JPH10100145A - Production of rubbery polymer and apparatus therefor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide method and apparatus of rubbery polymer which can enhance operability (simplifying operation and reducing the loss of a product even when the kind of a rubbery polymer to be produced is changed over and shortening a changeover time), reduce a process and machinery and achieve the reduction of equipment cost and production cost in the production of a rubbery polymer. SOLUTION: A coagulation soln. is added to a cementitious rubber soln. after polymerization to precipitate a rubbery polymer component which is, in turn, dried to obtain a rubbery polymer in a dry state. In this method, the cementitious rubber soln. and the coagulation soln. are respectively separatelysupplied to the area immediately before the inlet of a rotary blade 36 of a pump 14 equipped with grinding function and brought to a contact state to immediately sent to a dryer 16 by the pump 14.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method and an apparatus for producing a rubber-like polymer.

[0002]

2. Description of the Related Art In a synthetic rubber manufacturing process, for example, as shown in FIG.
After the cement-like rubber solution is obtained, the rubber-like polymer component is precipitated and washed by a coagulation device 9 composed of a large coagulation tank (for example, tanks 4, 6, and 8), and the crumb-like rubber-like component is washed. Obtain a polymer. Thereafter, the liquid containing the crumb-like rubber-like polymer is conveyed to the drying means by the pump 10 or the like, to obtain a rubber-like polymer in a dry state.

[0003] The polymer before dehydration and drying through the coagulator 9 is in the form of a crumb and contains a large amount of water inside. For dehydration of such a high water content rubbery polymer,
A centrifugal dehydrator can hardly perform dehydration. Therefore, water is evaporated by hot-air drying using a heat source, and is supplied to a molding machine in a dry state.

However, this heating and drying means not only requires enormous energy but also is exposed to a high temperature for a long time, so that the rubber-like polymer itself deteriorates. In addition, since these heating and drying means are provided separately from the supply system to the molding machine, there are various problems that the equipment cost is increased and the installation space is increased.

In view of the above, a twin-screw extruder (Japanese Patent Laid-Open No. 59-214631) has been proposed in which dewatering is performed at the stage of supplying raw materials to a molding section of a molding machine to solve the above-mentioned problems. I have. This is driven in a different direction 2
A flange is formed at a predetermined interval in the axial direction on the book screw, and the water-containing raw material is condensed by the flange to squeeze out moisture, and is drained from a vent provided in the barrel. .

[0006]

However, in the conventional method and apparatus for producing a rubber-like polymer, as shown in FIG. 6, a large-sized coagulation device 9 was required in the coagulation step, so that the operation was complicated. However, operability is poor, and a large installation space is required, which increases equipment costs and manufacturing costs.

Further, it has been extremely difficult to produce a rubbery polymer having high tackiness or a rubbery polymer having a low Mooney viscosity by the conventional method and apparatus.

The present invention has been made in view of such a situation, and has improved operability (simplification of operation, reduction in product loss even when switching the type of rubber-like polymer to be produced, and the like). It is an object of the present invention to provide a method and an apparatus for producing a rubber-like polymer capable of reducing the number of processes and equipment, reducing the equipment cost and the production cost. Another object of the present invention is to provide a method and an apparatus for producing a rubbery polymer which can easily produce a rubbery polymer having a high tackiness or a rubbery polymer having a low Mooney viscosity.

[0009]

In order to achieve the above object, a method for producing a rubber-like polymer according to the present invention comprises the steps of: adding a coagulating liquid to a cement-like rubber solution to precipitate a rubber-like polymer component; A method for producing a rubber-like polymer, in which a rubber-like polymer in a dried state is obtained by drying a rubber-like polymer component that has been precipitated, wherein a cement-like rubber solution and a coagulation liquid are separately separated, and a crushing function is provided. The rubber solution and the coagulating liquid are supplied immediately before the inlet of the rotary blade of the pump, and immediately sent to the drying means by the pump.

An apparatus for producing a rubbery polymer according to the present invention comprises:
Cement feeding means for sending a cement-like rubber solution, coagulation liquid sending means for sending a coagulating liquid for precipitating a rubber-like polymer component in the rubber solution, and the cement feeding means and the coagulating liquid sending means, respectively. The rubber solution and the coagulating liquid include a pump with a crushing function in which a suction port is configured to come into contact immediately before the inlet of the rotor, and a crumb-like rubber-like polymer that is crushed and sent by the pump with the crushing function. Drying means for drying the slurry to obtain a dry rubbery polymer.

The suction port of the pump with a crushing function can be any of a bladed pump having a rotary blade mounted in front of a rotary blade or a bladeless pump such as a homogenizer or a high-speed air mixer. From the viewpoint, a pump with a blade is preferable. The pump with a crushing function is not particularly limited, but a pump called a so-called crushing pump is preferable. The flow of the fluid in the pump may be a centrifugal flow or an axial flow. The discharge line of the pump preferably has a flow velocity of 1 m / sec or more. Also, it is preferable that the distance of the discharge line to the drying means is short.

The drying means preferably has a washing means. In the cleaning means, cleaning water is supplied. The amount of water to be supplied to the washing water is preferably about 1: 1 to 1:30 by weight based on the rubber-like polymer component. If the amount of the washing water is too large, the washing water is not effectively used, and the recovery of the washing water becomes insufficient, which may cause the rubber polymer to be undried. Further, the temperature of the water provided for the washing water is preferably warm water of 40 ° C. or higher. This is because the cleaning effect is improved.

As a drying means, as shown in Japanese Patent Publication No. 6-9825, two screws whose temperature is controlled are provided in parallel in a barrel, these screws are driven to rotate in the same direction, and the screw ridges are formed. The barrel receives a slurry containing a rubber-like polymer from the feed side toward the tip using a co-rotating intermeshing twin-screw extruder in which the barrel and the valley are meshed as closely as possible. It is preferable that the drying device includes a barrel and at least one dehydration barrel having a discharge port such as a slit for discharging a liquid dehydrated from the slurry containing the rubbery polymer.

It is preferable that at least two dewatering barrels are mounted at the front and rear stages of the drying device. The slit width of the dewatering barrel at the front stage is preferably larger than that at the rear stage, and is 0.1 to 0.2 mm. It is preferable to select a wedge-shaped screen of a certain degree. Further, the gap between the slits of the subsequent dewatering barrel is preferably about 0.05 to 0.1 mm. It is preferable that the former dehydration barrel also serves as a feed barrel, and it is preferable that the slurry containing the crumb-like rubber-like polymer be quickly squeezed and the serum containing the solvent be discharged. It is difficult to feed the serum itself to the subsequent stage with the screw of the twin-screw extruder, which causes so-called shabtsuki. In addition, the shabbing means that the serum pushed into the twin-screw extruder returns to the inlet side without being sufficiently discharged, and the penetration of the crumb becomes worse.

The drying device includes a feed barrel (preferably provided with a slit), a vent barrel equipped with an atmospheric vent or a vacuum vent in addition to the dehydration barrel, a washing water supply barrel to which washing water is supplied, It is preferable to further have a mere ordinary barrel. The washing water supply port attached to the washing water supply barrel may be a commercially available one equipped with a check valve, but minimizing the clearance between the screw and the flight is an effective means for not closing the supply port. Further, in the vent barrel, when the gas is released, the rubber-like polymer component inside may vent up or flake up, thereby blocking the gas passage. In order to prevent such a point, it is preferable that a wedge-shaped cut is made in the inner surface of the vent block in the vent barrel to allow the rubber-like polymer component to bite into the barrel.
When vent up or flake-up is more severe, it is preferable that the vent barrel be a slit barrel.

In the present invention, as the drying means,
When a screw extruder type drying device is used, the screw immediately below the supply section to which the crumb-like rubber-like polymer is supplied, has a deep valley and a large pitch, and has a high water content and a high bulk. It is preferable that a large crumb is quickly sent to a subsequent process. This is because, although this part is a closed system, it is not pushed by the discharge pressure of the pump with a crushing function, but is pushed by the rotation of the screw in a normal pressure system. Insufficient feeding by the screw may cause clogging in the supply unit, and may cause a supply stop, which is not preferable. Further, by making the valley portion of the screw deeper and increasing the pitch, the rotation speed of the screw can be reduced, and the temperature of the die can be reduced.

Further, it is preferable to mount one forward kneading disc and one reverse kneading disc in series on the screw in the ordinary barrel after the serum is discharged. The subsequent screw in the washing water supply barrel is equipped with two forward kneading discs, and the subsequent screw in the normal barrel is equipped with one reverse kneading disc. It is preferable to improve the mixing and to extract the soap. A dewatering barrel and a normal barrel are connected successively at the subsequent stage of the normal barrel.
It is preferable to mount the disc and one inverted kneading disc in series. The dewatering barrel after the washing water supply barrel is for squeezing the washing water in the crumb.

The barrel connected after the barrel for squeezing the washing water becomes a barrel for the desolvation step, that is, the drying step. Depending on the degree of drying, the number of barrels connected varies, but it has at least two vent barrels and a normal barrel connected between them. Preferably, at least one of the vent barrels is an atmospheric vent barrel leading to a normal pressure system, and at least one other is a vacuum vent barrel leading to a reduced pressure system.
The screw located in the normal barrel between these vent barrels promotes the renewal of the crumb surface and performs degassing,
It is preferable to mount one forward kneading disk, one neutral disk, and one reverse kneading disk as a set. In the case where water washing is insufficient, the number of washing water supply barrels to be connected is increased, a dewatering barrel is attached to the barrel, and a screw corresponding thereto is used.

Although the temperature of the barrel is not particularly limited, the barrel at the preceding stage up to the barrel from which the washing water is discharged is 40 to 40.
70 ° C. is preferable, and the subsequent barrel is 15 ° C.
It is preferable to keep the temperature at 0 to 170 ° C. If the temperature of the barrel in the preceding stage is low, the cleaning effect is reduced, and if it is too high, the serum and the cleaning water are gasified, causing breathing and impeding the smooth flow in the twin-screw machine. Also, if the temperature of the barrel at the subsequent stage is too high, the product will be deteriorated. Conversely, if it is too low, degassing will be insufficient.

In the drying means, it is preferable that the slurry containing the crumb-like rubbery polymer is squeezed and the serum water containing the solvent discharged is all recovered and sent to the solvent purification step. Preferably. First, fresh process water is supplied as washing water for a twin-screw extruder-type drying device at the barrel position after collecting the serum, and is recovered by a wedge screen or the like of a subsequent dewatering barrel. It is preferable to supply a coagulating liquid to a suction port of a pump with a crushing function. The recovered water contains a few percent (eg, 3%) of the washed solvent and includes any fine crumbs that have leaked out of the wedge screen. become. At the same time, it leads to reduction of process water consumption.

As the coagulating liquid, for example, water is used. The supply amount of the coagulating liquid is not particularly limited, but is 1: 1 by volume ratio to the solvent of the rubber solution (for example, acetone).
It is preferably about 0.05 to 1: 3. If the supply amount of the coagulating liquid is too small, the rubber-like polymer component is not precipitated in the pump, and the drying means does not sufficiently separate the crumb and the liquid, resulting in crumb loss or The effect of the subsequent cleaning may be adversely affected. If the supply amount of the coagulating liquid is too large, the effect of the washing is positively affected. However, in the drying means, the liquid is insufficiently separated from the crumb and the separated liquid (solvent + coagulating liquid) This makes it difficult to recover and reuse the solvent.

The temperature of the coagulating liquid supplied by the coagulating liquid feeding means varies depending on the type of solvent such as acetone in the rubber solution, but is preferably higher than normal temperature and lower than the boiling point of the solvent. About 30 to 60 ° C. is preferable. By setting the temperature of the coagulating liquid in such a range, the crumbs are softened, and the crumbs are smoothly bitten by the twin-screw extruder as a drying means.
This is because the soap content in the rubber solution is extracted in advance and the cleaning effect is exhibited. From such a viewpoint, it is preferable that the temperature of the rubber solution supplied by the cement feeding means is substantially equal to the temperature of the coagulating liquid.

In the method and apparatus for producing a rubber-like polymer according to the present invention, the cement-like rubber solution is
Although not particularly limited, for example, an acrylonitrile-butadiene copolymer rubber (NBR) solution using acetone as a solvent, a maleated NBR solution, a hydrogenated NBR solution, a maleated hydrogenated NBR solution, and the like can be exemplified. Water is used as the liquid. Further, in the present invention, in the solution polymerization system, the third solvent (extractant) is fed as a coagulating liquid to a pump having a crushing function, the rubber solution is made poor solvent, and the rubbery polymer is precipitated. Washing and drying can also be performed. For example, a chlorhydrin rubber solution polymerized in benzene is separately sent to a suction port of a pump with a crushing function together with a coagulating liquid consisting of a solvent such as cyclohexane or methanol, and a drying step by a drying means is obtained. Can also be obtained.

[0024]

In the production method using the rubber-like polymer production apparatus according to the present invention, the cement-like rubber solution and the coagulation liquid are separately supplied just before the inlet of the rotor of the pump with a crushing function. The rubber solution and the coagulation liquid are brought into contact with each other and immediately sent to the drying means by the pump. For this reason, a rubber-like polymer precipitates before the rotor of the pump, and the deposited rubber-like polymer is crushed by a pump having a crushing function and has a rubber-like weight of an appropriate size to be transported. The slurry containing the combined crumb is sent to the drying means. In the drying means, serum is recovered from the slurry containing the rubbery polymer,
Thereafter, the rubbery polymer is washed with washing water and then degassed and dried. It was confirmed that the dry rubber-like polymer thus obtained had a quality equal to or higher than that of the rubber-like polymer obtained by the conventional method and apparatus.

Therefore, according to the production method using the production apparatus for a rubbery polymer according to the present invention, it is possible to reduce the conventionally used coagulation device comprising a large tank,
In the drying step, equipment such as a slurry storage tank and a screen is not required, so that the number of processes and equipment can be reduced, and the equipment cost and the manufacturing cost can be reduced. Further, the operation is simplified, the loss of the product is reduced even when the type of the rubber-like polymer to be produced is switched, the switching time can be shortened, and the operability is improved. Further, in the present invention, a rubbery polymer having a high tackiness or a rubbery polymer having a low Mooney viscosity can be easily produced.

Further, according to the present invention, the accuracy of measurement of raw materials or products is remarkably improved, and automation of the manufacturing process can be facilitated. That is, in the present invention, the flow rate of the cement-like rubber solution fed to the pump with the crushing function can be accurately measured, and the amount is supplied to the drying means as it is, so that a stable operation can be obtained only. Alternatively, for example, other components can be easily added in proportion to the amount of crumb. On the other hand, in the conventional method, when the slurry containing the crumb-like rubber-like polymer is quantitatively supplied to the drying means including the twin-screw or single-screw extruder, the crumb is liable to adhere and stagnate. Difficult from things. Conventionally, it is conceivable to install an impact-type crumb flow meter, but the accuracy is low.

[0027]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a method and an apparatus for producing a rubber-like polymer according to the present invention will be described in detail based on an embodiment shown in the drawings.

FIG. 1 is a schematic view of an apparatus for producing a rubbery polymer according to an embodiment of the present invention, FIG. 2 is an exploded perspective view of a pump having a crushing function, FIG. 3 is a cross-sectional view of a drying apparatus, and FIG. FIG. 5 is a schematic sectional view of the screw, and FIG. 5 is a schematic sectional view of the screw.

As shown in FIG. 1, the apparatus 12 for producing a rubbery polymer has a pump 14 with a crushing function and a drying apparatus 16 as drying means. The drying device 16 according to the present embodiment is a so-called twin-screw extruder type dehydration drying device,
4 and a plurality of barrels 20 surrounding the screws 18 as shown in FIG.
a to 20n. Screws 18, 18 shown in FIG.
Are rotationally driven by a motor 22 shown in FIG. As shown in FIGS. 3 and 4, the screws 18, 18 are meshing types in which the crests 18A and the valleys 18B are meshed as closely as possible, and the spiral directions of the screws 18, 18 are right and left. And are driven to rotate in the same direction.

The barrel 20 a shown in FIG. 1 is a feed barrel and has a feed port 24 for receiving a slurry containing a crumb-like rubber-like polymer sent from a pump 14. The barrel 20n at the last stage has a discharge port 26, and continuously forms a product made of a plate-like or linear rubber-like polymer after drying. Details of these barrels 20a to 20n will be described later.

The pump 14 with a crushing function shown in FIG. 1 is a so-called crushing pump. As shown in FIGS. 1 and 2, a pump casing 28 having a suction port 30 and a discharge port 32 is provided in a pump casing 28. A rotary blade 34 for crushing and a rotary blade 36 for feeding liquid are rotatably mounted. The rotary blade 34 is for crushing crumbs contained in the fluid sucked from the suction port 30, and includes a motor 37 together with a rotary wing 36 for sucking and discharging the fluid.
Is driven to rotate.

The suction port 30 is provided with an adapter 38. Two flow paths 40 and 42 are separately formed in the adapter 38, and one of the flow paths 40 is connected to a cement transport pipe 44 as cement feed means into which a cement-like rubber solution is fed. The other flow path 42 is connected to a coagulating liquid transport pipe 46 as a coagulating liquid feeding means into which the coagulating liquid is fed.

The cement transport pipe 44 directly transports a cement-like rubber solution containing a rubber-like polymer polymerized in the polymerization tank 2 shown in FIG. 6 to the suction port 30 of the pump 14. In the middle of the pipe 44, a transport pump is arranged. In this embodiment, the rubber solution transported by the pipe 44 is a solution obtained by dissolving rubber such as NBR with a solvent such as acetone, and is a viscous liquid (cement).
The rubber content is about 12 to 13% by weight.

The coagulating liquid transported by the coagulating liquid transport pipe 46 is, for example, water. In this embodiment, in order to reduce consumption of water and waste of crumbs, a dehydrating barrel 20e shown in FIG. The washing water collected from the company is used. That is, the washing water containing some crumbs is collected, and the washing water is transported from a tank storing the washing water by a pump or the like,
As coagulated water, the suction port 3 of the pump 14
0. The supply amount of the coagulation water from the pipe 46 is not particularly limited, but is preferably about 1: 0.05 to 1: 3 by volume ratio with respect to the solvent (for example, acetone) of the rubber solution. If the supply amount of the coagulation water is too small, the rubber-like polymer component is not precipitated in the pump, and the drying device 16 does not perform good separation of the crumb and the liquid. This may adversely affect the effect of the subsequent cleaning step. If the supply amount of the coagulation water is too large, the effect of the washing is positively affected. However, in the drying device 16, insufficient separation of the liquid from the crumb occurs, and the separated liquid (solvent + coagulation liquid) ) Makes it difficult to recover and reuse the solvent.

The temperature of the coagulated water supplied through the pipe 46 varies depending on the type of solvent such as acetone in the rubber solution, but is preferably higher than normal temperature and lower than the boiling point of the solvent. About 60 ° C is preferable. By setting the temperature of the coagulated water in such a range, the crumb is softened, the crumb is bitten into the twin screw 18 in the drying device 16, and the soap content in the rubber solution is reduced in advance. This is because it is extracted and the cleaning effect is exhibited. From such a viewpoint, it is preferable that the temperature of the rubber solution supplied through the cement transport pipe 44 is substantially equal to the temperature of the coagulated water.

The adapter 38 shown in FIGS. 1 and 2 is arranged so that the rubber solution and the coagulated water sent through the cement transport pipe 44 and the coagulated liquid transport pipe 46 come into contact with the rotary blade 36 and the rotary blade 34 immediately before the inlet. Then, it is inserted into the suction port 30. Between the rotary blade 36 and the rotary blade 36,
A grid or the like provided with slits may be mounted.

The discharge port 32 of the pump 14 is connected to the feed port 24 of the drying device 16 through a slurry supply pipe 48 shown in FIG. It is preferable that the velocity of the fluid in the slurry supply pipe 48 has a flow velocity of 1 m / sec or more. It is preferable that the length of the pipe 48 is also short.

Feed barrel 20 having feed port 24
The first dehydration barrel 20b1 having a slit or the like is connected to the rear side of the section a. First dehydration barrel 20b
In step 1, the serum water squeezed out of the slurry by the rotation of the screws 18 is discharged through the slit. It is preferable that all the serum water containing the solvent discharged through the slit be recovered and sent to the solvent purification step. The distance between the slits of the first dewatering barrel 20b1 is preferably larger than the distance between the slits of the second dewatering barrel 20e described later, and it is preferable to select a wedge type screen of about 0.1 to 0.2 mm.

A washing water supply barrel 20c is connected to the downstream side of the first dehydration barrel 20b1 via a normal barrel 20b2. A cleaning water supply port 50 is provided in the barrel 20c.
Is provided, from which washing water is supplied into the barrel 20c. The cleaning water supply port 50 may be a commercially available one with a check valve, but minimizing the clearance between the screw 18 and the flight is an effective means for preventing the supply port 50 from being closed. In this embodiment, fresh process water is used as the cleaning water.

The amount of water to be supplied to the washing water is preferably about 1: 1 to 1:30 by weight based on the rubber-like polymer component. If the amount of the washing water is too large, the washing water is not effectively used, and the recovery of the washing water becomes insufficient, which may cause the rubber polymer to be undried. Further, the temperature of the water provided for the washing water is preferably warm water of 40 ° C. or higher. This is because the cleaning effect is improved.

A barrel 20d is usually mounted downstream of the washing water supply barrel 20c. Usually, the barrel 20d has a temperature control means for controlling the inside of the barrel to a predetermined temperature. A second dewatering barrel 20e is connected to a stage subsequent to the barrel 20d. The second dewatering barrel 20e is provided with a wedge screen type slit or the like, and discharges and collects the washing water supplied by the washing water supply barrel 20c. The slit gap of the barrel 20e is preferably about 0.05 to 0.1 mm. The washing water collected here contains a few percent (eg, 3%) of the washed solvent (solvent), and includes fine crumbs leaked from the wedge screen. When used and supplied to the suction port 30 of the pump, all solvent and fine crumb will be recovered. At the same time, it leads to reduction of process water consumption.

The barrels 20f to 20n for the deaeration and drying step are connected to the second stage of the second dewatering barrel 20e.
In the earlier barrels 20a to 20e before that, the temperature of the barrel is preferably set to about 40 to 70 ° C.
It is preferable to keep the temperature at ~ 170 ° C. If the temperature of the barrel in the previous stage is low, the cleaning effect is reduced, and if it is too high, the serum and cleaning water are gasified, causing breathing,
The smooth flow by the twin screw 18 is impeded. Also, if the temperature of the barrel at the subsequent stage is too high, the product will be deteriorated. Conversely, if it is too low, degassing will be insufficient.

Of the barrels at the subsequent stage, an atmospheric vent barrel 20g connected to the rear stage of the normal barrel 20f is provided with an atmospheric vent 52 communicating with the atmospheric pressure and discharging vaporized substances. The solvent and water contained in the slurry are volatilized and removed. Subsequent to the atmospheric vent barrel 20g, a normal barrel 20h, 20i, a vacuum vent barrel 20j, a normal barrel 20k, 20l, a vacuum vent barrel 20m, and a die mounting barrel 20m are mounted in this order. Vents 54 and 56 are attached to the vacuum vent barrels 20j and 20m.
Is connected to a vacuum pump or a vacuum tank so as to forcibly exhaust volatile components contained in the rubbery polymer in the barrel.

These bent barrels 20g, 20j, 20
In the case of m, when the gas is released, the rubbery polymer component inside may vent up or flake up, thereby blocking the gas passage. In order to prevent such a point, it is preferable that a wedge-shaped cut is made on the inner surface of the vent block in the vent barrels 20g, 20j, and 20m to allow the rubber-like polymer component to bite into the barrel.
If vent up or flake up is more severe, the vent barrels 20g, 20j, and 20m may be formed as slit barrels.

Screws 18 for these divided barrels
The configuration of No. 18 is shown below. As shown in FIG. 4, the area corresponding to the feed barrel 20a and the first dewatering barrel 20b1 is a forward screw 60. Moreover, the valleys of the screws 18, 18 are deepened and the pitch is increased,
The bulky crumb having a high water content is quickly sent to the subsequent process. This is because, although this part is a closed system, it is not pushed by the discharge pressure of the pump with a crushing function, but is pushed by the rotation of the screw in a normal pressure system.

As shown in FIG. 4, one forward kneading disk 62 and one reverse kneading disk 63 are provided on the screws 18, 18 located in the normal barrel 20 b 2 on the rear side of the barrel 20 b 1 for discharging the serum. And are mounted in series. The subsequent screws 18 in the washing water supply barrel 20c are equipped with two sequential kneading disks (not shown), and the subsequent normal barrel 2
One reverse kneading disc (not shown) is mounted on the screws 18 in the area 0d to improve the mixing of the washing water and the crumb and to extract the soap. A dewatering barrel 20e and a normal barrel 20f are connected successively after the normal barrel 20d, and one normal kneading disk 68 and one reverse kneading disk 69 are provided in the normal barrel 20f. Are installed in series.

As shown in FIG. 4, reverse screws 64, 70, as shown in FIG.
74 and progressive screws 66, 72, 76 are arranged alternately. In order to prevent the screws 18, 18 from being heated by frictional heat or the like during the transfer of the rubber-like polymer,
As shown in FIG. 5, the inside of the screw 18 in the axial direction is hollow substantially over the entire area, and a pipe member 78 is inserted into the hollow part. A cooling water supply pipe 80 is inserted into the pipe member 78. A cooling medium whose temperature is controlled in advance through a control valve or the like is supplied to this pipe 80,
The cooling medium supplied from the pipe flows through the inside of the pipe member 78 in the axial direction, and then is discharged from an end outlet of the pipe member 78. As a result, screw 1
8 is cooled from the inside.

In the drying device 16 according to the present embodiment, the slurry containing the crushed crumb supplied from the feed port 24 is sent to the downstream side by the rotation of the left and right screws 18, 18 in the same direction, and is sent in the order shown in FIG. When the slurry reaches the kneading desk 62, the reverse kneading disk 63, and the reverse feed screw 64, the slurry is transported in the reverse direction and a squeezing action occurs, and the serum water is separated from the slurry. It is discharged to the outside through the slit of the first dewatering barrel 20b1 shown.

Thereafter, the washing water is supplied in the washing water supply barrel 20c, the slurry is washed, and the washing water is collected in the dewatering barrel 20e. By such washing, a part of the solvent contained in the slurry is washed away by the washing water. Then, barrels 20f to 20 shown in FIG.
By n, the slurry is dried and degassed, and finally, a sheet-shaped or linear-shaped molded product (product) made of a rubber-like polymer in a dry state is obtained from a die mounted on the barrel 20n.

In the manufacturing method using the rubber-like polymer manufacturing apparatus 12 according to this embodiment, the cement-like rubber solution and the coagulating liquid are separately separated from each other by the rotary blade 36 and the rotary blade of the pump 14 having a crushing function. The rubber solution and the coagulating liquid are brought into contact immediately before the inlet of
To the drying device 16. For this reason, a rubber-like polymer precipitates before the rotary blade 34 of the pump 14, and the deposited rubber-like polymer is crushed by the rotary blade 34, and a rubber-like polymer having a size suitable for transportation is provided. The slurry containing the polymer crumb is sent to the drying device 16. In the drying device 16, serum is recovered from the slurry containing the rubbery polymer,
Thereafter, the rubbery polymer is washed with washing water and then degassed and dried. It was confirmed that the dry rubber-like polymer thus obtained had a quality equal to or higher than that of the rubber-like polymer obtained by the conventional method and apparatus.

Therefore, in the production method using the production apparatus 12 for a rubbery polymer according to the present embodiment, it is possible to reduce the conventionally used coagulation device comprising a coagulation tank,
It is possible to reduce the number of processes and equipment, and to reduce equipment costs and manufacturing costs. Further, the operation is simplified, the loss of the product is reduced even when the type of the rubber-like polymer to be produced is switched, the switching time can be shortened, and the operability is improved. Further, in the present embodiment, a rubbery polymer having high tackiness or a rubbery polymer having low Mooney viscosity can be easily produced.

Further, in the present embodiment, the accuracy of measurement of raw materials or products is significantly improved, and automation of the manufacturing process can be facilitated. That is, in the present embodiment, the flow rate of the cement-like rubber solution fed to the pump 14 with the crushing function can be accurately measured, and the amount is supplied to the drying device 16 as it is. Not only can it be obtained, but also, for example, other components can be easily introduced in proportion to the amount of crumb.

The present invention is not limited to the above-described embodiment, but can be variously modified within the scope of the present invention.

For example, the barrels 20a to 20 shown in FIG.
The number of n is not particularly limited and can be variously modified. Further, the screw configuration can be modified by variously selecting the barrel configuration.

[0055]

EXAMPLES Hereinafter, the present invention will be described with reference to more specific examples, but the present invention is not limited to these examples.

Embodiment 1 A pump 14 with a crushing function and a drying device 16 shown in FIGS.
Was prepared. As the pump 14, a model HD4MCs-SC manufactured by Komatsu Zenoa Co., Ltd. was used, and the structure of the suction port 30 was improved using an adapter 38 as shown in FIGS. The rotation speed of the pump is
1750 rpm, the flow capacity was 10 m ³ / H, and the head was 20 m. Further, as the drying device 16, a twin-screw extruder (TEM-50B-manufactured by Toshiba Corporation) is used.
12 / 4V, L / D = 41.5), so that the cleaning process can be performed. The output of the dryer drive motor is 5
The power was 5 kW, the maximum number of revolutions was 440 rpm, and the number of barrels was 12. The configuration of the screw was such that the collection of serum, the cleaning of the rubbery polymer, and the degassing and drying described in the above-described embodiment were conveniently performed by the respective barrels.

As the rubber solution supplied from the cement transport pipe 44 shown in FIG. 1, a rubber solution comprising NBR dissolved in an acetone solvent was used. The rubber content was 12 to 13% by weight based on the whole solution. As the coagulated water supplied from the coagulated water transport pipe 46, water collected by the dehydration barrel 20e of the drying device 16 was used.
The supply flow rate of the rubber solution was 7.5 l / min, and the supply flow rate of water was 15 l / min.

The washing water supply barrel 20c was supplied with 15 liters of fresh water per minute. Vacuum vent 54,
56 was connected to a decompression tank having a vacuum of 20 Torr.

When the degree of drying of the rubber product obtained from the barrel 20n at the last stage of the drying apparatus was examined, the moisture content was 0.24% by weight based on the whole, and was obtained by a conventional method. It was confirmed that the quality was equivalent to that of rubber products. Further, when the vulcanization curve of this rubber product was examined, it was confirmed that the quality was equal to or higher than that of the rubber product obtained by the conventional method. Furthermore, the residual ratio of the solvent in the rubber product obtained by the method of this example is 0.03% by weight based on the whole, and the quality is equal to or higher than that of the rubber product obtained by the conventional method. Was confirmed.

[0060]

As described above, according to the production method using the production apparatus for a rubbery polymer according to the present invention, a large-sized coagulation apparatus conventionally used can be reduced, and the process and equipment can be reduced. Can be reduced, and equipment costs and manufacturing costs can be reduced. Further, the operation is simplified, the loss of the product is reduced even when the type of the rubber-like polymer to be produced is switched, the switching time can be shortened, and the operability is improved. Further, in the present invention, even a rubbery polymer having a high tackiness or a rubbery polymer having a low Mooney viscosity can be easily produced without the rubbery polymer adhering to the coagulation tank.

Further, according to the present invention, the accuracy of measurement of raw materials or products is remarkably improved, and automation of the manufacturing process can be facilitated. That is, in the present invention, the flow rate of the cement-like rubber solution fed to the pump with the crushing function can be accurately measured, and the amount is supplied to the drying means as it is, so that a stable operation can be obtained only. Alternatively, for example, other components can be easily added in proportion to the amount of crumb.

[Brief description of the drawings]

FIG. 1 is a schematic view of an apparatus for producing a rubbery polymer according to one embodiment of the present invention.

FIG. 2 is an exploded perspective view of a pump with a crushing function.

FIG. 3 is a cross-sectional view of the drying device.

FIG. 4 is a schematic view of a twin screw.

FIG. 5 is a schematic sectional view of a screw.

FIG. 6 is a schematic view showing a part of an apparatus for producing a rubber-like polymer according to a conventional example.

[Explanation of symbols]

 Reference Signs List 12: Rubber polymer production device 14: Pump with crushing function 16: Drying device 18: Screws 20a to 20n: Barrel 24: Feed port 30: Suction port 32: Discharge port 34: Rotating blade 36: Rotating blade 38: Adapter

Claims (3)

[Claims] A coagulating liquid is added to a cement-like rubber solution,
A method for producing a rubbery polymer in which a rubbery polymer component is precipitated and a rubbery polymer component in a dry state is obtained by drying the deposited rubbery polymer component, comprising a cement-like rubber solution and a coagulating liquid. And, separately,
A method for producing a rubber-like polymer, comprising supplying the rubber solution immediately before the inlet of a rotary impeller of a pump having a crushing function, bringing the rubber solution into contact with a coagulating liquid, and immediately sending the rubber solution to a drying means by the pump. 2. A cement feeding means for feeding a cement-like rubber solution, a coagulation liquid feeding means for sending a coagulation liquid for precipitating a rubber-like polymer component in the rubber solution, and the cement feeding means and the coagulation liquid feeding means. A pump with a crushing function, the suction port of which is configured so that the rubber solution and the coagulating liquid sent by the pump are brought into contact immediately before the entrance of the rotary blade, and a crumb-like rubber crushed and sent by the pump with the crushing function A drying means for drying a slurry containing the polymer to obtain a dry rubbery polymer. 3. The method according to claim 1, wherein the drying means is supplied with washing water to wash the rubbery polymer before drying.