WO2014196707A1

WO2014196707A1 - Device for manufacturing polymer latex resin powder and method for manufacturing polymer latex resin powder using same

Info

Publication number: WO2014196707A1
Application number: PCT/KR2013/012119
Authority: WO
Inventors: 김창술; 주민철; 이형섭; 정회인
Original assignee: (주) 엘지화학
Priority date: 2013-06-03
Filing date: 2013-12-24
Publication date: 2014-12-11

Abstract

The present invention relates to a device for manufacturing polymer latex resin powder and a method for manufacturing polymer latex resin powder using the same, wherein introduction of a non-continuous type screw into a reactor, which performs coagulation and aging, of the device for manufacturing polymer latex resin powder increases the efficiency of mixing steam, latex, and coagulant, lowers the water content ratio of slurry, improves the drying efficiency, and reduces the amount of coagulant used, thereby manufacturing polymer latex resin powder having excellent color and powder characteristics.

Description

Apparatus for manufacturing polymer latex resin powder and method for preparing polymer latex resin powder

The present invention relates to a device for producing a polymer latex resin powder and a method for producing a polymer latex resin powder using the same, and more particularly, a device for producing a polymer latex resin powder comprising a latex tank, agglomeration tank, a aging tank, a dehydrator and a dryer. In the process of agglomeration and maturation of the steam, latex and flocculant by introducing a discontinuous screw By increasing the mixing efficiency, it is possible to increase the drying efficiency by lowering the water content of the slurry, and to reduce the amount of flocculant used to produce a polymer latex resin powder having excellent color and powder characteristics, and an apparatus for producing the polymer latex resin powder using the same A method for producing a polymer latex resin powder.

The polymer material formed by emulsion polymerization is preferably processed into powder for reducing the volume, various applications and ease of handling. In order to obtain the polymer material formed by emulsion polymerization in powder, it is required to aggregate, dehydrate and dry the latex formed by emulsion polymerization.

Agglomeration of the emulsion polymerized polymer latex may be performed by breaking the stability of the latex particles stabilized by the emulsifier applied during the emulsion polymerization by a chemical method using various flocculants or by a mechanical method using a mechanical force by applying a strong shearing force. . The chemical method breaks the stability by using a different flocculant depending on the type of emulsifier used to secure the stability of the latex, and in the case of breaking the stability using the mechanical method, the repulsive force between the emulsifiers is applied by applying a strong shear force to the latex. Overcome and let the latex particles and particles stick together.

Rapid coagulation has been proposed as a method for preparing polymer latex into powder. In this method, an excessive amount of flocculant aqueous solution such as an inorganic salt and an acid is added to break the stability of the emulsifier, thereby rapidly agglomerating the polymer in the latex. The agglomeration of the polymer particles of latex is called coagulation, and the agglomeration of the polymer particles is called a slurry, and since they are physically weakly bound, they are easily crushed by an external shear force by an agitator. break-up phenomenon. Therefore, the first aggregated slurry is subjected to an aging process, which is a process of increasing the binding force by mutual penetration between chains by raising the temperature. The slurry thus produced is finally dehydrated and dried to obtain a powder form.

As described above, in the case of rapid agglomeration using an excessive coagulant, the latex stability is broken very quickly, so that the process of gluing the polymer latex particles occurs very quickly and disorderly. Due to such disordered aggregation, the apparent specific gravity is lowered, and the particle size distribution of the final particles is very wide.

1 is a view schematically showing an apparatus for producing a polymer latex resin powder according to the prior art. The apparatus comprises a latex storage tank (1), agglomeration tank (2), aging tank (3), a dehydrator (4) and a dryer (5).

First, the polymer latex stored in the latex storage tank (1) is introduced into the coagulation tank (2) through the polymer latex inlet line (11), and then the flocculant aqueous solution through the coagulant inlet line (12), and the water supply line (13) Water to adjust the solid content concentration is added to the polymer latex in the flocculation tank (2). The added solution of the flocculant serves to break the electrostatic stabilization by the emulsifier to agglomerate the polymer particles in the latex, and through this agglomeration process to obtain a polymer slurry. The agglomerated polymer slurry is transferred to the aging tank (3) and subjected to the process of aging by maintaining for 40 to 90 minutes under high temperature. The finally obtained slurry is dehydrated in the dehydrator (4) and then dried in the dryer (5), the final polymer powder is discharged through the polymer powder discharge line (15). The flocculant added in the dehydrator 4 is discharged through the flocculant discharge line (14).

However, the apparatus as described above is difficult to stir the slurry having a high viscosity, and also has a problem in that the efficiency of processing into a powder is inferior because the slurry is not smooth, the slurry having a high solid content in order to increase the dehydration and / or drying efficiency It is difficult to use, and therefore has a limitation that it can be operated only for slurries having a low solids content, and thus there is a problem that a lot of time, effort and energy are consumed in subsequent dehydration and drying.

In order to improve the above problems, a multistage continuous flocculation and aging process has been proposed. This process has the advantage of effectively aging the polymer slurry having a low solids content. However, it is not applicable to the slurry having a high solids content, and there is a problem in that the process efficiency is somewhat reduced because it has to go through several steps.

In addition, a slow coagulation process has been proposed to improve the powder characteristics of the final particles produced by controlling the coagulation rate through split dosing of coagulant. Since aggregation occurs in the secondary well region in which the energy barrier is present, the aggregation rate is slow and there is a possibility of rearrangement of the particles, so that spherical particles can be produced by regular filling. However, the overall amount of flocculant used is similar to that of rapid flocculation, and is merely a method of flocculation by performing split injection. Therefore, it is not possible to prevent the generation of wastewater due to excessive flocculant, and in the case of the primary flocculation tank, a small amount of flocculant is added to the rapid flocculation, so that the viscosity of the slurry rises, so that water must be added to the rapid flocculation to ensure flowability. It also has the disadvantage of having a high water content compared to rapid aggregation.

After both methods, the flowability of the polymer latex slurry produced after aggregation is influenced by the solid content, the particle size distribution of the slurry, and the inclusion water content of the slurry, and is particularly affected by the solid content. When the solids content of the slurry is more than a certain degree, the flowability of the slurry rapidly deteriorates and becomes a lump, thus making operation impossible. Therefore, in order to facilitate the flow of the slurry, an additional amount of water must be added during the flocculation process. The addition of excess water raises the energy costs incurred when the slurry is raised to the flocculation and maturation temperatures, and also generates excess wastewater during the dehydration process, thereby raising the post-treatment cost. In addition, the efficiency is lowered by not using steam directly, condensing in water as a medium to transfer energy to the slurry.

Another method of recovering the powder from the emulsion-polymerized latex is to recover the powder of the polymer latex by means of a gas-phase spray system. This method is a method in which a polymer latex is agglomerated and recovered into a spherical powder by spraying a polymer latex having a high solid content on the side through which an excessive flocculant flows using an atomizer. In this case, since the polymer latex is in contact with the flocculant while maintaining a high solid content, rapid flocculation is achieved at the moment of contact with the flocculant, thereby enabling spherical powder recovery that can be obtained in a high apparent specific gravity and a slow flocculation process. However, it is necessary to use an excessive flocculant to prevent unreacted, so that it is not possible to prevent the generation of excess wastewater, the clogging of the atomizer frequently occurs, it can be said to be disadvantageous in terms of process stability.

In addition, there are studies that control the particle size of the powder and improve the apparent specific gravity in the presence of an organic solvent, but in this case, it is disadvantageous that such powder characteristics can be secured only by using an excess of an organic solvent.

Another method is shear coagulation, which produces a slurry by applying shear force with strong mechanical force to agglomerate particles of latex. It applies a shear stress due to high speed rotation of 4,000 rpm or more without using a flocculant to prepare a polymer latex slurry. However, in the case of emulsion polymerized polymer latex in which stability is secured by using an emulsifier, a residual emulsifier remains in the recovered powder, which has a disadvantage of adversely affecting thermal stability and color during processing.

Accordingly, the apparatus for producing a polymer latex resin powder capable of producing a polymer latex resin powder having excellent color and powder characteristics by reducing the water content of the slurry to increase the drying efficiency and reducing the amount of flocculant used, and the polymer latex resin powder using the same Development of the manufacturing method is still required.

An object of the present invention is to introduce a non-continuous screw into the reactor to perform agglomeration and maturation to increase the mixing efficiency of steam, latex and flocculant, to lower the water content of the slurry to increase the drying efficiency, reducing the amount of flocculant used It is to provide an apparatus for producing a polymer latex resin powder capable of producing a polymer latex resin powder excellent in color and powder properties, and a method for producing a polymer latex resin powder using the same.

The above object of the present invention can be achieved by the present invention described below.

In order to achieve the above object, the present invention is a device for producing a polymer resin powder comprising a reactor for agglomeration of polymer latex, the reactor is a reaction tube of the hollow tube through which the latex passes, and the reaction from the inner wall of the reaction tube At least one barrel pin protruding inwardly of the tube, a rotating shaft extending along the central axis in the longitudinal direction of the reaction tube, and at least one agitator protruding from the outer surface of the rotating shaft toward the inner wall of the reaction tube; In addition, the at least one stirrer provides a polymer resin powder manufacturing apparatus comprising a discontinuous screw.

The apparatus for producing the polymer resin powder may include, for example, a dehydrator, a dryer, or both.

The stirrer may be 1 to 20, for example.

The discontinuous screw may include, for example, one or more openings.

The total area of the opening may be, for example, within the range of 0.05 to 1 relative to the total area of the rotary blade.

For example, the discontinuous screw may have an inclination angle α of the rotary blade from an axis perpendicular to the rotation axis within a range of 0.1 to 10 °.

The reaction tube of the reactor may include, for example, one or more barrel pins extending from the outside of the reaction tube into the reaction tube.

The reactor may include, for example, a polymer latex input line, a flocculant input line, and a steam input line.

The reactor may be, for example, an integrated reactor for agglomeration and ripening of the polymer latex.

In addition, the present invention provides a method for producing a polymer resin powder, characterized in that for using the polymer resin powder production apparatus.

For example, the polymer resin powder may have a water content of 25% or less.

The method for preparing the polymer resin powder may be, for example, 0.5 to 30 minutes of the polymer slurry in the aggregation and aging step.

The polymer resin may be, for example, a vinyl cyan compound-conjugated diene compound-aromatic vinyl compound graft copolymer.

The present invention also provides a polymer resin powder produced by the above method.

According to the present invention, by introducing a non-continuous screw which prevents the flow of uncondensed steam and latex fluid in the reactor to perform agglomeration and maturation to induce turbulent flow of the latex to increase the mixing efficiency of the latex and flocculant, and The water content is improved by simplifying post-processing such as dehydration and drying, increasing energy saving effects, and improving the color of the polymer powder obtained by reducing the amount of flocculant required for the flocculation process.

In addition, by increasing the condensation efficiency of the non-condensed steam to ensure the residence time of the slurry in the device due to the reduction of steam volume and pressure, the powder characteristics (coarse particle removal and apparent specific gravity increase due to the increase in the number of impact of the slurry ) To increase the process stability of the post-process and to reduce the logistics costs such as energy savings, packaging costs, transportation costs.

1 is a block diagram schematically showing a process for producing a polymer latex resin powder according to the prior art.

FIG. 2 is a cross-sectional view schematically showing the configuration of a reactor for preparing a polymer latex resin powder according to an embodiment of the present invention and performing agglomeration and aging.

3 is a front view according to one embodiment of a discontinuous screw introduced into the reactor of FIG.

4 is a side view according to one embodiment of the discontinuous screw of FIG. 3.

5 is a front view of other embodiments of a discontinuous screw introduced into the reactor of FIG.

[Explanation of code]

100: reactor 110, 11: polymer latex input line

120, 12: flocculant input line 130: steam input line

140: barrel pin 150: stirrer

210: discontinuous screw

1: latex storage tank 2: flocculation tank

3: aging tank 4: dehydrator

5: dryer 13: water supply line

14: discharge of flocculant 15: final polymer powder

The inventors of the present invention, while studying a method for efficiently preparing polymer latex resin powder from emulsion polymerization latex, unlike the conventional process of individually flocculating and aging process, discontinuous screw in the reactor (100) made of both coagulation and aging By increasing the mixing efficiency of the steam, latex and flocculant, it is possible to increase the drying efficiency by lowering the water content of the slurry, and to reduce the amount of the flocculant to prepare a polymer latex resin powder having excellent color and powder characteristics. Confirmed.

The present invention for achieving the above object, as shown in Figure 2, in the apparatus for producing a polymer latex resin powder comprising a latex tank, a reactor for coagulation and maturation of latex, a dehydrator and a dryer, A hollow reaction tube 160 through which latex passes, at least one barrel pin protruding inward from the inner wall of the reaction tube 160, and a center in the longitudinal direction of the reaction tube A polymer latex comprising a rotating shaft extending along an axis and at least one stirrer protruding from the outer surface of the rotating shaft toward the inner wall of the reaction tube, wherein the at least one stirrer is a discontinuous screw 210. An apparatus for producing a resin powder is provided. That is, the present invention induces turbulent flow of latex by replacing at least one or more of the plurality of agitators 150 in the reactor for coagulation and maturation as described above with a discontinuous screw 210, thereby causing latex and flocculant To increase the mixing efficiency of the slurry, to reduce the water content of the slurry, to simplify the post-processing and energy saving effect such as dehydration and drying, and to reduce the color of the polymer powder obtained by reducing the amount of flocculant required for the flocculation process. It is characterized by providing quality improvement effect. The cross section of the reaction tube 160 may be any polygon or circle, preferably may be circular.

The stirrer may be, for example, a continuous rotary blade or a continuous screw.

The reactor 100 is designed to perform agglomeration and aging together, and the hollow reaction tube 160 through which latex passes and protrudes inwardly of the reaction tube 160 from an inner wall of the reaction tube 160. At least one or more barrel pins 140, a rotating shaft 170 extending along the longitudinal central axis of the reaction tube 160, and from the outer surface of the rotating shaft 170 toward the inner wall of the reaction tube 160 It comprises at least one stirrer 150 protruding, the reaction tube 160 is connected to the latex input line 110, the flocculant input line 120 and the steam input line 130 is connected to the reaction tube ( 160) to supply latex and flocculant and steam.

In one embodiment of the present invention, the discontinuous screw 210 may be provided with 1 to 20, preferably 4 to 16, most preferably 8 to 12 in the reactor 100, When in the above range, there is an effect of increasing the mixing efficiency of steam, latex, and flocculant by hindering the flow of fluid (non-condensed steam and latex) and inducing turbulent flow of latex, but the present invention is not limited thereto. It will be understood by those skilled in the art that the discontinuous screw 210 may be arranged in an appropriate number depending on the length L of the reactor 100. In addition, the discontinuous screw 210 may be a biaxial screw, and the discontinuous screw 210 used in the present invention is illustrated in more detail in FIGS. 3 and 4.

As shown in FIG. 3, the discontinuous screw 210 used in the present invention is a rotary blade 212 protruding radially from the outer surface of the screw shaft 211 around the central screw shaft 211. At least a portion of the) is characterized in that it comprises at least one or more openings 214 are formed discontinuously. The opening 214 is a direction in which latex is conveyed by rotation in the direction of rotation of the discontinuous screw 210 (in the direction of rotation in FIG. 2, counterclockwise around the screw shaft 211). (Conveying direction in Fig. 2), that is, a portion of the rotary blade 212 is not formed with respect to the direction extending along the longitudinal axis of the screw shaft 211. The openings 214 may be at least one, for example one (FIG. 5A), three (FIG. 5B) or four (FIG. 5C), as shown in FIG. 5, as shown in FIG. 3. The number may be two, but the present invention is not limited thereto, and a larger number of openings 214 may be formed. That is, the openings 214 may be 1 to 6, preferably 1 to 5, and most preferably 2 to 4, to hinder the flow of fluid (non-condensed steam and latex) within this range Induces turbulent flow of latex to increase the mixing efficiency of steam, latex, and flocculant is excellent. The openings 214 may be formed evenly (2, 4, 6, 8) rather than oddly (1, 3, 5, 7), and are formed evenly, compared to the odd number. In this case, less noise or vibration is generated. In FIG. 4, reference numeral 213 indicates a side surface corresponding to the blade tip of the rotary blade 212.

The area ratio of the opening 214 in the discontinuous screw 210 (ie, the total area of the opening 214 / the total area of the rotary blade 212) is 0.05 to 1, preferably 0.1 to 0.4, most Preferably it can be within the range of 0.2 to 0.3, within this range while maintaining the proper moving speed of the latex, while interfering with the flow of fluid (non-condensed steam and latex) and induce a turbulent flow of the latex, steam and latex, The effect of increasing the mixing efficiency of the flocculant is excellent.

The area of the rotary blade may mean the area of one surface 212 of the rotary blade, the area of the opening may mean the area of one surface 214 of the opening.

The opening may mean an empty space in which some sections of the rotary blade are omitted.

In the discontinuous screw 210, the smaller the inclination angle α of the rotary blade from the axis perpendicular to the screw axis, that is, the perpendicular to the screw axis, the back pressure opposite to the conveying direction. ) Increases, which induces turbulent flow to increase the mixing efficiency of steam, latex, and flocculant, and secures residence time. On the other hand, if the degree of inclination is too small, it will not be transported and will accumulate. Therefore, it is important to design by selecting an appropriate inclination, and this degree of inclination, i.e., the inclination angle α, is within the range of 0.1 to 10 degrees, preferably 0.2 to 4 degrees, and most preferably 0.4 to 2 degrees.

In the reactor 100 according to the present invention, a barrel pin 140 extending from the outside of the reaction tube 160 to the inside is fixed, and the agitator 150 and / or the discontinuous inside the reaction tube 160. The screw 210 is rotatably fixed. Specifically, the reaction tube 160 of the reactor 100 includes one or more barrel pins 140 extending from the outside of the reaction tube 160 into the reaction tube 160. Accordingly, the reaction tube 160 rotates between the stirrer 150 and / or the discontinuous screw 210 between the barrel pins 140 fixed to the reaction tube 160. 2) As the latex is introduced into the conveying direction of FIG. 2 as a result, the latex is in contact with the rotary blades of the stirrer 150 and / or the discontinuous screw 210 and receives mechanical force therefrom. The barrel pins 140 are subjected to a strong mechanical force, that is, a shear force, and the latex stabilized by the emulsifier added during the emulsion polymerization is stabilized by a mechanical method is broken, thereby agglomerated accordingly And, it is aged in the second half of the reaction tube (160).

The barrel pin 140 may have any shape such as a circle, a triangle, an inclination, an ellipse, a diamond, a rectangle, and the like, and is not particularly limited. In the case of the stirrer 150, anything such as a paddle, a screw, a biaxial screw, a pin, etc. Can be used

The reactor 100 comprising the discontinuous screw 210 is machined into a latex obtained by emulsion polymerization under the action of the barrel pin 140 and the internal stirrer 150 and / or the discontinuous screw 210. It is possible to control the viscosity of the polymer slurry by applying a force, and to make a slurry of high viscosity to control the moisture content using a mechanical force.

The reactor 100 includes a polymer latex input line 110, a flocculant input line 120, and a steam input line 130, and agglomeration reaction is performed at a portion close to a position where the polymer latex, flocculant, and steam are introduced. Occurs, and a aging reaction occurs in the second half of the reactor so that coagulation and aging can be performed simultaneously in substantially the same reactor.

The present invention provides a method for producing a polymer latex resin powder using the apparatus for producing a polymer latex resin powder as described above.

The polymer latex used in the present invention is an emulsion polymerized polymer latex having a solid content of 10 to 90% by weight, and may be a vinyl cyan compound-conjugated diene compound-aromatic vinyl compound graft copolymer. The graft copolymer is prepared by polymerizing a monomer mixture of an aromatic vinyl compound and a vinyl cyan compound on a conjugated diene-based compound.

The conjugated diene compound is butadiene rubber, ethylene-propylene-diene monomer rubber (EPDM), ethylene propylene rubber (EPR), halobutyl rubber, butyl rubber, styrene-isoprene-styrene (SIS) and styrene-butadiene rubber (SBR It may be selected from the group consisting of), specifically butadiene-based rubber is used.

The vinyl cyan compound may be acrylonitrile, methacrylonitrile, ethacrylonitrile or derivatives thereof, specifically acrylonitrile is used.

The aromatic vinyl compound may be styrene, alpha methyl styrene, alpha ethyl styrene, paramethyl styrene, vinyl toluene or a derivative thereof. Specifically, styrene is used.

The flocculant may be an inorganic salt such as a water-soluble inorganic acid or sulfate, such as sulfuric acid, phosphoric acid, hydrochloric acid. Generally, the flocculant is added to the theoretical value required for aggregation, and in the present invention, 0.5 to 5 parts by weight, specifically 0.5 to 3.0 parts by weight, most specifically 0.5 to 2.0 parts by weight, based on 100 parts by weight of the polymer latex. . That is, in the present invention, only a very small amount of flocculant can effectively flocculate the polymer latex. Thus, the effect of improving the color and increasing the thermal stability can be obtained by reducing the content of the flocculant.

The polymer resin powder may have, for example, a water content within 25%, or 10% to 20%.

The residence time of the polymer slurry in the reactor in the aggregation and aging step may be 0.5 minutes to 30 minutes, for example 0.5 minutes to 10 minutes, or 0.5 minutes to 5 minutes. In the existing device, the residence time was not secured due to the low steam condensation efficiency, but after the introduction of the discontinuous screw, the residence time can be secured.

The aggregation and aging temperature may be 60 to 100 ℃ or 65 to 85 ℃, within this range the coagulation and ripening effect is large.

This is different from the conventional apparatuses in which the flocculation and maturation processes are performed separately. However, a long residence time of about 30 minutes to 1 hour is required, but in the present invention, by introducing a discontinuous screw, the pressure difference is increased by increasing the condensation efficiency of steam. As a result, slurries with excellent powder properties can be prepared with very short residence times. The aggregation section of the residence time is substantially completed within a few seconds to 1 minute, and as soon as the aggregation is completed during the time, the aging proceeds until the polymer slurry is discharged out.

In the present invention, the residence time of the polymer slurry in the flocculation and aging process may be reacted to exceed 30 minutes, but in this case, the size of the device is not economical.

The solids content of the polymer latex slurry of the present invention prepared by the above process depends on the solids content of the polymer latex, but is generally 25 to 60% by weight. If the solid content is less than 25% by weight, there may be a problem in that the flowability of the slurry is too high to secure the residence time of the slurry, and in the case of more than 60% by weight, the slurry has a poor transport force and the slurry may There may be a problem that the operation is impossible to prevent.

The polymer slurry in which the agglomeration and aging proceeds is taken out of the reactor and transferred to the slurry storage tank. The flocculated and aged slurry is recovered in powder through a conventional dehydration and drying process.

Hereinafter, preferred examples are provided to help understanding of the present invention, but the following examples are merely for exemplifying the present invention, and various changes and modifications within the scope and spirit of the present invention are apparent to those skilled in the art. Naturally, changes and modifications belong to the appended claims.

EXAMPLE

Example 1

Graft copolymer latex consisting of vinyl cyan compound-conjugated diene compound-aromatic vinyl compound is acrylonitrile (AN) -butadiene (BD) -styrene (SM) copolymer latex as AN / BD / SM = 13/60 / 27, and the solid content was 44%.

The latex was introduced into a reactor having a configuration including eight discontinuous screws (A2 / A1 = 0.33, α = 3.60 °) in a reactor as shown in FIG. 2 at a flow rate of 12 kg / hr and a flocculant. For the furnace, 1.0 part by weight of diluted sulfuric acid (H ₂ SO ₄ ) was used based on 100 parts by weight of the total polymer. While directly steaming, the liquid water was added to the solids content of the slurry and mixed with sulfuric acid to adjust the solids content of the polymer latex slurry to 30% by weight.

The residence time of the reactor was 1.5 minutes on average, and the aggregation and aging temperatures were 75 ° C. The ripening section begins as soon as the agglomeration is complete and continues until the slurry is discharged out. The aggregated slurry is drawn out through the stirrer and moved to the slurry storage tank. The aggregated and aged slurry was recovered to polymer resin powder through a dehydration and drying process.

Example 2

A polymer resin powder was prepared in the same manner as in Example 1, except that the solid content of the polymer latex slurry in Example 1 was 35% by weight.

Example 3

A polymer resin powder was prepared in the same manner as in Example 1, except that the solid content of the polymer latex slurry was 44 wt% in Example 1.

Example 4

A polymer resin powder was prepared in the same manner as in Example 1 except that the amount of the flocculant used in Example 1 was 0.7 parts by weight based on 100 parts by weight of the polymer.

Example 5

A polymer resin powder was prepared in the same manner as in Example 1 except that the amount of the flocculant used in Example 1 was 0.6 parts by weight based on 100 parts by weight of the polymer.

Comparative Example 1

To the latex, the reactor having a configuration which does not include the non-continuous screw reactor, 12㎏ / hr flow rate introduced into the, and as a flocculating agent is a sulfuric acid (H ₂ SO ₄₎ was diluted as shown in Figure 2. Total 1.0 weight part was used with respect to 100 weight part of polymer contents. While directly steaming, the liquid water was added to the solids content of the slurry and mixed with sulfuric acid to adjust the solids content of the polymer latex slurry to 30% by weight.

Comparative Example 2

A polymer resin powder was prepared in the same manner as in Comparative Example 1 except that the solid content of the polymer latex slurry was 35 wt% in Comparative Example 1.

Comparative Example 3

A polymer resin powder was prepared in the same manner as in Comparative Example 1 except that the solid content of the polymer latex slurry was 44 wt% in Comparative Example 1.

Comparative Example 4

A polymer resin powder was prepared in the same manner as in Comparative Example 1 except that the amount of the flocculant used in Comparative Example 1 was 0.7 parts by weight based on 100 parts by weight of the polymer.

Comparative Example 5

A polymer resin powder was prepared in the same manner as in Comparative Example 1 except that the amount of the flocculant used in Comparative Example 1 was 0.6 parts by weight based on 100 parts by weight of the polymer.

[Test Example]

The water content, apparent specific gravity, particle size distribution, and whiteness of the polymer latex resin powders prepared in Examples 1 to 5 and Comparative Examples 1 to 5 were measured by the following method, and the results are shown in Table 1 below.

* Moisture Content: The water content was measured until the water sample evaporated at 150 ° C. and the sample weight was no longer changed (less than 0.5% by weight of residual water) using a moisture meter (METTLER / TOLEDO HR83-P). .

* Apparent specific gravity: measured according to ASTM D1985.

* Particle size distribution: The particle size was measured using a standard network, and the content of large particles (cos, coarse) was measured to 1400 µm or more.

* Whiteness of powder: b value was measured using a colorimeter (Color Quest II, Hunter Lab Co.). The b value may have a positive value and a negative value with respect to 0, which means that the value is yellow when the value is larger than 0, and the color is blue when the value is smaller than 0.

Table 1

	Solid content (% by weight)	Coagulant (parts by weight)	Moisture content (% by weight)	Apparent specific gravity (g / ml)	Course content (%)	Color (b)
Example 1	30	1.0	18.32	0.38	8.9	1.78
Example 2	35	1.0	17.93	0.42	9.2	1.64
Example 3	44	1.0	16.33	0.44	9.9	1.61
Example 4	30	0.7	19.22	0.37	6.3	1.42
Example 5	30	0.6	22.21	0.35	5.4	1.51
Comparative Example 1	30	1.0	26.10	0.32	16.3	2.35
Comparative Example 2	35	1.0	24.85	0.34	17.2	2.24
Comparative Example 3	44	1.0	21.23	0.37	18.4	2.13
Comparative Example 4	30	0.7	34.91	0.30	15.6	2.05
Comparative Example 5	30	0.6	40.33	0.28	12.77	3.11

As shown in Table 1, the polymer latex resin powder prepared using the production apparatus according to the present invention has improved water content and color (b value) compared to the comparative example, the apparent specific gravity is increased and the average particle diameter is about 1400㎛ Coarse content of the larger particles (coarse) was significantly reduced, and the amount of flocculant used was reduced, thereby confirming that the color was improved.

Example 6

Area ratio occupied by the opening 214 of the discontinuous screw shown in FIG. 2 (i.e., the total area of the opening 214 / the rotor blade in order to examine the characteristics in the configuration of the discontinuous screw introduced according to the present invention). Tonality b was measured using water content, apparent specific gravity, course content, and colorimeter (Color Quest II, Hunter Lab Co.) through different experiments (total area of (212)), and the results are shown in Table 2 below. Here, the inclination angle α of the rotary blade from the axis perpendicular to the screw axis was 3.6 °.

TABLE 2

A2 / A1	Water content	Apparent weight	Course content	Color (b)
A2 / A1	(weight%)	(g / ml)	(%)	Color (b)
One	19.63	0.37	12.51	1.85
0.5	18.98	0.37	10.1	1.82
0.33	18.32	0.38	8.9	1.78
0.2	17.56	0.4	6.5	1.71
0.09	18.55	0.38	7.2	1.82

As can be seen in Table 2, the area ratio occupied by the opening (ie, the total area of the opening / the total area of the rotary blades) is within the range of 0.05 to 1, preferably 0.1 to 0.4, most preferably 0.2 to 0.3. It was confirmed that the effect of increasing the mixing efficiency of steam, latex, and flocculant by interfering the flow of the fluid (non-condensed steam and latex) and inducing turbulent flow of the latex while maintaining the proper moving speed of the latex at.

Example 7

In order to examine the characteristics of the configuration of the discontinuous screw introduced according to the present invention, an experiment in which the inclination angle α of the rotary blades from the axis in the vertical direction with respect to the screw axis of the discontinuous screw shown in FIG. Tone b was measured using a water content, apparent specific gravity, course content, and colorimeter (Color Quest II, Hunter Lab Co.), and the results are shown in Table 3 below. The area ratio occupied by the opening portion 214 of the discontinuous screw was 0.33.

TABLE 3

α	Water content	Apparent weight	Course content	Color (b)
α	(weight%)	(g / ml)	(%)	Color (b)
7.2	20.78	0.36	13.44	2.01
3.6	18.32	0.38	8.9	1.78
2	16.12	0.44	5.3	1.21
0.15	17.73	0.38	6.6	1.81

As can be seen in Table 3, the inclination angle α of the rotary blade from the axis perpendicular to the screw axis of the discontinuous screw is 0.1 to 10 °, preferably 0.2 to 4 °, most preferably Excellent effect of increasing the mixing efficiency of steam, latex and flocculant by interfering the flow of fluids (non-condensed steam and latex) and inducing turbulent flow of latex while maintaining the proper moving speed of latex within 0.4 to 2 ° It could be confirmed that it appears. In particular, as the inclination angle α is smaller, that is, the screw is perpendicular to the screw axis, the back pressure opposite to the conveying direction is increased, thereby inducing turbulent flow to increase the mixing efficiency of steam, latex, and flocculant. It was confirmed that the effect of increasing and securing the residence time occurred. Therefore, it is important to select and design the proper slope.

Claims

An apparatus for producing polymer resin powder comprising a reactor for agglomeration of polymer latex, the reactor comprising: a hollow reaction tube through which the latex passes, and at least one protruding inwardly from the inner wall of the reaction tube; And at least one barrel pin, a rotating shaft extending along a central axis in the longitudinal direction of the reaction tube, and at least one agitator protruding from an outer surface of the rotating shaft toward an inner wall of the reaction tube, wherein the at least one agitator is discontinuous. Apparatus for producing a polymer resin powder comprising a screw.
The method of claim 1,

The apparatus for producing a polymer resin powder is a device for producing a polymer latex resin powder, characterized in that it comprises a dehydrator, a dryer or both.
The method of claim 1,

Apparatus for producing a polymer resin powder, characterized in that it comprises 1 to 20 agitators.
The method of claim 1,

The discontinuous screw is an apparatus for producing a polymer resin powder, characterized in that it comprises one or more openings.
The method of claim 4, wherein

The total area of the opening is an apparatus for producing a polymer resin powder, characterized in that within the range of 0.05 to 1 relative to the total area of the rotary blade.
The method of claim 1,

The discontinuous screw is a device for producing a polymer resin powder, characterized in that the inclination angle (α) of the rotary blade from the axis in the vertical direction with respect to the rotation axis is within the range of 0.1 to 10 °.
The method of claim 1,

Apparatus for producing a polymer resin powder, characterized in that the reaction tube of the reactor comprises at least one barrel pin extending from the outside of the reaction tube into the reaction tube.
The method of claim 1,

Apparatus for producing a polymer resin powder, characterized in that the reactor comprises a polymer latex input line, flocculant input line and steam input line.
The method of claim 1,

The reactor is a polymer resin powder manufacturing apparatus, characterized in that the integrated reactor for the aggregation and aging of the polymer latex.
The manufacturing method of the polymer resin powder using the manufacturing apparatus of the polymer resin powder in any one of Claims 1-9.
The method of claim 10,

The polymer resin powder is a method for producing a polymer resin powder, characterized in that the water content is within 25%.
The method of claim 10,

The manufacturing method of the polymer resin powder is a polymer resin powder production method, characterized in that the residence time of the polymer slurry in the aggregation and aging step is 0.5 minutes to 30 minutes.
The method of claim 10,

The polymer resin is a vinyl cyan compound-conjugated diene compound-aromatic vinyl compound graft copolymer, characterized in that the polymer resin powder production method.
Polymer resin powder prepared by the method according to claim 10.