determined according to the type of polymer compound used. For example, when the polymer compound is cellulose triacetate, acetone or methyl acetate is used as a preferred solvent.
Examples of solvents that can be used include ketones (eg, acetone, methyl ethyl ketone, cyclohexanone), esters (eg, methyl formate, methyl acetate, ethyl acetate, amyl acetate, butyl acetate), ethers (eg, dioxane, dioxolane). , THF, diethyl ether, methyl-t-butyl ether) and hydrocarbons (eg, benzene, toluene, xylene, hexane).
The boiling point of the solvent is preferably 20 to 300 ° C, more preferably 30 to 200 ° C, and most preferably 40 to 100 ° C.

[Swelling process]
In the swelling step, the polymer compound and the solvent are mixed at −10 to 55 ° C., and the polymer compound is swollen with the solvent.
The temperature of the swelling process is usually room temperature.
The ratio between the polymer compound and the solvent is determined according to the concentration of the solution finally obtained. However, when the solvent is replenished in the cooling step described later, the amount of the solvent is reduced by the replenishment amount. In general, the amount of the polymer compound in the swelling step is preferably 5 to 30% by weight of the solution to be prepared, more preferably 8 to 20% by weight, and most preferably 10 to 15% by weight. .
The swelling mixture of the solvent and the polymer compound is preferably stirred until the polymer compound is sufficiently swollen. The stirring time is preferably 10 to 150 minutes, more preferably 20 to 120 minutes.
In the swelling step, components other than the solvent and the polymer compound, for example, a plasticizer, a deterioration preventing agent and an ultraviolet ray preventing agent may be added.

[Cooling process]
In the cooling step, the swollen mixture is cooled to −100 to −10 ° C. The cooling temperature is preferably a temperature at which the swollen mixture is solidified.
It is preferable to rapidly cool the swollen mixture at a rate of 1 ° C./min or more. The cooling rate is more preferably 2 ° C./min or more, further preferably 4 ° C./min or more, and most preferably 8 ° C./min or more. The higher the cooling rate, the better. However, about 40 ° C./min is a general upper limit.
The cooling rate is a value obtained by dividing the difference between the temperature at the start of cooling and the final cooling temperature by the time from the start of cooling to the final cooling temperature.
In order to cool the swollen mixture rapidly, it is preferable to transport the inside of the cylindrical container while stirring the swollen mixture and cool the swollen mixture from the periphery of the container. When such a cooling device is used, the swollen mixture can be cooled quickly and uniformly. This cooling device will be described later.

Moreover, the solvent cooled to -105 thru | or -15 degreeC can be added to a swelling mixture, and also it can be made to cool more rapidly. The temperature of the solvent to be replenished is preferably −100 to −25 ° C., more preferably −95 to −35 ° C., and most preferably −85 to −55 ° C.
The time required for the cooling step (the total of the time required for cooling the swollen mixture and the time for maintaining the swollen mixture at the cooling temperature) is preferably 10 to 300 minutes, and more preferably 20 to 200 minutes.
In the cooling process, it is desirable to use an airtight container in order to avoid moisture mixing due to condensation during cooling. Further, if the pressure is reduced during cooling, the cooling time can be shortened. In order to perform decompression, it is desirable to use a pressure resistant container.

[Heating process]
In the heating step, the cooled swelling mixture is heated to 0 to 55 ° C. The final temperature of the heating step is usually room temperature.
It is preferred to rapidly warm the swollen mixture at a rate of 1 ° C./min or more. The heating rate is more preferably 2 ° C./min or more, further preferably 4 ° C./min or more, and most preferably 8 ° C./min or more. The heating rate is preferably as high as possible, but about 40 ° C./min is a general upper limit.
The heating rate is the value obtained by dividing the difference between the temperature at the start of heating and the final heating temperature by the time from the start of heating until the final heating temperature is reached. is there.
In order to warm the swollen mixture rapidly, it is preferable to transport the inside of the cylindrical container while stirring the swollen mixture and to heat the swollen mixture from the periphery of the container. When such a heating apparatus is used, the swollen mixture can be heated quickly and uniformly. This heating device will be described later.

The time required for the heating step (the sum of the time required for heating the swollen mixture and the time for maintaining the swollen mixture at the heating temperature) is preferably 10 to 300 minutes, and preferably 20 to 200 minutes. Further preferred.
When heating is performed while applying pressure, the heating time can be shortened. In order to perform pressurization, it is desirable to use a pressure-resistant container.
In addition, when the dissolution is insufficient, the cooling step and the heating step may be repeated. Whether or not the dissolution is sufficient can be determined by merely observing the appearance of the solution with the naked eye.

[Processing after solution production]
The manufactured solution can be subjected to treatment such as concentration adjustment (concentration or dilution), filtration, temperature adjustment, and component addition as necessary.
The component to be added is determined according to the use of the polymer compound solution. Typical additives are plasticizers, deterioration inhibitors (eg, peroxide decomposers, radical inhibitors, metal deactivators, acid scavengers) and UV inhibitors.
The solution should be stored within a stable temperature range. For example, a solution prepared by cooling and dissolving cellulose triacetate using acetone as a solvent has two phase separation regions in a high temperature region and a low temperature region in a practical storage temperature range. In order to store this solution stably, it is necessary to maintain the temperature in the intermediate homogeneous phase region.
The obtained polymer compound solution is used for various applications.

[Manufacture of polymer films]
The production of the polymer film by the solvent cast method, which is a typical use of the polymer compound solution, will be described.
The polymer compound solution is cast on a support and the solvent is evaporated to form a film. The concentration of the solution before casting is preferably adjusted so that the solid content is 18 to 35%. The surface of the support is preferably finished in a mirror state. A drum or a band is used as the support. For casting and drying methods in the solvent casting method, U.S. Pat. Nos. 736892, JP-B 45-4554, 49-5614, JP-A-60-176834, 60-203430, and 62-1115035.
In the case of a cellulose acetate solution, the solution is preferably cast on a support having a surface temperature of 10 ° C. or lower. It is preferable to cast and dry for 2 seconds or longer. The obtained film can be peeled off from the support and further dried with high-temperature air whose temperature is successively changed from 100 to 160 ° C. to evaporate the residual solvent. The above method is described in Japanese Patent Publication No. 5-17844. According to this method, it is possible to shorten the time from casting to stripping.

[manufacturing device]
The manufacturing apparatus will be described with reference to the drawings.
FIG. 1 is a flowchart showing a combination of each process and apparatus of the present invention.
In the swelling step, the polymer compound (P) and the solvent (S1) are added to the stirring tank (1). The polymer compound and the solvent are mixed in the stirring tank, and the polymer compound is swollen with the solvent.
The swollen swollen mixture is sent from the liquid feed pump (2) to the cooling device (3). As the liquid feeding pump (2), a snake pump suitable for feeding a viscous liquid is used.

The cooling device (3) includes a cylindrical container, a spiral conveyance mechanism (3-1) provided in the container for conveying the inside of the cylindrical container while stirring the swollen mixture, and the swelling in the container It consists of a cooling mechanism (3-2) provided around the container to cool the mixture. By rotating the spiral conveyance mechanism (3-1), the swollen mixture is not retained (for example, the swollen mixture remaining on the wall surface of the container is also scraped off), while being sheared, mixed and cooled. , Send liquid. The cooling mechanism (3-2) shown in FIG. 1 is mounted around the container in a jacket shape. The refrigerant (24) sent from the refrigerant tank (21) flows inside the cooling mechanism (3-2). As the refrigerant, for example, a mixture of methanol and water is used. Note that the spiral conveyance mechanism may be fixed, and the swollen mixture may be passed through the spiral structure by pressure.
The refrigerant used for cooling returns to the refrigerant tank (21). The refrigerant is cooled by the refrigerator (22). The heat generated by this cooling is processed by the cleaning tower (23).
The cooling device (3) shown in FIG. 1 has a mechanism for replenishing the container with the solvent cooled to −105 to −15 ° C. The replenishing solvent (S2) is cooled to a necessary temperature in the cooling stock tank (19), and is sent to the container of the cooling device (3) by the liquid feed pump (20). By adding the replenishing solvent thus cooled, the swollen mixture can be cooled very quickly.
The cooling device (3) will be described in more detail with reference to FIG.
In the above cooling device, the swollen mixture is cooled quickly and uniformly to −100 to −10 ° C. The cooled swelling mixture is sent to the warming device (4).

Similarly to the cooling device (3), the heating device (4) is provided in the cylindrical container and the container for transporting the cylindrical mixture while stirring the swelling mixture while stirring the swelling mixture. It consists of a spiral conveyance mechanism (4-1) and a heating mechanism (4-2) provided around the container for heating the swollen mixture in the container. The spiral conveyance mechanism (4-1) rotates to feed the liquid while being swollen, mixed and heated without staying in the swollen mixture. The heating mechanism (4-2) shown in FIG. 1 is mounted around the container in a jacket shape. Inside the heating mechanism (4-2), hot water (26) sent from the thermostat (27) flows. Note that the spiral conveyance mechanism may be fixed, and the swollen mixture may be passed through the spiral structure by pressure.
As with the cooling device, a warmed replenishing solvent may be added, but from the viewpoint of thermal efficiency, the addition of the replenishing solvent to the warming device is not very effective. In the warming device, heat generated by stirring contributes to warming of the swollen mixture in addition to warm water (26).
The hot water used for heating is exchanged with water from the cleaning tower (23) in the heat exchanger (25). Thereby, the energy efficiency of the whole apparatus can be improved. The heat-exchanged hot water returns to the constant temperature bath (27).
In the above heating apparatus, the swollen mixture is quickly and uniformly heated to 0 to 55 ° C., and the polymer compound is dissolved in the solvent. The obtained solution passes through the heater (6), the filter (7), and the pressure adjustment valve (8) by the liquid feed pump (5), and is subjected to temperature adjustment, filtration, and pressure adjustment.

The solution is further concentrated in a concentration tank (9). That is, the solution brought to a high temperature and high pressure state by the heater (6) and the pressure adjusting valve (8) is concentrated by evaporating the solvent in the concentration tank (9), thereby evaporating the solvent. The evaporated solvent is sent to the cooling stock tank (19) through the liquefying device (18). The liquefied solvent is sent to the container of the cooling device (3) by the pump (20) again together with the replenishing solvent (S2).
The concentrated solution is sent to the stock tank (12) through the temperature adjusting device (11) by the liquid feed pump (10).
The apparatus shown in FIG. 1 further includes an apparatus for producing a polymer film by a solvent cast method.
The solution in the stock tank (12) is sent to the slit-shaped die (15) through the filter (14) by the liquid feed pump (10). The solution is extruded into a film shape by a die (15), cast onto a belt-like support (16), dried and then peeled off to produce a film (17). The film (17) is further dried and wound up.

FIG. 2 is an enlarged sectional view of the cooling device (3 in FIG. 1).
The swelling mixture of the polymer compound and the solvent enters the container from the inlet (31-1), is cooled, and is sent from the outlet (31-2) to the next heating device.
The container is also provided with a cooled replenishing solvent inlet (32), a refrigerant inlet (33-1) and a refrigerant outlet (33-2).
In the container, the spiral conveying mechanism rotates around the helical axis (34), so that the swollen mixture is not retained, and the inlet (31-1) to the outlet (32- Pump up to 2). That is, the swollen mixture remaining on the wall surface of the housing (35) of the container is also scraped off and fed.

Inside the jacket-like cooling mechanism (36), in other words, outside the housing (35) of the container, turbulent fins (37) are provided in a spiral shape to increase the cooling efficiency of the refrigerant.
The helical shaft (34) is rotated by a motor (not shown) external to the container housing (35). Since the inside of the container is in a high pressure state, the portion where the spiral shaft (34) and the housing (35) are in contact is sealed with the seal member (38) and the seal pressing portion (39).
As the heating device (4 in FIG. 1), the same device as in FIG. 2 can be used. However, in the case of a heating device, it is not necessary to provide an inlet (32) for the replenishing solvent.

[Example 1]
A solution in which 26 parts by weight of cellulose triacetate was dissolved in 74 parts by weight of acetone was prepared using the apparatus shown in FIG. Of 74 parts by weight of acetone, 70 parts by weight were added in the swelling process, and the remaining 4 parts by weight were added as a replenishing solvent in the cooling process.
The obtained solution was visually observed to confirm that a transparent and uniform solution was obtained.
Specific processing conditions are as follows.
Temperature of swelling process: room temperature Time of swelling process: 30 minutes Cooling rate: 10 ° C./minute Temperature of replenishing solvent: −80 ° C.
Final cooling temperature: adjusted to −75 to −65 ° C. Cooling process time: 60 minutes Heating rate: 10 ° C./minute Final heating temperature: 50 ° C.
Warming process time: 60 minutes

[Comparative Example 1]
When 26 parts by weight of cellulose triacetate and 74 parts by weight of acetone were stirred at 30 ° C. for 1 hour, cellulose triacetate was swollen by acetone but was not dissolved at all.
The swollen mixture was cooled to −70 ° C. using methanol / dry ice as a refrigerant. The cooling rate was 0.4 ° C./min. The swelling mixture was left at -70 ° C. for 2 hours.
While stirring this, the temperature was raised to 50 ° C. over 5 hours. The heating rate was 0.4 ° C./min. The swollen mixture was further stirred at 50 ° C. for 3 hours.
Most of the cellulose triacetate was dissolved, but part of the cellulose triacetate was not dissolved and was visually observed as white turbidity in the solution.

[Example 2]
A solution in which 18 parts by weight of cellulose triacetate was dissolved in 82 parts by weight of methyl acetate was prepared using the apparatus shown in FIG. Of the 82 parts by weight of methyl acetate, 75 parts by weight were added in the swelling step, and the remaining 7 parts by weight were added as a replenishing solvent in the cooling step.
The obtained solution was visually observed to confirm that a transparent and uniform solution was obtained.
Specific processing conditions are as follows.
Swelling step temperature: room temperature Swelling step time: 45 minutes Cooling rate: 12 ° C./min Replenishing solvent temperature: −50 ° C.
Final cooling temperature: adjusted to −45 to −40 ° C. Cooling process time: 40 minutes Heating rate: 8 ° C./minute Final heating temperature: 50 ° C.
Warming process time: 50 minutes

[Example 3]
A solution in which 18 parts by weight of cellulose triacetate was dissolved in 62 parts by weight of methyl acetate and 20 parts by weight of ethanol was prepared using the apparatus shown in FIG. Of the total 82 parts by weight of methyl acetate and ethanol, 75 parts by weight were added in the swelling process, and the remaining 7 parts by weight were added as a replenishing solvent in the cooling process.
The obtained solution was visually observed to confirm that a transparent and uniform solution was obtained.
Specific processing conditions are as follows.
Swelling process temperature: room temperature Swelling process time: 60 minutes Cooling rate: 12 ° C./min Replenishing solvent temperature: −55 ° C.
Final cooling temperature: adjusted to −50 to −45 ° C. Cooling process time: 50 minutes Heating rate: 10 ° C./min Final heating temperature: 50 ° C.
Warming process time: 60 minutes

It is a flowchart which shows the combination of each process and apparatus of this invention. It is sectional drawing of a cooling device.

Explanation of symbols

S1 Solvent P Polymer Compound S2 Replenishment Solvent 1 Stirring Tank 2 Liquid Pump 3 Cooling Device 3-1 Spiral Conveyance Mechanism 3-2 Jacket-shaped Cooling Mechanism 4 Warming Device 4-1 Spiral Conveyance Mechanism 4-2 Jacket-shaped heating mechanism 5 Liquid feed pump 6 Heater 7 Filter 8 Pressure adjustment valve 9 Concentration tank 10 Liquid feed pump 11 Temperature adjustment device 12 Stock tank 13 Liquid feed pump 14 Filter 15 Die 16 Belt-like support 17 Film 18 Liquefaction device DESCRIPTION OF SYMBOLS 19 Cooling stock tank 20 Liquid feed pump 21 Refrigerant tank 22 Refrigerator 23 Cleaning tower 24 Refrigerant 25 Heat exchanger 26 Hot water 27 Thermostatic bath 31-1 Swelling mixture inlet 31-2 Swelling mixture outlet 32 Cooled replenishing solvent inlet 33 -1 Refrigerant inlet 33-2 Refrigerant outlet 34 Spiral shaft 35 Vessels of the housing 36 the jacket-like cooling mechanism 37 turbulence fin 38 seal member 39 seal pressing portion

Claims (9)

A device for producing a polymer solution in which a stirrer, a cooling device, and a heating device are connected in this order,
An apparatus for producing a polymer compound solution, wherein the cooling device comprises a cylindrical container, a helical transport mechanism provided in the container, and a cooling mechanism provided around the container.   The apparatus for producing a polymer compound solution according to claim 1, wherein the stirring device is a device that mixes the polymer compound and the solvent at −10 to 55 ° C. and swells the polymer compound with the solvent.   The apparatus for producing a polymer compound solution according to claim 2, wherein the cooling device is a device that cools the swelling mixture to -100 to -10 ° C.   The apparatus for producing a polymer compound solution according to claim 3, wherein the cooling device further has a mechanism for replenishing the container with the solvent cooled to -105 to -15 ° C.   The apparatus for producing a polymer compound solution according to claim 4, wherein the heating device is a device for heating the cooled swelling mixture to 0 to 55 ° C. A device for producing a polymer solution in which a stirrer, a cooling device, and a heating device are connected in this order,
The apparatus for producing a polymer compound solution, wherein the heating device includes a cylindrical container, a spiral conveyance mechanism provided in the container, and a heating mechanism provided around the container .   The apparatus for producing a polymer compound solution according to claim 6, wherein the stirring device is a device that mixes the polymer compound and the solvent at -10 to 55 ° C and swells the polymer compound with the solvent.   The apparatus for producing a polymer compound solution according to claim 7, wherein the cooling device is a device for cooling the swelling mixture to -100 to -10 ° C.   The apparatus for producing a polymer compound solution according to claim 8, wherein the heating device is a device for heating the cooled swelling mixture to 0 to 55 ° C.

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