JPH01230605A - Method and apparatus for production of coagulated resin - Google Patents

Abstract

PURPOSE:To recover efficiently a coagulated resin from a latex by forming a coagulated mass obtd. from a thermoplastic resin latex and a coagulating liq. into small granules to prepare a slurry of coagulated particles and bringing it into contact with steam in a specified tubular apparatus. CONSTITUTION:A latex of a thermoplastic resin in a heat insulating tank for the latex and a coagulating liq. in a heat insulating tank for the coagulating liq. are respectively fed from feed ports 1 and 2 by means of a metering pump into a coagulating section 3 and brought into contact with each other at a softening temp. or below of the thermoplastic resin to obtain a coagulated mass, which is formed into small granules in a granulator 4 for coagulated particles to form a slurry of coagulated particles. Then, this slurry is fed to a homogenizer 5 for the coagulated particles having a mixing mechanism such as a mixing element 10 to make the particle diameter uniform and then fed to a steam contacting part 6 having a mixing element 10 to bring it into contact with steam introduced from a feed port 7 at a softening temp. or higher of the thermoplastic resin and a slurry of coagulated particles is led flow out from an outlet 8. Furthermore, this slurry is dehydrated and dried and, pelletized as necessary.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing coagulated resin from thermoplastic resin latex and an apparatus for producing the same.

(Conventional technology) Thermoplastic resin latex obtained by emulsion polymerization etc. (hereinafter referred to as
As a method of recovering polymerized products (abbreviated as latex), inorganic salts and inorganic acids are added to the stabilized latex.
A coagulation operation is generally carried out in which the micelles are destroyed and the polymer particles are agglomerated by adding one or more organic acids or hydrophilic polar solvents to obtain a polymer in the form of a lump. After washing, dehydrating, and drying the coagulated particles obtained by the coagulation operation, stabilizers and other additives are often added to the particles, or they are mixed with other polymers and then used as pellets. Although it is.

The difficulty of these series of operations after coagulation largely depends on the state of the aggregated particles obtained by coagulation (two-particle size distribution, bulk density, hardness, etc.). for example.

With coagulated particles containing many fine particles, only a wet powder with a high moisture content can be obtained even after the washing and dehydration steps, resulting in a high coagulant residual rate. In addition, it may cause clogging of the centrifuge cloth during the dehydration process, resulting in poor dehydration. In addition, in the drying process,
Problems such as scattering of fine particles 2 and a decrease in the recovery rate, as well as poor penetration into the rug when the obtained particles are made into pellets, occur. - In the case of coagulated particles with many large particles, it is difficult to remove the water contained therein, and this also causes transportation troubles such as clogging of pipes. therefore,
It has always been desired to establish a coagulation method that efficiently recovers the desired coagulated particles. The specific methods are roughly divided into:
(1) Stirring tank method in which latex and coagulation liquid are stirred and mixed in a stirring tank (% Publication No. 46-17121, JP-A-57
-98503 Publication), (21 Latex and coagulation liquid are brought into parallel flow and the two liquids are brought into contact in a single laminar flow state (co-current contact method)
(Japanese Patent Publication No. 46-32055), (31 spray one type (Japanese Patent Publication No. 57-5256, Japanese Patent Application Laid-Open No. 56-3040)
3, JP-A No. 56-95905), [4) Extrusion shaping method (Japanese Patent Publication No. 42-22295, 2% Publication No. 4)
2-22684, Japanese Patent Publication No. 50-17227), etc.

(Problems to be Solved by the Invention) In the stirred tank system, the particle size distribution of coagulated particles cannot be avoided due to its structure, and there is a limit to operation at a high concentration of coagulated particles. Specifically, the co-current contact method described in Japanese Patent Publication No. 46-32055 is a method in which latex flows out from a nozzle placed in the flow of coagulating liquid. The size of the particles is determined.

Although this method has been improved in narrowing the particle size distribution of coagulated particles, it is not possible to increase the nozzle hole diameter in order to suppress the generation of giant particles.

Problems with nozzle blockage are likely to occur.

K operating at high coagulated particle concentrations has limitations.

The one-spray method has the drawbacks that there are limitations on the latex that can be applied and that the equipment becomes larger.

In the extrusion shaping method, generally, solidified particles are obtained as pellets with a certain shape, but these pellets are easily broken and, in some cases, have the disadvantage of progressing to fine particles, so a curing process is required. Equipment becomes more complex and larger. Furthermore, although the method described in Japanese Patent Publication No. 50-17227 is improved in terms of process simplification, there is a limit to the latex softening temperature of 100°C to 300°C, and it is not suitable for mass processing. Not suitable.

The present invention solves these problems.

When recovering coagulated resin from latex, dehydration, drying,
The present invention relates to a method for continuously obtaining coagulated particles in a highly concentrated slurry state with an average particle size and particle size distribution that allow each process such as pelletization to be carried out efficiently, and an apparatus for producing the same.

(Means for Solving Problem 1!f!) The present invention provides a step (a) of bringing a thermoplastic resin latex and a coagulating liquid into contact with each other at a temperature below the softening temperature of the thermoplastic resin to produce a coagulated lump. , step (b) of pulverizing the coagulated agglomerates to produce a coagulated particle slurry;

A step of making the coagulated particle slurry 0 particle size uniform (c1 and a step of bringing the coagulated particle slurry with a uniform particle size into contact with steam at a temperature equal to or higher than the softening temperature of the core thermoplastic resin)
The present invention relates to a method for producing a coagulated resin and an apparatus for producing a coagulated resin, characterized by containing dl.

The thermoplastic resin latex used in the present invention is not particularly limited as long as it can be obtained by ordinary emulsion polymerization or the like. Specifically, rubbery polymers include vinyl aromatic hydrocarbons such as styrene and α-methylstyrene, acrylonitrile,
Vinyl cyanide compounds such as methacrylonitrile, acrylic acid esters.

Graft polymer latex obtained by polymerizing one or more vinyl monomers such as methacrylic acid ester, vinyl (co)polymer latex obtained from one or more of the above vinyl monomers. , a polymer mixed latex containing the graft polymer latex and the vinyl (co)polymer latex, etc. Additives such as antioxidants, heat stabilizers, and light stabilizers are added to these thermoplastic resin latexes. There is no problem even if it is added.

The coagulating liquid used in the present invention contains a coagulating agent. A coagulant has the function of coagulating and separating the resin components of thermoplastic resin latex (hereinafter simply referred to as latex). As the coagulant, any one commonly used for coagulating latex may be used, and inorganic salts, inorganic acids, organic acids, etc. can be used. Specifically, calcium chloride and sodium chloride.

Examples include magnesium sulfate, aluminum sulfate, potassium alum, sulfuric acid, hydrochloric acid, and formic acid. The amount of these coagulants to be used is appropriately determined depending on the resin concentration of the latex, coagulability, amount of emulsifier, and coagulation ability of the coagulant used. These coagulants have both sufficient coagulation ability and economic efficiency.

Generally, in the case of inorganic salts, the resin content in latex is 100%
It is preferable to use 2 to 10 parts by weight,
Acids account for 1.0 to 1.5 of the emulsifier contained in latex.
It is preferable to use double weight. The coagulant is used by dissolving it in a solvent such as water to form a coagulating liquid.

Next, each step of the present invention will be explained.

First, step (a) is a step of bringing the latex and the coagulating liquid into contact to obtain a coagulated lump, and step (bl) is a step of coarsely crushing the latex and dispersing the coagulating liquid inside the coagulated lump to obtain a coagulated particle slurry. The contact method is shown in Figure 3 (b).
There is a parallel current method using a device as shown in 1. Also,
There is a stirring and mixing method using a device as shown in FIG. 3 (3), which combines contact (step a) and coarse crushing (step b). In both figures, 1 is a latex inlet, and 2 is a coagulation liquid inlet. The stirring and mixing method is preferable from the point of view that coagulated particles can be handled at a high concentration. In order to prevent troubles due to blockage of the coagulated resin in the coagulation section outer cylinder 9 or latex inlet 1 during the process (al), or troubles caused by the formation of large coagulated lumps, the latex and coagulation liquid are kept at a temperature below the softening temperature of the resin contained in the latex. It is necessary to bring the resin into contact at a temperature of about 100 ml, preferably below the softening temperature of the resin, in order to prevent excessive granulation.

It is necessary to contact the resin at a softening temperature of −30° C. or higher.

Note that the softening temperature in the present invention refers to the temperature at which it can be determined that the resin particles have started deforming in a constant temperature increase test using a Koka type flow tester.

The contact temperature in step (a) can be adjusted by keeping the latex and coagulant at a predetermined temperature in advance and supplying them.

Next, in step (b), the coagulating liquid is dispersed inside the coagulated mass obtained in step (a), and sufficient stirring power is applied depending on the method in order to prevent troubles in step (c1) caused by residual uncoagulated latex. In addition to ensuring a residence time of 2 seconds or more,
Preferably, it is necessary to secure 5 seconds or more. Incidentally, increasing the residence time more than necessary leads to an increase in the size of the apparatus, so the decision should be taken also from an economic point of view.

It is preferable to carry out step (bl) using a capillary because the apparatus is simple and suitable small lumps can be obtained. When using a capillary, sufficient stirring ability is to be obtained.

The relationship between flow velocity and pipe diameter is flow velocity/pipe diameter>7 (unit: 1/sec)
It is preferable that the relationship between the tube length and the tube diameter is such that tube length/tube diameter>(1,12X slurry-concentration).

Next, in step (c), on the surface of the coagulated particles present in the coagulated particle slurry obtained in step (b), the points of application are momentarily uneven and move over time to become statistically uniform. By applying shear stress, the fine particles constituting the flocculated particles are rearranged, and at the same time, the flocculated particles are completely consolidated, and at the same time, at the contact points where the bonding force between the fine particles constituting the flocculated particles is weak,
This is a step in which this bond is broken to obtain a slurry of aggregated particles having a statistically uniform particle size.

If the process moves from step (b) to step fd) without going through this step, troubles will occur in step (d) due to the formation of giant particles. However, it may be possible to omit it if a stirring-mixing type device is used in step (al).As step (c), the stirring-type mixer type shown in Fig. 4(a) and (b), Fig. 4 There are methods such as [C) using a static mixer, and the method using a static mixer is preferred from the standpoint of being able to handle coagulated particles at a high concentration. Furthermore, various types of mixing elements for static mixers have been considered and put into practical use, as described in Table 6.2 on page 129 of "Advances in Chemical Engineering" 16 (Maki Shoten Publishing). , especially static mixers (K
It is preferable to use one that has a simple structure and is suitable for handling coagulated particle slurry, such as those manufactured by Enics (trade name). In addition.

Preferably, there are six or more mixing elements.

This step is preferably carried out at a temperature below the softening temperature of the resin in order to prevent troubles due to the formation of giant particles.
Especially below the softening temperature of the resin, and the softening temperature of the resin -30℃
It is preferable to carry out the above. Further, conditions such as flow rate and residence time for obtaining coagulated particles having a uniform particle size in the two-step process are determined depending on each mixer selected to be used.

Step (d) is heating the coagulated particle slurry whose particle size has been made uniform in step FC+ to a temperature above the softening temperature of the resin, preferably above the softening temperature of the resin, but below the softening temperature of the resin +30°C by contacting it with high temperature steam. This is necessary to uniformly enlarge the particles.

It is possible to adjust the particle size of the coagulated particles by adjusting the temperature of the coagulated particle slurry in this step, but if the temperature is below the resin softening temperature, the particles will not enlarge, and the resin softening temperature + 30'C Exceeding this value tends to cause problems due to the generation of giant particles. In addition, as a heating method,
A heating method using steam contact is necessary because it can heat quickly and uniformly and prevents adhesion to walls. The temperature in step (d) can be determined by adjusting the temperature and flow rate of the steam. Steam contact methods include a pipe type as shown in fal in Figure 5, and a steam contact type as shown in Figure 5 [b].
There is a tubular type having a mixing element inside as shown in (), and the latter is preferable from the viewpoint of making the particle size distribution of coagulated particles uniform and being able to handle coagulated particles at a high concentration. Further, in order to achieve uniform contact with steam, the flow rate of the coagulated particle slurry is preferably 0.5 to 2 m/sec, and the residence time is preferably 0.1 second or more. The method for producing a coagulated resin of the present invention is carried out using a single management device in which nine device mechanisms, for example, step (a), step (b), step FC), and step (d), are successively connected. Figures 1 and 2
It is particularly preferable to use a device as shown in the figure, since troubles such as blockage are less likely to occur.

An example of a management device for carrying out the manufacturing method of the present invention will be described in detail below. Figures 1 and 2 are.

An example of this device is shown, and FIG. 1 is an external view, and FIG. 2 is a sectional view of the device shown in FIG. 1. The coagulating section 3 has a latex inlet 1 and a coagulating liquid inlet 2, and the latex and the coagulating liquid are brought into contact at a temperature lower than the softening temperature of the resin. Each part can be supplied to the coagulation section 3 from the latex heat retention tank and the coagulation liquid heat retention tank through metering pumps, respectively. The coagulated mass obtained by bringing the respective parts into contact passes through the coagulated particle coarse crushing section 4 and becomes a coagulated particle slurry.

The preferred relationship among the pipe length, pipe diameter, and flow rate of the coagulated particle coarse crushing section 4 is as described above. A coagulated particle homogenizing section 5 is connected to the coagulated particle crushing section 4 . The solidified particle homogenizing section 5 has a mixing mechanism such as a mixing element 10. Subsequently, the steam contact portion 6 is connected. The steam contact section 6 has a steam introduction lower, and further has a mixing element 10 and a coagulated particle slurry outlet 8 for uniformly contacting the steam. The temperature of the steam contact area can be determined by adjusting the steam flow rate.

Each part is connected by a smooth flow path, that is, a pipe line with the same inner diameter, by flange connection or the like.

3 containing uniform coagulated resin particles obtained by the present invention
The rally is dehydrated using a centrifugal filter or the like, and the resulting wet powder is dried using a flash dryer, paddle dryer, or the like to obtain coagulated resin particles.

The obtained coagulated resin particles can be pelletized using, for example, a twin-screw or single-screw extruder, and can be made into a thermoplastic resin for molded products.

(Operation) In step fa), agglomerates are generated simply by bringing the latex into contact with the coagulation liquid. At this time, if the temperature is higher than the softening temperature of the resin, the operation becomes troublesome, such as making the latex nozzle finer or requiring strong stirring in order to maintain a uniform coagulated particle size.

Accumulation of adhesion due to the latex condition is unavoidable and clogging problems are likely to occur. In order to solve these problems, the coagulation section only has the function of coagulating the latex by operating below the softening temperature of the resin.

It is designed to accommodate a wide range of operating conditions.

Step (bl is a preparatory step for coarsely crushing the coagulated mass obtained in the coagulation section so that no uncoagulated latex remains, and obtaining particles with a uniform particle size in step fc).

Step (bl) is a process in which shear stress due to fluid viscosity is generated when the fluid flows through the two circular tubes, so a moderately small solidified mass can be obtained by using an appropriate tube diameter and flow rate. The small coagulum obtained in step fbl is a random agglomeration of latex particles.

Step (c1) is a preparatory step for applying uniform shear stress to the randomly aggregated coagulated particles to consolidate the two particles, and at the same time making the particle diameter uniform to ensure uniform enlargement in step (d). In (c), if a static mixer is used, the shear stress can be applied uniformly, and a uniform particle size can be obtained.

In step (d), steam is brought into direct contact with the coagulated particle slurry that has been homogenized in advance, and the slurry is uniformly heated to a temperature higher than the softening temperature of the resin in a short period of time, so that the coagulated particles are fused together to form a denser and more uniform enlargement. becomes possible. Therefore by adjusting the heating temperature.

The average particle size can also be easily adjusted. Also in step (d), it is preferable to use a static mixer because uniform shear stress can be obtained.

Furthermore, in the second aspect of the manufacturing apparatus of the present invention, troubles due to blockages are less likely to occur because the entire apparatus can be constructed of pipes.

(Example) Next, the present invention will be explained in more detail with reference to Examples.

Example 1 A latex was obtained using the following polymerization recipe.

(1) Production of cross-linked acrylic rubber latex Add emulsifiers (fatty acid soap, Nonsal TN-
1. Aqueous solution in which 12M parts of Nippon Oil & Fats ■Product name) are dissolved,
An aqueous solution prepared by dissolving 1.2 parts by weight of potassium persulfate and 0.24 parts by weight of sodium sulfite in 200 parts by weight of separately prepared ion-exchanged water and 300 parts of polybutadiene rubber latex (solid content) were charged into a reaction vessel and mixed. After stirring, a monomer solution consisting of 1t76 parts of butyl acrylate AM and 24 parts of triallylisocyanurate was added, and after purging with nitrogen, the temperature was raised.

When the polymerization rate reached 40%, an emulsifier (Nonsal TN-
1) 200 parts by weight of ion-exchanged water in which 4 parts by weight was dissolved was added.

Polymerization was carried out at 60 to 65°C for 2 hours and at 85 to 90°C for 3 hours to obtain a crosslinked acrylic rubber latex (1). The weight percentage was 99%.

(2) Emulsion polymerization T in the presence of crosslinked acrylic rubber latex
In a container equipped with a K homo mixer (manufactured by Tokushu Kika Kogyo ■),
A solution of 28 parts by weight of Rongalit and 6.4 parts by weight of an emulsifier (Nonsal TN-1) dissolved in 1200 parts by weight of ion-exchanged water was added, followed by 600 parts by weight of styrene and 200 parts by weight of acrylonitrile.

A monomer solution consisting of 2.8 parts by weight of cumene hydroperoxide and 22 parts by weight of tertiary dodecyl mercaptan was added, and after purging with nitrogen, the stirring speed was set to K 4 m/S.
After homomixer treatment with EC for 5 minutes, 2001 HL parts (solid content) of cross-linked acrylic rubber latex was added, and homomixer treatment was performed for 30 minutes at a stirring speed of 4 m/see.
I did it for a minute. Afterwards, transfer to a reaction vessel purged with nitrogen, and
Polymerization was carried out at 0°C for 12 hours and then at 90°C for 4 hours.

When the softening temperature of the obtained thermoplastic resin was measured, it was 85.
It was ℃.

The conditions for measuring the softening temperature are shown below.

Measuring device: Shimadzu flow tester CFT-500 Cylinder cross-sectional area: 1 c Load: 10 kgf Temperature increase rate: 3° C./min Sample lid: Approximately 1 g Pushinger descent amount on the vertical axis and 9 hours on the horizontal axis.

This relationship was graphed, and the intersection of the continuation of the first rise of the obtained curve and the extension of the horizontal line before deformation was defined as the deformation start point, that is, the softening temperature.

An attempt was made to recover the υ solidified resin from the obtained latex in the following manner. The solidified resin manufacturing apparatus used was of the type shown in FIG. 2, and its specifications were as follows.

Coagulation and coarse crushing section outer cylinder inner diameter 25anaφ Coagulation and coarse crushing section length 1750mu + latex inlet inner diameter 1
7.5 weight m+φ coagulated particle homogenization section ■Noritake gN6
0 type static mixer (inner diameter 25anφ, length 275om+, number of elements 6
) Steam contact part ■Kutsuka NET- made by Noritake
D25 type (inner diameter 25 mm, length 425 aua, number of elements 10
f) The thermoplastic resin latex (11 with a fat concentration of 33% by weight) obtained by the above polymerization at 70°C was heated at a flow rate of 240 kg/
from the latex inlet 1 of the coagulation section 10.

Further, a coagulating liquid (an aqueous solution containing 2% by weight of potassium alum) at 70° C. is supplied to the coagulating liquid inlet 2 of the coagulating section 10 for 9 hours in streams 1 to 240 and brought into contact with each other to obtain a coagulated particle slurry. This coagulated particle slurry is passed through a coagulated particle coarse crushing section 4, then guided to a coagulated particle homogenizing section 5, and further mixed with steam in a steam contact section 6, heated to 95°C, and then passed through a coagulated particle slurry outlet 8. A coagulated slurry having a coagulated particle concentration of 16.5% by weight was obtained.

After washing the resulting coagulated particle slurry with water, dehydration and drying yielded highly hard and homogeneous granular coagulated particles. When this was sieved, the powder properties were measured as shown in Table 1. was obtained.

Particle size: Z: No giant particles larger than 38 weight m+, and particle size: 0
, the number of fine particles of 25 ttm or less was small.

Comparative Example 1 Coagulation liquid (potassium alum 5
After setting 16 to 9 (aqueous solution) at 70 °C, 9 to 80 °C latex at 70 °C, the same as the latex used in Example 1, was continuously added to the stirring tank over 2 hours. and solidified. After coagulation.

Further, the temperature in the stirring tank was raised to 95° C. and held for 1 hour, and then the powder characteristics of the coagulated particles were measured in the same manner as in Example 1. The results are shown in Table 1. Diameter 'L compared to Example 1
It is clear that there are many giant particles with a diameter of 38 II m or more and fine particles with a diameter of 0.25 mm or less, and the uniform number is also low, which is not preferable.

Example 2 A coagulated particle slurry was obtained using the same latex/coagulating liquid and coagulating apparatus as in Example 1, and under the same conditions and method, except that the temperature of the coagulated particle slurry was raised to 98° C. in the steam contacting part. Further, the powder characteristics of the coagulated particles were measured in the same manner as in Example 1, and the results are shown in Table 1. The results were good, with even fewer fine particles with a particle size of 0.25 mm or less than in Example 1.

Example 3 A coagulated particle slurry was obtained using the same latex, coagulating liquid, and coagulating device as in Example 1, and using the same conditions and method, except that the temperature of the coagulated particle slurry was raised to 90° C. in the steam contacting part. Furthermore, the powder characteristics of the coagulated particles were measured in the same manner as in Example 1, and the results are shown in Table 1.
Although the number of fine particles with a particle size of 0.25 am or less increased compared to that of the previous example, good results were obtained. Also, Example 1. FIG. 6 shows the results of Examples 2 and 3 regarding the relationship between the temperature of the coagulated particle slurry in the steam contact area, the weight average diameter, and the uniform number n. It is clear from FIG. 6 that the weight average particle size can be adjusted while maintaining the sharpness of the particle size distribution by adjusting the temperature at the steam contact area.

Comparative Example 2 The same latex as in Example 1, except that the temperature of the coagulated particle slurry was raised to 80° C. in the steam contact area.

A coagulated particle slurry was obtained using a coagulating liquid and a coagulating device under the same conditions and method. Furthermore, the powder characteristics of the coagulated particles were measured in the same manner as in Example 1, and the results are shown in Table 1. If the temperature of the steam mixing section is lower than the resin softening temperature of 85°C, there will be many fine particles with a particle size of 0625 mm or less, and
It is clear that the bulk specific gravity is relatively low, which is not desirable.

Example 4 The solidified particle slurry was heated to 90°C in the steam contact area,
The same latex, coagulation liquid, and coagulation device as in Example 1 were used, and the same conditions and method were used, except that the latex flow rate was 480 kg/hour and the coagulation liquid flow rate was 240 kg/hour, respectively, to the coagulation section. A coagulated particle slurry was obtained. At this time, the coagulated particle concentration at the coagulated particle slurry outlet lower was 22% by weight. Furthermore, the powder characteristics of the coagulated particles were measured using the same method as in Example 1, and the results are shown in Table 1. As shown in step (a), the latex and coagulation liquid are brought into contact at a temperature below the softening temperature of the resin, and in step [b) the latex is coarsely crushed to obtain a coagulated particle slurry, and in step (c) it is homogenized. The coagulated particle slurry thus obtained is heated to a temperature higher than the softening temperature of the resin in a step (dl), and the structure is such that a coagulated resin having a diameter of 9 particles can be produced at the heating temperature.

Therefore, coagulated particles with an average particle size distribution of 9 and a bulk specific gravity that can be efficiently processed in the subsequent post-processing process can be continuously obtained, and the average particle size can be easily adjusted by adjusting the temperature of the steam mixing section. It has the effect of being able to.

Further, by using the manufacturing apparatus of the present invention, it is possible to increase the density of coagulated particles and to widen the operating range of the particle size. Furthermore, it is possible to shorten the residence time and downsize the device.

[Brief explanation of the drawing]

FIG. 1 is an external view showing an example of the apparatus of the present invention used in the method of the present invention, FIG. 2 is a sectional view of FIG. 1, and FIG. 3 is a step (1) in the method of the present invention. a) and step (b)
), FIG. 4 is a sectional view of an example of the device used in step (c) in the method of the present invention, and FIG. 5 is a cross-sectional view of an example of the device used in step (dl) in the method of the present invention. The cross-sectional view of the example, FIG. 6, is a graph showing the relationship between the temperature of the solidified slurry, the weight average particle diameter, and the uniform number in step (d) (steam contact area). Explanation of symbols 1...Latex introduction Port 2...Coagulation liquid inlet port 3
...Coagulation section 4...Coagulation particle coarse crushing section 5.
...Coagulated particle homogenization section 6...Steam contact section 7...
・Steam inlet 8...Coagulated particle slurry outlet 9...Outer cylinder 10...Mixing element 11...Stirrer field (b) (b) s (3) (4) Σ

Claims (1)

[Claims] 1. Step (a) of bringing a thermoplastic resin latex and a coagulating liquid into contact with each other at a temperature below the softening temperature of the thermoplastic resin to form a coagulated lump, and forming the coagulated lump into small lumps. Step (b) of generating a coagulated particle slurry, step (c) of making the particle size of the coagulated particle slurry uniform, and heating the coagulated particle slurry with a uniform particle size and steam at a temperature higher than the softening temperature of the thermoplastic resin. A method for producing a coagulated resin, comprising a step (d) of contacting with the coagulated resin. 2. The method for producing a solidified resin according to claim 1, wherein step (b) is carried out using a thin tube. 3. The method for producing a coagulated resin according to claim 1 or 2, wherein step (c) and/or step (d) are carried out using a static mixer. 4. Step (a), step (b), step (c) and step (
4. The method for producing solidified resin according to claim 1, 2 or 3, wherein each step is carried out continuously in a tubular device in which device mechanisms for step d) are successively connected. 5. A coagulation section having a latex inlet and a coagulation liquid inlet;
It has a coagulated agglomerate crushing section for coarsely crushing the agglomerates to obtain a coagulated particle slurry, a coagulated particle homogenizing section for homogenizing the coagulated particle slurry, a steam inlet and a coagulated particle slurry outlet,
A coagulated resin manufacturing device that sequentially connects steam contact parts that bring coagulated particle slurry into contact with steam. 6. The apparatus for producing coagulated resin according to claim 5, wherein the coagulated lump crushing section is a thin tube. 7. The coagulated resin manufacturing apparatus according to claim 5 or 6, wherein the coagulated particle homogenizing section and/or the steam contacting section are static mixers. 8. The solidified resin manufacturing apparatus according to claim 5, 6 or 7, which is a single tube type apparatus.