WO1994006847A1

WO1994006847A1 - Process for producing polycarbonate powder

Info

Publication number: WO1994006847A1
Application number: PCT/JP1992/001193
Authority: WO
Inventors: Masaya Okamoto; Noriyuki Kunishi
Original assignee: Idemitsu Petrochemical Company Limited
Priority date: 1992-09-18
Filing date: 1992-09-18
Publication date: 1994-03-31
Also published as: BR9206766A

Abstract

A process for producing polycarbonate powder readily by ejecting a mixture of a solution of polycarbonate in an organic solvent with steam through a mixing nozzle, wherein a lowness of the bulk density of the powder, which has been a shortcoming of the conventional processes using a mixing nozzle, can be remedied without causing any increase in the amount of a residual solvent by using a 3-45 wt.% solution of polycarbonate in an organic solvent and adjusting the ratio of the weight (Ws) of the steam to the weight (Wo) of the organic solvent in the solution to 1/10 to 1/5.

Description

Description Method for producing polycarbonate powder

Technical field

The present invention relates to a method for producing a polycarbonate powder, and more particularly to a method for producing a polycarbonate powder having a high bulk density. Background technology

Polycarbonate production methods include a melt polycondensation method (transesterification method) and an interfacial polycondensation method (phosgene method), and the methods for industrially producing polycarbonate include interfacial weight. The condensation method is preferably used.

In the method for producing polycarbonate based on the interfacial polycondensation method, the emulsion solution obtained by the interfacial polycondensation reaction is washed and separated to obtain an organic solvent solution of polycarbonate (in general, the solvent is methyl chloride). Len) is first obtained. Next, the polycarbonate is separated (recovered) as a powder or granules from the obtained organic solvent solution. Thereafter, if necessary, the obtained polycarbonate is formed into a pellet or the like.

A simple method for recovering polycarbonate as a powder from a solution of polycarbonate in an organic solvent is to use a jet nozzle (mixing nozzle) to remove the organic component of polycarbonate. A method is known in which a solvent solution and steam are introduced, a mixture injected from a jet nozzle is introduced into a separator through a pipe, and the polycarbonate powder is recovered by the separator (Japanese Patent Publication No. No. 633-1333, Japanese Patent Publication No. 2-65661, and US Pat. No. 3,508,339. Then, when recovering the poly Kabone DOO powder by this method, 1 ratios (WC ZWQ) of the weight of the steam (W _C) and weight of the organic solvent in the organic solvent solution of a poly Kabone bets (WQ) 5 Larger than that, steam and an organic solvent solution are introduced into a mixing nozzle.

This method includes a method of adding a poor solvent to a solution of polycarbonate in an organic solvent (Japanese Patent Publication No. 4-144474) and a method of using a crystallization method of a solution of polycarbonate in an organic solvent. Crushing method (Japanese Patent Publication No. Sho 53-15989), or a method of pouring an organic solvent solution of polycarbonate into warm water (Japanese Patent Application No. Sho 60-115,625). Compared with the method, it has an IJ point that powdered polycarbonate with less residual solvent can be easily recovered.

However, a polycarbonate obtained by a conventional method in which an organic solvent solution of polycarbonate and steam are introduced into the mixed nozzle, and the polycarbonate is recovered as a powder from the mixture sprayed from the mixed nozzle. Carbonate powder is in the form of lint and has a bulk density of 0.05 to 0.35. Low. For this reason, the volumetric efficiency of the processing equipment used for post-processing such as drying or storage of the obtained polycarbonate powder is reduced, and large-sized processing equipment is used or used as these processing equipment. The difficulty was that production adjustments had to be made to accommodate the volume of processing equipment. In addition, in the case of a polycarbonate powder having a low bulk density, the miscibility with various additives is low, and a dense pellet cannot be obtained when this powder is formed into a pellet.

An object of the present invention is to provide a method for producing a high bulk density polycarbonate powder capable of easily obtaining a polycarbonate powder having a high bulk density and a small residual solvent amount. Disclosure of the invention

The method of the present invention for achieving the above object is as follows. V method.

I. A method of polycarbonate powder in which an organic solvent solution of polycarbonate and steam are introduced into a mixing nozzle, and the polycarbonate is recovered as a powder from the mixture injected from the mixing nozzle. An organic solvent solution having a polycarbonate concentration of 3 to 45% by weight is used as the organic solvent solution, and the weight of the steam at the time of introduction and the weight of the organic solvent in the organic solvent solution are determined. The method for producing a high bulk density polycarbonate powder characterized in that the ratio of Below, this method is called method I).

Π. A mixture of an organic solvent solution with a polycarbonate concentration of 3 to 45% by weight and steam having a weight 1 to 20 times 1 to 20 times the weight of the organic solvent in the organic solvent solution The mixture injected from the mixing nozzle was introduced into the nozzle and mixed with steam having a weight IZSOOIZI times the weight of the organic solvent in the organic solvent solution after a residence time of 0.01 to 1 second. A method for producing a high bulk density polycarbonate powder, characterized by obtaining a mixture and recovering the polycarbonate as a powder from the second mixture (hereinafter, this method is referred to as method Π). ) O

m. An organic solvent solution having a polycarbonate concentration of 3 to 45% by weight, steam and polycarbonate powder are introduced into a mixing nozzle, and the mixture sprayed from the mixing nozzle is used to form a polycarbonate. A method for producing high bulk density polycarbonate powder, which comprises collecting the powder as a powder (hereinafter, this method is referred to as method m).

IV. An organic solvent solution having a concentration of polycarbonate of 3 to 45% by weight and steam are introduced into a mixing nozzle, and the mixture injected from the mixing nozzle is directly injected from the mixing nozzle or connected to a pipe. Characterized in that the mixture discharged from the mixer is introduced into a gas-solid separator through piping, and the polycarbonate powder is recovered by the gas-solid separator. Polycarbonate powder production method (hereinafter, this method is referred to as Method IV). BRIEF DESCRIPTION OF THE FIGURES

FIG. 1 is a cross-sectional view showing a mixing nozzle used in Examples 1 to 5, and FIG. 2 shows an apparatus used for obtaining a high bulk density polycarbonate powder in Examples 7 to 22. FIG. 3 is a schematic cross-sectional view showing a first mixed nozzle used in Examples 7 to 22. FIG. 4 is a sectional view showing a second mixed nozzle used in Examples 7 to 22. FIG. 5 is a schematic view showing an apparatus used to obtain a high bulk density polycarbonate powder in Examples 23 to 32, and FIG. 6 is an example 33 to Examples. FIG. 1 is a schematic diagram showing an apparatus used to obtain a high bulk density polycarbonate powder at 40.

BEST MODE FOR CARRYING OUT THE INVENTION

Hereinafter, the method I of the present invention! V will be described in detail sequentially. Method I

As described above, the concentration of the polycarbonate in the organic solvent solution of the polycarbonate used in the method I (hereinafter may be simply referred to as the organic solvent solution) is 3 to 4531% by volume (hereinafter, referred to as “the organic solvent solution”). Weight% is abbreviated as wt%). Here, the reason for limiting the concentration of polycarbonate to 3 to 45 wt% is that if the concentration is less than 3 wt%, This is because the productivity of the organic solvent solution becomes too low, and on the other hand, if it exceeds 45 wt, the fluidity of the organic solvent solution becomes too low, and it becomes difficult to introduce the mixed solvent into the mixed nozzle.

The types of the above polycarbonates are not particularly limited, and various types of polycarbonates obtained by reacting divalent phenol with phosgene or a carbonate compound are used. can do. The following are examples of the divalent phenol and the carbonate compound.

① Bivalent phenol

2, 2 '— bis (4-hydroxyphenyl) prono, ⁰ (bisphenol A), bis (4-hydroxyphenyl) methane, bis (4-hydroxyphenyl) phenylmethane, bis ( 4—Hydroxyphenyl) naphthylmethane, Bis (4-Hydroxyphenyl) methane, (4-Isopropylfurenyl) methane, Difujirubibis (4—Hydroxyquinphenyl) methane , Bis (3,5—dichloro-4-hydroxyphenyl) methane, bis (3,5—dimethyl-4-hydroxyphenyl) methane, 1,1 bis (4-hydroxyphenyl) Nore) ethane, 1 — naphthyl 1, 1-bis (4-hydroxyphenyl) ethane, 1 phenyl 1-1, 1-bis (4-hydroxy xyphenyl) ethane, 1, 2 — Bi (4-arsenate Dorokishifu enyl) E data down, 2 - main Chinore 1, 1 — Bis (4—hydroxythiphenyl) propane, 2,2_bis (3,5—Dimethyltinole 4—Hydroxysiphenyl) propane, 1—Ethyru1,1—Bis

(4-Hydroxyphenyl) propane, 2,2-bis (3,5-dichloro-4-propanol) propane, 2,2-bis (3,5-dibromo—4— Hydroquinine) propane, 2,2-bis (3,5-dichloro-4-hydroxyphenyl) propane, 2,2-bis (3-methylthiophenyl) propanol ⁰ , 2, 2 — Screw

(3 Funoreoro over 4-arsenide Doroki Schiff et two Honoré) Pro c ⁰ emissions, 1, 1 one-bis (4-arsenate Dorokishifu enyl) but down, 3, 2- bis (4-arsenate Dorokishifu Weniru) pigs down, 1 , 4-bis (4-hydroxyphenyl) butane, 2,2-bis (4-hydroxyphenyl) pentane, 4-methyl-2-, 2-bis (4-hydroxyphenyl) pentane, 1,1-bis (4-hydroxycyclobutane) cyclohexane, 1,1-bis (3,5-cyclohexyl 1-4-hydroxyphenyl) cyclohexane, 2 , 2-bis (4-hydroxyphenyl) hexane, 4,4-bis (4-hydroxyphenyl) heptane, 2,2-bis (4-hydroxyphenyl) nonane , 1, 1 0 — screw

(4-Hydroxysifenyl) decane and 1, 1-bis (4-Hydroxysifenyl) cyclododeca Dihydroxylalkanes such as diene;

Bis (4—hydroxyquinenyl) sulfone, bis (3,5—dimethyl-4-hydroxyhydroxy) sulfone and bis (3—cyclohexa-4-hydroxyphenyl) sulfone Reel sulfones;

Dihydroxyl ethers such as bis (4-hydroxyhydrenyl) ether and bis (3,5-dimethyltin-4-ether) phenyl ether;

4,4'-dihydroxybenzophenone and 3,3 ', 5,5'-tetrahydroxy-1,4-dihydroxy benzophenone Tons;

Bis (4-hydroxyphenyl) sulfide, bis (3—methyl-4-hydroxyphenyl) sulfide and bis (3,5—dimethyl-4-hydroxyphenyl) snolefide, etc. Rusulfides;

Dihydroxyarylsulfoxides such as bis (4-hydroxyquinphenyl) sulfoxide;

4,4'-dihydroxy mouth didiphenyls such as dihydroxydiphenyl;

Dihydroxybenzenes such as hydroquinone, resornol and methylhydroquinone; 1,5-dihydroquinnaphthalene and 2,6-dihydroquinnaphlene, and the like;

② Carbonate compound

Diaryl carbonate such as diphenyl carbonate, dialkyl carbonate such as dimethyl carbonate-jetinole carbonate, and the like.

The type of the organic solvent is not particularly limited as long as it can dissolve the polycarbonate and can be removed by evaporation with steam. As such an organic solvent, methylene chloride is preferred, but chloroform, carbon tetrachloride, dioxane, tetrahydrofuran and the like can also be used. These organic solvents may be used alone or as a mixture.

In the method I, the above-mentioned organic solvent solution and steam are introduced into a mixing nozzle, and polycarbonate is recovered as a powder from the mixture injected from the mixing nozzle.

Here, as described above, the ratio (W e / WQ) of the weight of steam (w _c ) to the amount of the organic solvent in the organic solvent solution (WQ) is l / l, as described above. i

It is introduced into the mixing nozzle so that the number becomes 0 to 1 no. The reason for limiting WS ZW Q to 1-10 to 1-5 is that WPZW Bone DOO powder amount of organic solvent remaining in is increased too, whereas W when _c / W_〇 is greater than 1/5, the bulk density of the port Li Kabone one preparative powder obtained Ru der because too low. Also preferably: LZ8 ~: LZ6.

Is a steam pressure (the pressure at the nozzle introduction) 1 ~ 1 0 0 kg / cm 2, temperature 1 00-3 1 0. It is preferable to use C's.

As a mixed nozzle into which the organic solvent solution and the steam are introduced, any type of mixed nozzle can be used, but a mixed nozzle having an ejector structure is preferable.

When the polycarbonate is recovered from the mixture injected from the mixing nozzle, if it is clear, the injected mixture is introduced into a separator such as a gas-solid separation cyclone through piping, and the polycarbonate is separated by this separator. It can be done by separation (recovery). In this case, the pipe connecting the mixing nozzle and the separator may be a straight pipe or a curved pipe. Its pipe diameter

(Inner diameter) is 5mn! It is preferable that the pipe length is 50 cm to 100 m. Pipe length for pipe diameter (inner diameter D)

The ratio (L / D) of (L) is preferably from 100 to 100000. If this ratio is less than 100, the evaporation of the organic solvent is insufficient, and if it exceeds 1 000, the pressure loss increases, so high-pressure steam is required as the steam introduced into the mixed nozzle. Becomes

According to Method I, an organic solvent solution of polycarbonate and steam are introduced into a mixing nozzle, and the mixture is introduced through a mixing nozzle. When the injected mixture Karapo Li Kabone preparative recovered as a powder, poly Kabone in the organic solvent solution - the concentration of bets defined as described above, and upon the introduction of w _s

By defining G as described above, it becomes possible to easily obtain a polycarbonate powder having a high bulk density and a small residual solvent amount.

In addition, the method I can be applied as a part of a process for producing a polycarbonate by an interfacial polycondensation method. In this case, a polycarbonate obtained by subjecting the emulsion solution obtained by the interfacial polycondensation reaction to a washing and separation operation as an organic solvent solution of polycarbonate mixed with steam. Using an organic solvent solution of Method Π

As in Method I, the organic solvent solution used in Method II is an organic solvent solution having a polycarbonate concentration of 3 to 45 wt%. Here, in Riyama, where the lower limit of the concentration of polycarbonate is limited to 3 wt%, the productivity of the polycarbonate powder becomes too low if the concentration is less than 3 wt%. Also, the reason that the upper limit of the concentration of polycarbonate is limited to 45 wt% is that if it exceeds 45 wt%, the fluidity of the organic solvent solution is too low, and the mixing nozzle (this mixing nozzle in method Π) This is sometimes referred to as the first mixing nozzle). A particularly preferred concentration of polycarbonate is 10 to 30 wt%.

The types of polycarbonate mentioned above are particularly limited, Instead, various polycarbonates obtained by the reaction of divalent phenol with phosgene or a carbonate ester compound can be used. Here, specific examples of the divalent phenol and the carbonate compound include various divalent phenols and various carbonates exemplified in the method I.

The type of the organic solvent is not particularly limited as long as it can dissolve the polycarbonate and can be removed by evaporation with steam. As such an organic solvent, methylene chloride is preferred, but as in Method I, ethylene chloride, chloroform, carbon tetrachloride, dioxane, tetrahydrofuran, etc. can also be used. . These organic solvents may be used alone or as a mixture.

In the method Π, the organic solvent solution described above and steam having a weight 1/20 to 1/8 times the weight of the organic solvent in the organic solvent solution (hereinafter sometimes referred to as w _Qi ) are used for the first step. Into a mixed nozzle. Here, the reason that the lower limit of the weight of steam introduced into the first mixing nozzle (hereinafter sometimes referred to as w _s ) is limited to 1 Z 20 times W _0i is that W _Si is smaller than W _Qi . If the ratio is less than 20 times 1 Z, the organic solvent is not sufficiently evaporated and removed, so that it is impossible to make the polycarbonate from the organic solvent solution bubble. Also, Riyama, who limits the upper limit of W ^S1 to 1 Z8 times of W _Q , ends when W ^S1 is more than 1 Z8 times of This is because the bulk density of the resulting polycarbonate powder is too low.

The pressure of the steam introduced into the first mixing nozzle (pressure at the time of introducing the nozzle) is preferably 1 to 10 O kgZcm ² , particularly preferably 3 to 80 kg / cm ^2. I like it. If the steam pressure is less than 1 kg / cm ² , the mixing speed required for mixing the organic solvent solution and steam cannot be obtained. In addition, high pressure equipment is required to obtain steam exceeding 100 kg / cn ^, and equipment costs are unnecessarily high.

As the first mixing nozzle, a mixing nozzle having a force and an ejector structure that can use any type of mixing nozzle commonly used is preferable.

In the method (1), the mixture injected from the first mixing nozzle (hereinafter sometimes referred to as the first mixture) is subjected to a residence time of 0.001 to 1 second, after which the weight of the organic solvent (W _Q1 ) To obtain a second mixture.

Here, the reason for limiting the lower limit of the residence time (hereinafter sometimes referred to as τ) of the first mixture to 0.001 second is that if the steam is less than 0.001 second, steam is applied twice. This is because the effects used separately cannot be obtained. In addition, Riyama limits the upper limit to 1 second.If r exceeds 1 second, polycarbonate exists as a completely evaporated dry solid when mixed with steam. Effect Is not obtained. Also, the reason for limiting the lower limit of the weight of steam (hereinafter, sometimes referred to as w _S2 ) used to obtain the second mixture to 1/200 times of that is that W _S2 is _1/20 times of If the amount is less than twice, the amount of the organic solvent remaining in the obtained polycarbonate powder becomes too large. _—The reason for limiting the upper limit of w _S2 to 11 times is

^W S2 change like the bulk density and the residual solvent amount of Po Li force Bone preparative powder also obtained by more than 1 1 times ^w 01 is not, because the excessive amount of steam.

The second mixture, for example, introduces the first mixture ejected from the first mixing nozzle through a pipe into the second mixing nozzle so as to be at the above-mentioned residence time, and simultaneously with the second mixture nozzle. It can be obtained by introducing the above-mentioned predetermined amount of steam into the mixed nozzle. As the second mixing nozzle in this case, it is preferable that the second mixing nozzle has a force that can use any type of mixing nozzle that is usually used. In addition, the first mixing nozzle is connected to a separator, which will be described later, by a pipe, and a predetermined position of the pipe, that is, a residence time of the mixture (first mixture) injected from the first mixing nozzle. A pipe for supplying steam is provided at a position where the temperature is 0.01 to 1 second, and the second mixture is also mixed here by mixing the first mixture with the above-mentioned predetermined amount of steam. Obtainable. In the method (2), the polycarbonate is recovered as a powder from the second mixed product obtained as described above. If it is clear, this recovery can be performed by introducing the second mixture into a separator such as a gas-solid separation cyclone by piping, and recovering the polycarbonate by this separator. In this case, the pipe for introducing the second mixture into the separator may be a straight pipe or a curved pipe, but the length of the pipe should be long enough to secure the residence time for the polycarbonate to evaporate to dryness. The length should be such that the piping pressure loss is comparable to the pressure of the steam to be used. Steam and organic solvent vapor can be condensed and recovered by a capacitor after separation of the polycarbonate powder.

The polycarbonate powder thus obtained has a high bulk density and a small amount of residual solvent. In addition, when the polycarbonate powder is manufactured by the method (1), even if the processing amount of the organic solvent solution of the polycarbonate fluctuates, the properties (bulk density and residual solvent amount) of the obtained polycarbonate powder are changed. Changes) are small. Therefore, even when the obtained polycarbonate carbonate powder is subjected to post-processing such as forming into a pellet or the like through a drying / granulation process, inconvenience of equipment (for example, the (The post-processing cannot be performed due to a change in the properties). On the other hand, since the bulk density of the polycarbonate powder is high, the volumetric efficiency of equipment used for post-processing is improved. In addition, the method (2) can be applied as a part of a process for producing a polycarbonate by a meta-polycondensation method. In this case, an organic solvent solution of the polycarbonate obtained by washing and separating the emulsion solution obtained by the interfacial polycondensation reaction is used as the organic solvent solution of the polycarbonate.

Method in

The organic solvent solution used in the method IE is an organic solvent solution having a polycarbonate concentration of 3 to 45 wt% as in the methods I and II. The reason why the lower limit of the concentration of polycarbonate is limited to 3 wL% is that if it is less than 3 wt%, the productivity of polycarbonate powder becomes too low. The reason why the upper limit of the concentration of polycarbonate is limited to 45 wt% is that if it exceeds 45%, the fluidity of the organic solvent solution will be too low and it will be difficult to introduce it into the mixing nozzle. is there.

The type of the above-mentioned polycarbonate is not particularly limited, and various polycarbonates obtained by reacting a divalent phenol with phosgene or a carbonate compound can be used. Here, specific examples of the dihydric phenol and the carbonate compound include various dihydric phenols and various carbonates that have been clarified by Method I.

Also, the type of organic solvent is one that dissolves polycarbonate and can be removed by evaporation with steam. If so, there is no particular limitation. As such an organic solvent, methylene chloride is preferable, but as in method I, ethylene chloride, chloroform, carbon tetrachloride, dioxane, tetrahydrofuran and the like can also be used. These organic solvents may be used alone or as a mixture.

In the method m, the above-described organic solvent solution, steam and polycarbonate powder are introduced into a mixing nozzle, and the polycarbonate is recovered as a powder from the mixture injected from the mixing nozzle.

Here, it is preferable to use steam having a pressure (pressure at the time of introducing the mixing nozzle) of 1 to 100 kgZcm ² and a temperature of 100 to 310. The amount of steam introduced into the mixing nozzle is the same as that of Method I, that is, 1 Z 10 to LZ 5 times the weight of the organic solvent in the organic solvent solution introduced into the mixing nozzle. (Hereinafter referred to as A in combination with Method I) or the same amount as the conventional method, that is, more than 1/5 times the weight of the organic solvent in the organic solvent solution introduced into the mixing nozzle. May be an amount

(Hereinafter, this case is referred to as combination A with the conventional method). If the amount of steam introduced into the mixed nozzle is less than 10 times, evaporation of the solvent becomes insufficient. On the other hand, even if a large amount of steam is introduced into the mixing nozzle, the bulk density and the production amount only decrease, so the amount of steam introduced into the mixing nozzle depends on the amount of the organic solvent solution introduced into the mixing nozzle. No It is particularly preferred that the weight is 110 to 1 times the weight of the organic solvent.

Further, as the polycarbonate powder introduced into the mixing nozzle, a polycarbonate powder of the same quality as the polycarbonate dissolved in the organic solvent solution described above may be used. Carbonate powder may be used, but practically, it is preferable to use polycarbonate powder of the same quality. When introducing the polycarbonate powder into the mixing nozzle, it may be introduced by a dedicated pipe alone, but in practice, it is preferable to introduce the powder in a state of being mixed with steam. As a method of introducing the polycarbonate powder into the mixing nozzle in a state of being mixed with steam, for example, a pipe for introducing steam into the mixing nozzle (hereinafter sometimes referred to as a steam line) is used. There is a method in which a pipe for supplying the polycarbonate powder is provided on the way, and the steam and the polycarbonate powder are mixed in the steam line. The amount of the polycarbonate powder introduced into the mixing nozzle may be 0.5 to 20%, particularly 1 to 20%, of the weight of the polycarbonate in the organic solvent solution introduced into the mixing nozzle. I like it. If the introduction amount is less than 0.5%, the degree of improvement of the bulk density in the finally obtained polycarbonate powder is low. On the other hand, even if it is introduced into the mixing nozzle in excess of 20%, there is no large difference in the degree of improvement in bulk density in the finally obtained polycarbonate powder. Further, it is preferable that the particle diameter of the polycarbonate powder to be introduced into the mixing nozzle be 8 mesh or less and 200 mesh or more. If the particle size exceeds 8 mesh, the feed to the mixed nozzle tends to be difficult, and if it is less than 200 mesh, the feed to the mixed nozzle tends to be difficult.

As the mixing nozzle into which the organic solvent solution, steam and the polycarbonate powder are introduced, any type of mixing nozzle can be used, but one having an ejector structure is preferable.

To recover polycarbonate from the mixture injected from the mixing nozzle, for example, the injected mixture is introduced into a separator such as a gas-solid separation cyclone via piping, and the polycarbonate is separated by this separator. (Recovery). In this case, the pipe connecting the mixing nozzle and the separator may be a straight pipe or a curved pipe, but the pipe diameter (inner diameter) is 5 mn! ~ 25 cm, tube length is 50 cn! It is preferably about 100 m. Further, the ratio (LZD) of the tube length (L) to the tube tube (inner diameter D) is preferably 100 to 10000. If this ratio is less than 100, the evaporation of the organic solvent is insufficient, and if it exceeds 1000, the pressure loss increases, so that high-pressure steam is introduced as the steam introduced into the mixing nozzle. Required.

The polycarbonate finally obtained in this way is in the form of granules. (In the present invention, the granular polycarbonate obtained by the method m is also regarded as a polycarbonate powder. The bulk density is higher than that of the polycarbonate powder obtained by the conventional method or method I using mixed nozzles. The amount of the residual solvent in the polycarbonate powder obtained by the method m is equal to or less than the amount of the residual solvent in the polycarbonate powder obtained by the conventional method or the method I.

Method m can also be applied as a part of a process for producing polycarbonate by an interfacial polycondensation method. In this case, as an organic solvent solution of the polycarbonate to be introduced into the mixed nozzle, the polymer obtained by subjecting the emulsion solution obtained by the interfacial polycondensation reaction to washing and separation operations is used. Use a solution of carbonate in an organic solvent. Method W

The organic solvent solution used in Method IV is an organic solvent solution having a polycarbonate concentration of 3 to 45 wt%, as in Methods I, n, and m. The reason why the concentration of the polycarbonate is limited to 3 to 45 wt% is that if it is less than 3 wt%, the productivity of the high bulk density polycarbonate powder becomes too low. If it exceeds 5 wt%, the fluidity of the organic solvent solution will be too low, and it will be difficult to introduce it into the mixed nozzle. Particularly preferred concentrations are between 10 and 30 wt%.

The types of the above polycarbonates are not particularly limited, and various polycarbonates obtained by the reaction of divalent phenol with phosgene or a carbonate compound can be used. Bones can be used. Here, specific examples of the divalent phenol and the carbonate esterification product include various divalent phenols and various carbonates exemplified in the method I.

In the method IV, the above-mentioned organic solvent solution, steam and polycarbonate powder are introduced into a mixing nozzle, and the mixture injected from the mixing nozzle is introduced into a mixer.

Here, as the steam to be introduced into the mixing nozzle, it is preferable to use a steam having a pressure (pressure at the time of introducing the mixing nozzle) of l to 100 kgZcm ² and a temperature of 100 to 310. Yes. Also, the amount of steam introduced into the mixing nozzle should be the same as in Method I, that is, 1/10 to 1/5 times the weight of the organic solvent in the organic solvent solution introduced into the mixing nozzle. Good (hereinafter, this case is referred to as combination B with method I), but the same amount as in the conventional method, that is, more than 1 to 5 times the weight of the organic solvent in the organic solvent solution introduced into the mixed nozzle. (Hereinafter referred to as B in combination with the conventional method). If the amount of steam introduced into the mixing nozzle is less than 1/10, the evaporation of the solvent will be insufficient. -On the other hand, even if a large amount of steam is introduced into the mixing nozzle, the bulk density and production volume are reduced. Therefore, it is particularly preferable that the amount of steam introduced into the mixing nozzle is 110 to 1/1 times the weight of the organic solvent in the organic solvent solution introduced into the mixing nozzle.

As the mixing nozzle into which the above-mentioned steam and the above-mentioned organic solvent solution are introduced, any type of mixing nozzle can be used, but one having an ejector-single structure is particularly preferable.

The mixer into which the mixture injected from the mixing nozzle is introduced may be a dynamic mixer or a static mixer, and a crushable dynamic mixer is particularly preferable. Specific examples of the dynamic mixer include a pipe line homomixer 110 homomix clean flow manufactured by Tokushu Kika Kogyo Co., Ltd., a multiline mixer manufactured by Satake Chemical Industry Co., Ltd., and a Komatsu Zenoa Co., Ltd. Commuter—a day integrator. Specific examples of the static mixer include a Kenics-type static mixer, a Sulza-type static mixer, and a Toray-type static mixer.

The position of the mixer is L from the flow path from the mixing nozzle to the gas-solid separator, and from the mixing nozzle to the mixer. When the length of the flow path is jg, the position where the L value J2 is 5 or more, particularly 10 or more is preferable. When the mixer is disposed at a position where L is less than 5, the effect of improving the bulk density of the obtained polycarbonate powder is lower than when the mixer is at L = 5 or more. L means the length of the flow path from the outer end face of the jet outlet in the mixing nozzle to the outer end face of the inlet in the gas-solid separator. Also, 1 means the flow path length from the outer end face of the jet port in the mixing nozzle to the inner end face of the suction port in the mixer.

When using a dynamic mixer, the tip speed of the blade is preferably 50 to 2500 mZ, particularly 100 to 1500 m. When the blade tip speed is less than 50 mZ, the effect of improving the bulk density of the obtained polycarbonate is lower than in the case of 50 to 2500 mZ. Further, even when driven at a speed exceeding 250 OmZ, no further improvement in bulk density is observed.

In the method IV, the mixture discharged from the mixer is introduced into a gas-solid separator through piping, and the polycarbonate powder is recovered by the gas-solid separator. The recovery of the polycarbonate powder by the gas-solid separator can be carried out by an ordinary method using a usual gas-solid separator represented by a gas-solid separation cyclone.

In Method IV, when connecting the mixing nozzle to the mixer by a pipe, the pipe connecting the mixer and the gas-solid separator may be a straight pipe or a curved pipe, respectively. Pipe diameter (inner diameter) of each pipe D is 5 mn! It is preferable that the ratio of the flow path length L to the pipe diameter D (LZD) is 100 to 100 cm. If this ratio is less than 100, the evaporation of the organic solvent is insufficient, and if it exceeds 100 °, the pressure loss increases, so high-pressure steam is required as the steam introduced into the mixing nozzle. Becomes

The polycarbonate finally obtained in this way is in a granular form (in the present invention, the granular polycarbonate obtained by the method IV is also collectively referred to as a polycarbonate powder), and the organic solvent Compared with those having the same residual amount, they have a higher bulk density than the polycarbonate powder obtained by the conventional method or method I using a mixing nozzle. Further, the amount of residual solvent in the high bulk density polycarbonate powder is substantially the same as the amount of residual solvent in the polycarbonate powder obtained by the conventional method or method I.

In addition, the method w can be applied as a part of a process for producing a polycarbonate by an interfacial polycondensation method. In this case, the organic solvent solution to be introduced into the mixed nozzle is washed with the emulsion solution obtained by the interfacial polycondensation reaction, and the organic solvent of the polyethylene bottle obtained by performing the separation operation is used. Use solution.

Hereinafter, examples of the present invention will be described.

Example 1 (Method I) Polycarbonate (hereinafter sometimes abbreviated as PC) is Taflon A250〇 (trade name) manufactured by Idemitsu Petrochemical Co., Ltd., which is used as an organic solvent, methylene chloride. [Hiroshima Wako Pure Chemical Co., Ltd., special grade. Hereinafter, it may be abbreviated as MC. To prepare a methylene chloride solution of PC with a concentration of 13 wt% (hereinafter referred to as PCMC).

Next, this PCMC was used at a pressure of 14 kg / cm ² and a temperature of 195. The steam of C was simultaneously introduced into the mixing nozzle at a rate of 172.4 kg / hr and a rate of 25 kg / hr using a diaphragm pump. The ratio of the weight of a steam beam weight (w _c) and methylene chloride in this case _{_{(w MC) (W C ZW}} MC) was 1 Z6.

As the mixing nozzle, a mixing nozzle having the structure shown in Fig. 1 was used. The mixing nozzle 1 includes a first nozzle 3 having a spout 2 and a second nozzle 4 arranged such that the outer wall of the spout comes into contact with the inner wall of the spout of the first nozzle 3. ing. A mixing chamber 5 is formed in the inner space of the spout of the first nozzle 3. The spout of the first nozzle 3 is provided with a through hole 6 communicating with the mixing chamber 5, and the through hole 6 communicates with the PCMC supply pipe 7. The outer diameter a of the ejection beak of the first nozzle 3 is 50 mm, the maximum diameter b of the mixing chamber 5 is 30 mm, and the distance from the tip of the second nozzle 4 to the end face of the mixing chamber 5 on the side of the ejection port 2. c is 50 mm, internal space of nozzle 2 The diameter d of the narrowest part in is 5 mm. In the mixing nozzle 1, PCMC introduced into the mixing chamber 5 through the PCMC supply pipe 7 and the through hole 6 is mixed with steam introduced into the mixing chamber 5 through the second nozzle 4, and the mixture is mixed. As a result, it is jetted from spout 2.

The mixture injected from the mixing nozzle 1 passes through a stainless steel pipe with an inner diameter (D) of 10 mm, a pipe length (L) of 10 m, and an L / D of 100 mm, and the inner volume is ◦, 3 m Introduced to the ^third cycle.

After one hour operation, the desired high bulk density PC powder was obtained from the lower part of the cyclone. Table 1 shows the bulk density of the obtained high bulk density PC powder and the residual amount of MC (hereinafter referred to as residual MC amount). Table 1 also shows the amount of residual MC after drying the obtained high bulk density PC powder at 12 CTC for 4 hours (hereinafter referred to as the amount of residual MC after drying).

Example 2 (Method I)

PCMC were introduced into the mixing Bruno nozzle 1 at a rate of 2 1 5. 5 kg / hr, except that the W _S / W _M to 1 / 7.5 in the same manner as in Example 1, a high bulk density PC powder Obtained.

Table 1 shows the bulk density, the amount of residual MC, and the amount of residual MC after drying of the obtained high bulk density PC powder.

Example 3 (Method I)

PCMC were introduced into the mixing nozzle 1 at a rate of 2 58. 6 kgZhr, except that the W _s ZW _Me 1 Bruno 9 in the same manner as in Example 1 to obtain a high bulk density PC powder. Table 1 shows the bulk density, residual MC amount and residual MC amount after drying of the obtained high bulk density PC powder.

Example 4 (Method I)

The concentration of PC in PCMC was set to 8 wt%, and this PCMC was introduced into mixing nozzle 1 at a rate of 203.8 kgZhr,

A high bulk density PC powder was obtained in the same manner as in Example 1 except that the ratio was changed to 1 / 7.5.

Example 5 (Method I)

The same procedure as in Example 1 was carried out except that the concentration of PC in PCMC was 25 wt%, this PCMC was introduced into the mixing nozzle 1 at a rate of 250 kgZhr, and W s ZW _Me was changed to 1 Z7.5. A high bulk density PC powder was obtained.

Example 6 (Method I)

The structure of the mixing nozzle is the same as that of the mixing nozzle 1 shown in Fig. 1; the outer diameter a of the spout of the first nozzle 3 is 150 mm, and the maximum diameter b of the mixing chamber 5 is 90 mnu. Distance from the tip of the second nozzle 4 to the end face on the side of the jet port 2 in the mixing chamber 5 c Force << 100 mni, mixing nozzle whose diameter d at the narrowest part in the internal space of the second nozzle is 15 mm Was used. Then, the mixed nozzle was concentrated at 13 wt% PCMC, the pressure was 14 kg / cm ² and the temperature was 195. With the steam of C, They were simultaneously introduced at a rate of 1 724 kgZhr and 200 kgZhr, respectively, using a diaphragm pump. At this time, _{WS /} _WMC was 1 / 7.5.

The mixture injected from the mixing nozzle passes through a stainless steel pipe with an inner diameter (D) of 30 mm, a pipe length (L) of 30 m, and an L nozzle of 100, and an internal volume of 2 m ³ Introduced to the cyclone.

After running for 1 hour, the desired high bulk density PC powder was obtained from the lower part of the cyclone. Table 1 shows the bulk density, residual MC amount and residual MC amount after drying of the obtained high bulk density PC powder.

Comparative example 1

PC powder was obtained in the same manner as in Example 1 except that PCMC was introduced into the mixing nozzle 1 at a rate of 1 14.9 kgZhr and W _s ZWj ^ was reduced to 1/4.

Table 1 shows the bulk density, the amount of residual MC and the amount of residual MC after drying of the obtained PC powder.

Comparative Example 2

PCMC were introduced into the mixing nozzle 1 at a rate of 5 7. 5 kg hr, except that the W _s ZW _M to 1 Bruno 2 in the same manner as in Example 1 to obtain a PC powder.

Comparative Example 3

PCMC mixed nozzle at a rate of 344.8 kg / hr 1 Introduced into, except that the W _s Roh W _Me 1 Bruno 1 2 in the same manner as in Example 1 to obtain a PC powder.

PC powder in PCMC

PC concentration ^W S ^{/ W} MC Bulk density Residual MC amount Residual MC amount after drying

(wt%) (g / cc) (w 1 ppm) (, w 1 ppmExample 1 13 1/6 0.41 90 <10 Example 2 13 1 / 7.5 0.48 90 1/9 0.55 100 <10 Example 4 8 1 / 7.5 0.50 100 <10 Example 5 25 1 / 7.5 0.47 90 <10 Example 6 13 1 / 7.5 0. 48 90 <10 Example 1 13 1/4 0.35 90 <10 Example 2 13 1/2 0.25 25 90 <10 Example 3 13 1/12 0.50 20000 500

* 1: Indicates the concentration of PC in PCMC.

* 2: Indicates the ratio of the weight of steam introduced into the mixing nozzle (WcJ and the weight of methylene chloride (W _Me ).

Table l As is apparent, the bulk density of the high bulk density PC powder obtained by w _s w _Me first to sixth embodiments were within the limit fixed range of methods I and the ◦. 4 1 0. 55 g Zcc. These values are based on the bulk density (0.35 to 0.25 g) of each PC powder obtained in Comparative Examples 1 and 2 in which W _s ZW ^ was larger than the upper limit of the limited range of Method I. Much larger than Z cc).

The residual MC amount of each of the high bulk density PC powders obtained in Examples 1 to 6 was as small as 90 to 100 wtppm, and these values were obtained in Comparative Examples 1 and 2. It is equivalent to the residual MC amount of PC powder (90 wtppni). Regarding the amount of residual MC after drying, any of the high bulk density PC powders obtained in Examples 1 to 6 was the same as each PC powder obtained in Comparative Example 1 and Comparative Example 2. , Less than 10 tppm.

Note that w _s

The PC powder of Comparative Example 3 obtained by making it smaller than the lower limit of the limited range of I has a large bulk density of 0.50 g / cc, but has an extremely large amount of residual MC and residual MC after drying.

Example 7 (Method Π)

As shown in FIG. 2, a first mixing nozzle 11 into which PCMC and steam are introduced, and a mixture injected from the first mixing table nozzle 11 are introduced through a pipe 20 and steam is also introduced. The second mixing nozzle 21 and the mixing injected from the second mixing nozzle 21 Using a device equipped with a cyclone 31 into which the compound (second mixture) was introduced through a pipe 30, a high bulk density PC powder was produced in the following manner based on Method II.

First, Teflon A 2200 (trade name) manufactured by Idemitsu Petrochemical Co., Ltd. was used as the PC, and this PC was used as an organic solvent, methylene chloride (MC) [Hiroshima Wako Pure Chemicals, special grade] To prepare PCMC with a concentration of 15 wt%.

Next, this PCMC and steam having a pressure of 15 kg / cm ² and a temperature of 20 CTC were applied to the first mixing nozzle 11 using a diaphragm pump at a ratio of 14 ◦ kgZhr and 10 kgZhr, respectively. Introduced at the same time. At this time, the weight of the steam (w _si ) is 1Z11.9 times the weight of the methylene chloride (w _CM ).

As the first mixing nozzle 11, a mixing nozzle having the structure shown in FIG. 3 was used. That is, the first mixing nozzle 11 is disposed such that the outer wall of the jet nozzle is in contact with the first nozzle 13 having the jet port 12 and the inner wall of the jet nozzle of the first nozzle 13. And a second nozzle 14. A mixing chamber 15 is formed in the internal space of the spout of the first nozzle 13. The spout in the first nozzle 13 is provided with a through hole 16 communicating with the mixing chamber 15, and the through hole 16 communicates with the PCMC supply pipe 17. The outer diameter ai of the spout of the first nozzle 13 is 50 mm, and the maximum diameter of the mixing chamber 15 b _} Is 30 mm, the distance c from the tip of the second nozzle 14 to the end face on the side of the outlet 12 in the mixing chamber 15 is 50 mnu, the diameter of the narrowest part in the internal space of the second nozzle 14 di Is 5 mm, and the diameter e ^ of the spout 12 is 10 mni. In the mixing nozzle 11, the PCMC introduced into the mixing chamber 15 via the PCMC supply pipe 17 and the through-hole 16 is the steam introduced into the mixing chamber 15 via the second nozzle 14. And mixed with each other, and the mixture is ejected from the ejection port 12.

The mixture injected from the first mixing nozzle 11 was introduced into the second mixing nozzle 21 through the pipe 20. As the pipe 20 at this time, a stainless steel pipe having an inner diameter of 10 mm was used, and the length of the pipe 20 was set so that the residence time r of the mixture was 0.01 second. Separately, steam at a pressure of 15 kg / cm ² and a temperature of 200 ° C. was introduced simultaneously into the second mixing nozzle 21 at a rate of 3 kg / hr. The weight of the steam (w _S2 ) at this time is

It is 1 / 3.7 times the weight (W _M ) of the MC introduced into one mixing nozzle 11.

As the second mixing nozzle 21, a mixing nozzle having a structure shown in FIG. 4 was used;]]. That is, the mixing nozzle 21 is arranged such that the outer wall of the jet nozzle is in contact with the first nozzle 23 having the jet port 22 and the inner wall of the jet nozzle of the first nozzle 23. The second nozzle 24 is provided, and the internal space of the jet nozzle of the first nozzle 23 is mixed. A joint room 25 is formed. In addition, the spout in the first nozzle 23 is provided with a through-hole 26 that communicates with the mixing chamber 25. The through-hole 26 communicates with the steam supply pipe 27. The outer diameter a ₂ of the jetting beak of the first nozzle 23 is 50 mm, the maximum ¾b ₂ of the mixing chamber 25 is 30 mm, from the tip of the second nozzle 24 to the end face of the mixing chamber 25 on the side of the jet port 22. the distance c ₂ 50mni, the diameter d ₂ of the narrowest portion in the interior space of the second nozzle 24 1 0 mm, diameter € ₂ jets 2 2 is 1 0 mm. In this mixing nozzle 21, the mixture from the first mixing nozzle 11 introduced into the second nozzle 24 through the pipe 20 is introduced into the mixing chamber 25 through the second nozzle 24, At 25, the mixture is mixed with the steam introduced into the mixing chamber 25 through the steam supply pipe 27 and the through hole 26, and is jetted from the outlet 22.

The mixture (second mixture) injected from the second mixing nozzle 21 is introduced into the cyclone 31 through the pipe 30, and when the PC powder is separated (collected) by the cyclone 31. At the same time, MC and steam were condensed and recovered by capacitor-32. As the pipe 30, a stainless steel pipe with an inner diameter of 1 Omm and a length of about 20 m was used.

The device shown in Fig. 2 was operated for 2 hours continuously. During the operation period, there was no trouble such as blockage, and stable operation was possible. 0 After rotating for 2 hours, the desired high bulk density PC powder was obtained from the lower part of cyclone 31. Table 2 shows the bulk density and residual MC amount of the obtained high bulk density PC powder.

Examples 8 to 18 (Method Π)

The amounts of PCMC and steam introduced into the first mixing nozzle 11 and the amount of steam introduced into the second mixing nozzle 21 were changed as shown in Table 2, and the first mixing nozzle 1 1 In the same manner as in Example 7 except that the length of the pipe 20 connecting the second mixing nozzle 21 and the second mixing nozzle 21 was appropriately set so that the residence time of the mixture was as shown in Table 2, FIG. High bulk density PC powder was obtained using the apparatus shown.

Table 2 shows the bulk density and residual MC amount of each of the obtained high bulk density PC powders.

In each of Examples 8 to 18, during the operation period of the apparatus, there was no trouble such as blockage, and stable operation was possible.

Example 1 9 (Method Π)

A high bulk density PC powder was obtained using the apparatus shown in FIG. 2 in the same manner as in Example 7 except that CMC having a PC concentration of 12 2% was used. In addition, as the concentration of PC decreased from 15 wt% (Example 7) to 12 wt%, the amount of introduced steam _wsl (= 1

O kg / hr) is 1/1/3 times the _MC introduction amount W _MC , and W _S9 (= 3 kg / hr) in the second mixed nozzle 21 is 1 Z4 1.1 of W _MC Doubled. The bulk density and residual MC amount of the obtained high bulk density PC powder were not changed to ^;

In addition, the operation period Φ of the device was stable without any trouble such as blockage.

Example 20 (Method Π)

A high bulk density PC powder was obtained using the apparatus shown in FIG. 2 in the same manner as in Example 7 except that pulp CMC having a PC concentration of 271% was used. As the concentration of PC increased from 15 wt% (Example 7) to 27%, W _S1 (= 10 kg / hr) at the first mixing nozzle 11 became smaller than W _M. The ratio of W _C2 (= 3 kg / hr) in the second mixing nozzle 21 was 1 / 14.1 times as large as that of W ^{M, and} was 134.1 times as large as that of WM.

Table 2 shows the bulk density and residual M C amount of the obtained high bulk density PC powder.

During the operation period of the equipment, there was no trouble such as blockage. The operation was stable.

Example 2 1-2 (Method Π)

Example 7 except that the amount of PCMC and steam introduced into the first mixing nozzle 11 and the amount of steam introduced into the second mixing nozzle 21 were changed as shown in Table 2, respectively. In the same manner as described above, high bulk density PC powder was obtained using the apparatus shown in FIG. However, the inner diameter of the pipe 2 ◦ connecting the first mixing nozzle 11 and the second mixing nozzle 21 was set to 20 mm in Example 21 and 35 mm in Example 22. By making the respective changes, the residence time r of the mixture was set at 0.01 seconds, which was the same as in Example 7.

In each of Examples 21 to 22, there was no trouble such as blockage during the operation of the apparatus, and stable rotation was possible.

Comparative example 4

As shown in Table 3, a PC powder was obtained using the apparatus shown in FIG. 2 in the same manner as in Example 7 except that no steam was supplied to the second mixing nozzle 21.

At this time, the solvent MC (liquid) is discharged together with the PC powder from the outlet of the cyclone 31 side of the pipe 3 ◦ connecting the second mixing nozzle 21 and the cyclone 31, which is extremely unsuitable for practical use. It turned out that there was.

Table 3 shows the bulk density and the amount of residual MC of the obtained PC powder.

Comparative Examples 5 to 8

As shown in Table 3, the example was conducted except that the amount of steam introduced into the first mixing nozzle 11 or the amount of steam introduced into the second mixing nozzle 21 was out of the limited range of the method Π. In the same way as in 7, the production of PC powder was attempted using the equipment shown in Fig. 2. However, by changing the length of the pipe 20 connecting the first mixing nozzle 11 and the second mixing nozzle 21 as appropriate for each comparative example, the mixture was retained. The retention time was the same as that of Example 7 and was set to 0. 1 second. Table 3 shows the results.

Comparative Example 9

As shown in Table 3, the amounts of PCMC and steam introduced into the first mixing nozzle 11 and the amounts of steam introduced into the second mixing nozzle 21 were changed, respectively. In the same manner as in Example 7, except that the amount of steam introduced in 11 and the amount of steam introduced in the second mixing nozzle 21 were out of the limited range of the method により, the apparatus shown in FIG. PC powder was obtained. However, by changing the length of the pipe 20 connecting the first mixing nozzle 11 and the second mixing nozzle 21, the residence time r of the mixture was the same as in Example 7: 0.01 second. I made it.

Table 3 shows the bulk density and residual MC amount of the obtained PC powder.

Comparative Example 10: L 1

Example 1 except that the residence time τ of the mixture was set to the time shown in Table 3 by changing the length of the pipe 20 connecting the first mixing nozzle 11 and the second mixing nozzle 21. In the same manner as in 7, a PC powder was obtained using the apparatus shown in FIG.

Table 3 shows the bulk density and residual MC content of the obtained PC powder.

Comparative Example 1 2

As shown in Table 3, PC to first mixed nozzle 11 The amount of MC introduced and the amount of steam introduced to the second mixing nozzle 21 were changed respectively, and the length of piping 20 connecting the first mixing nozzle 11 and the second mixing nozzle 21 In the same manner as in Example 7, except that the residence time of the mixture was set to 0.00 Was.

^ 7] "90

Table 2

No. 1 mixing nozzle No. 2 mixing nozzle High bulk density Pc powder

P C M C Steam Team

Bulk density Residual MC amount

PC concentration Introduction shaking Introduced amount w _sl w Introduced amount for _Me W _C2 w _M Residence time r

(g / cc) t w 1 D D m)

(wl%) (ig / hr) (kg / hr) Factor (times) Og / hr) Factor (times) (seconds)

Example 7 15 140 10 1/11. 9 3 1/39. 7 0.01 0.49 40 Example 8 15 1 0 8 1 / 14.9 10 \ / \ 1.90.005 0.46 60 Male Example 9 15 140 6 1/19. 8. 50 1 / 2.4 0 03 0.49 45 Implemented clear 10 15 1 0 10 1/11. 9 1 1/119 0.01 0.42 90 M i 1 15 140 10 10 1/11. 9 0.01 0.45 30

Hife example 12 15 140 10 1 / 11.9 100 1 / 1.2 0.01 0.48 40Example 13 15 140 10 3 1 / 39.7 0.001 0.36 80

15 200 20 1/8. 5 10 1/17. 0 0.02 0.51 45

1—

Example 15 15 200 20 1 / 8.5 10 1 / 17.0 0.02 0.46 30

¾ί¾ ^ 116 15 200 25 50 1/3. 4 0.005 0.39 30 Example 17 15 50 5 1/8. 5 10 1 / 4.3 0.01 0.1 50 Implementation cool 18 15 50 3 1 / 14. 2 1 1 / 42.5 0.01 0.39 45 Example 19 12 140 10 1 / 12.3 3 1 / 1.1 0.01 0.54 20 Example 20 27 140 10 1/10. 2 3 1 / 34.1 0.01 0.44 100 Implementation ^ 21 15 400 40 1 / 8.5 12 1 / 28.3 0.01 0.48 55 Example 22 15 900 90 1 / 8.5 30 1 / 25.5 0.01 0.46 30

Table 3

The first mixed nozzle The second mixed nozzle c of the powder mixture

P C M C Steam Team

Bulk density Residual MC amount

The residence time r to the introduction amount w _S2 ^W _MC for PC concentration introduction amount introduced amount w _sl w _MC

(g / cc) (w 1 p pm) (wt%) (kg / hr) (kfj / lir) Factor (times) (kg / hr) Factor (times) (seconds)

Comparative example 4 15 1 0 10 1/11. 9 0 0.01 0.25 1800 Comparative example 5 15 140 2 1 / 59.5 10 1/1 1.9 0.01 0.10 12000 Comparative school ^ 6 15 140 1 1/119 10 1/11. 9 0.01 Not powdered Comparative example 7 15 140 500 1 / 0.238 10 1/11. 9 0.01 0.12 <10 Comparative mosquito example 8 15 140 10 1/11. 9 200 1 / 0.595 0.01 0.32 360 Comparative example 9 15 50 10 1 / 4.25 200 1 / 0.213 0.01 0.13 <10 Comparative example 10 15 140 10 1/11. 9 3 1/39. 7 3 0.41 32000 Comparative example 11 15 140 10 1/11. 9 3 1/39. 7 0.0005 0.16 30 Comparative example 12 15 200 10 1/17. 0 10 1/17. 0 0.0005 0. 1 120

As apparent from Table 2, the bulk density of each of the high bulk density PC powders obtained in Examples 7 to 22 is 0.36 to 0.54 g / cc. These values are larger than the bulk density of the PC powder obtained by the conventional method using one mixing nozzle, ie, ◦.05 to 0.35 g / cc. Further, the residual MC amount of each of the high bulk density PC powders obtained in Examples 7 to 22 is as small as 20 to: LOO wtppm. In addition, in Examples 7 to 22, even though the treatment amount of the organic solvent solution of PC (methylene chloride solution) was varied in the range of 50 to 900 kg / hr, Also in Example 1, a high bulk density PC powder was stably obtained, and a change in properties of the obtained high bulk density PC powder was small.

On the other hand, as is clear from Table 3, in Comparative Examples 4 to 12, no PC powder was obtained (Comparative Example 6), and the solvent MC (liquid) was discharged together with the PC powder (Comparative Example 4). The bulk density of the obtained PC powder is low (Comparative Examples 5, 7, 8, 91, and 12), and the bulk density of the obtained PC powder is high but the residual amount of MC is large (Comparative Example 10). And other difficulties.

Example 2 3 (Method ΠΙ; Combination with Method I A)

As shown in FIG. 5, a mixing nozzle 41 into which PCMC, steam, and PC powder (abbreviated as PCF in the figure) are introduced, and a mixture injected from the mixing nozzle 41 is introduced through a pipe 50. High bulk density PC powder was produced using the equipment equipped with a cyclone 51 as follows. Was.

First, Taflon A250 (trade name) manufactured by Idemitsu Petrochemical Co., Ltd. was used as the PC, and this PC was converted to methylene chloride (MC) [Hiroshima Wako Pure Chemical Co., Ltd., special grade. To prepare PCMC with a concentration of 13 wt%.

Next, this PCMC was used at a pressure of 14 kg / cm ² and a temperature of 195. C steam and PC powder [Product name: Toughlon FN2200, manufactured by Idemitsu Petrochemical Co., Ltd.] Particle size: 10 ~: L00 mesh. Hereinafter, it is called PCF. Were simultaneously introduced into the mixing nozzle 41 at a rate (feed speed) of 25.5 kg / hr, 25 kg / hr, and 1.4 kg / hr using a diaphragm pump. The PCF is connected to a steam line (not shown in Fig. 5) via a rotary valve (not shown in Fig. 5) from a hopper (not shown in Fig. 5) whose internal pressure is kept equal to the steam pressure. ) And introduced into the mixing nozzle 41 in a state of being mixed with steam.

At this time, the amount of steam introduced into the mixed nozzle 41 (weight per unit time; the same applies hereinafter) is determined by the weight of MC in PCMC introduced into the mixed nozzle 41 (weight per unit time). The same shall apply hereinafter.) 1 / 7.5 times that of the above, and the amount of PCF introduced into the mixing nozzle 41 (weight per unit time; the same applies hereinafter) is the PCMC width introduced into the mixing nozzle 41. 5% of the weight of the PC (weight per unit time; the same applies hereinafter). As the mixing nozzle 41, a mixing nozzle having the same shape and the same size as the mixing nozzle shown in FIG. 1 was used.

The mixture injected from the mixing nozzle 41 passes through a stainless steel pipe 50 with an inner diameter (D) force of <10 mni, a pipe length (L) of 1 1m, and a L force of D <100 m, as shown in 5, it is introduced into re-Gu b down 5 1 of internal volume of 0. 3 m ^3, this cyclic black down 5 1 separated PC powder (recovery) then both the MC and steam condenser 5 2 More condensed and recovered.

After operating the apparatus shown in FIG. 5 for 1 hour, the desired high bulk density PC powder was obtained from the lower part of the cyclo 51. Table 4 shows the bulk density and residual amount of MC of the obtained high bulk density PC powder.

Examples 24 to 28 (Method ΙΠ; Combination with Method I A) In the same manner as in Example 23 except that the amounts of PCMC and PCF introduced into the mixing nozzle 41 were as shown in Table 4. Thus, high bulk density PC powder was obtained using the apparatus shown in FIG. As shown in Table 4, the amount of steam introduced into the mixing nozzle 41 (= 25 kg / hr) was changed according to the introduction amounts of PCMC and PCF as shown in Table 4. 4 1 Z 7.5 to 9 times the weight of MC in PCMC introduced into 1 and the amount of PCF introduced into mixing nozzle 41 is PC in PCMC introduced into mixing nozzle 41 2-1% of the weight.

Bulk density and residual MC of high bulk density PC powder obtained The amounts are not shown in Table 4.

Example 2 9 (combination A with method I)

Using PCMC with a PC concentration of 8 wt%, the amount of PCMC introduced into the mixing nozzle 41 and the amount of PCF introduced into the mixing nozzle 41 were 203.8 kgZhr, as shown in Table 4, respectively. A high bulk density PC powder was obtained using the apparatus shown in FIG. 5 in the same manner as in Example 23 except that the amount was changed to 8 15 g Zhr. As shown in Table 4, the concentration of PC,

With the amount of PCMC introduced and the amount of PCF introduced as shown in Table 4, the amount of steam introduced into mixing nozzle 41 (= 25 kgZhr) was determined by the amount of PCMC introduced into mixing nozzle 41. The amount of PCF introduced into the mixing nozzle 41 was 5% of the weight of PC in the PCMC introduced into the mixing nozzle 41. Same as Example 23.

Table 4 shows the bulk density and residual M C amount of the obtained high bulk density PC powder.

Example 30 (combination A with method I)

Using PCMC with a PC concentration of 25 wt%, the amount of PCMC introduced into the mixing nozzle 41 and the amount of PCF introduced into the mixing nozzle 41 were determined as shown in Table 4, respectively. A high bulk density PC powder was obtained using the apparatus shown in FIG. 5 in the same manner as in Example 23, except that kgZhr and 3.13 kg, hr were used. Table 4 shows the concentration of PC, the amount of PCMC introduced, and the amount of PCF introduced, as shown in Table 4. As a result, the amount of steam introduced into the mixed nozzle 41 (= 25 kg / hr) was 1% of the weight of MC in PCMC introduced into the mixed nozzle 41 7. Five times, the amount of PCF introduced into the mixing nozzle 41 was 5% of the weight of PC in PCMC introduced into the mixing nozzle 41, and these values were the same as in Example 23. .

Example 3 1 to 32 (combination with conventional method A)

A high bulk density PC powder was obtained using the apparatus shown in FIG. 5 in the same manner as in Example 23 except that the amount of PCCM introduced into the mixing nozzle 41 and the amount of PCF introduced were as shown in Table 4. Was. As shown in Table 4, the introduction amount of steam into the mixing nozzle 41 (= 25 kg / hr) was changed with the introduction amounts of PCMC and PCF as shown in Table 4. 12 times the weight of MC in PCMC introduced into the nozzle 41, and the amount of PCF introduced into the mixing nozzle 41 is the amount of PC in PCMC introduced into the mixing nozzle 41. Between 5 and 10%.

Reference Example 1 (Method I)

As shown in Table 5, in the same manner as in Example 23 except that PCF was not introduced into the mixing nozzle 41, the PC powder (high bulk density PC by Method I) was obtained using the apparatus shown in FIG. One of the powders) was obtained.

Table 5 shows the bulk density and residual MC amount of the obtained PC powder.

Reference Example 2 (Method I)

As shown in Table 5, in the same manner as in Example 26 except that PCF was not introduced into the mixing nozzle 41, PC powder was used (one of the high bulk density PC powders by Method I) using the apparatus shown in FIG. I got

Reference Example 3 (Method I)

As shown in Table 5, in the same manner as in Example 29 except that PCF was not introduced into the mixing nozzle 41, PC powder was used (one of the high bulk density PC powders by Method I) using the apparatus shown in FIG. I got

Reference Example 4 (Method I)

As shown in Table 5, in the same manner as in Example 30 except that PCF was not introduced into the mixing nozzle 41, the PC powder was used by the apparatus shown in FIG. 5 (one of the high bulk density PC powders by Method I). I got

Table 5 shows the bulk density and residual amount of MC of the obtained PC powder.

Comparative Example 13 (Conventional method) As shown in Table 5, in the same manner as in Example 31 except that PCF was not introduced into the mixing nozzle 41, PC powder (one of the conventional PC powders) was obtained using the apparatus shown in FIG. Was.

* 2 The figures in parenthesis [], the ratio of steam to the weight of MC was introduced into the mixing nozzle (weight per unit time) (unit: times) _c showing the

* 3 The value in [] indicates the ratio (unit:%) of PCF to the weight (weight per unit time) of PC introduced into the mixing nozzle.

What

m

Table 5

Amount introduced into the PC mixed nozzle (weight per unit time) PC powder concentration * 1 PCM C (kg / hr) Steam bulk density Residual MC amount

P C F

(t%) Total amount P C M C (kg / hr) i.wt ppm)

twenty five

Reference example 1 1 3 2 1 5.5 5 28. 0 1 87. 5 0. 4 8 9 0

53

twenty five

Reference Example 2 25 8. 6 33. 6 22 5.0 0 0.5 5 00

[1/9]

twenty five

Reference Example 3 203. 8 1 6. 3 1 87. 5 0.5 0.50 1 00

Five]

twenty five

Reference example 4 2 5 2 50 62.5 87.5 0.4 7 9 0

Five]

twenty five

Comparative example 13 1 3 57.5 7.5 5.50 0 .0 2 .5 9 0

[1/2]

* 1: Inconcentration of PC in PCCM.

* 2: The value in [] indicates the ratio of steam (unit: times) to the weight (weight per unit time) of MC introduced into the mixing nozzle.

As is clear from Table 4, the bulk density of each of the high bulk density PC powders obtained in Examples 23 to 30 in which PCF was introduced into the mixed nozzle based on Method I was 0.58 to 0.5. It is 66 g Zcc. These values are much larger than the bulk density (0.47 to 0.55 g / cc, see Table 5) of the PC powders obtained in Reference Examples 1 to 4, which are examples of Method I. . The bulk density of each of the high bulk density PC powders obtained in Examples 31 to 32 in which PCF was introduced into the mixing nozzle based on the conventional method is 0.36 to 0.38 g / cc. These values are much larger than the bulk density (0.25 g / cc) of the PC powder obtained in Comparative Example 5, which is an example of the conventional method.

Furthermore, the residual MC amount of each of the high bulk density PC powders obtained in Examples 23 to 32 was as small as 80 to: L00 wtppm, and these values were found in Reference Examples 1 to 4 and Comparative Example 13. It is equal to or less than the residual MC amount (90 to 100 wtppm) of each PC powder obtained in the above.

Example 33 (Method IV; Combination with Method I B)

As shown in FIG. 6, a mixing nozzle 61 into which PCCM and steam are introduced, a dynamic mixer 71 into which a mixture injected from the mixing nozzle 61 is introduced through a pipe 70, and Using a device equipped with a cyclone 73 through which the mixture discharged from the mechanical mixer 71 was introduced via a pipe 72, high bulk density PC powder was produced in the following manner. First, Taflon A250 (trade name) manufactured by Idemitsu Petrochemical Co., Ltd. was used as the PC, and this PC was used as the organic solvent, methylene chloride (MC) [Hiroshima Wako Pure Chemical Co., Ltd. PCMC with a concentration of 13 wt% was prepared.

Next, the PCMC and steam at a pressure of 14 kg / cm ² and a temperature of 195 ° C. were mixed at a rate of 25.5 kg / hr and 25 kg / hr, respectively (feed). At the same time, a diaphragm pump was used to simultaneously introduce the mixture into the mixing nozzle 61. At this time, the amount of steam introduced into the mixing table nozzle 6 1

(Weight per unit time; the same applies hereinafter) is 7.5 times the weight of the MC in the PCMC introduced into the mixing nozzle 61 (weight per unit time; the same applies hereinafter).

As the mixing nozzle 61, a mixing nozzle having the same shape and the same size as the mixing nozzle shown in FIG. 1 was used.

The mixture injected from the mixing nozzle 61 was introduced into the dynamic mixer 71 through a pipe 70 having an inner diameter D of 10 mm. The dynamic mixer 71 is a dynamic mixer manufactured by Tokushu Kika Kogyo Co., Ltd. (trade name: TK Pipeline Ho-Mixer SL type, 50 cc capacity, 4-turbine blade, The blade diameter was about 754 m (600 rpm) using a 4-turbine blade with a diameter of 4 cm.

The mixture discharged from the dynamic mixer 71 is passed through a stainless steel pipe 72 having an inner diameter D of 10. Introduced into re-Gu B down 7 3 Sekiryokuku 0. 3 m ^8, the PC powder Ri by this re-Gu B down 7 3 separation (recovery) Then in together, Ri by the MC and steam condensers 74 It condensed and collected.

In Example 33, the flow path length 1 from the mixing nozzle 61 to the dynamic mixer 71 was 0.5 m, and the flow path length from the mixing nozzle 61 to the gas-solid separator (cyclone 73) was 0.5 m. The flow path length L is 10 m, and L / 1 is 20.

Figure 6 (After operating the indicated device for 1 hour, the desired high bulk density PC powder was obtained from the lower part of the cyclone 73. The bulk density and residual MC amount of the obtained high bulk density PC powder are shown in Table 6. Shown in

Example 34 (Method IV; Combination with Method I B)

A high bulk density PC powder was obtained using the apparatus shown in FIG. 6 in the same manner as in Example 33, except that the amount of PCMC introduced into the mixed nozzle 61 was 258.6 kg / hr. As shown in Table 6, the amount of steam introduced into the mixing nozzle 61 (= 25 kg / hr) was changed due to the change in the amount of PCMC introduced. The weight of the MC was 9 times higher.

Table 6 shows the bulk density and residual M C amount of the obtained high bulk density PC powder.

Example 35 (Method IV; Combination with Method I B)

Using PCMC with a PC concentration of 8 wt%, the amount of PCMC introduced into the mixing nozzle 61 was 203.8 kg / hr. A high bulk density PC powder was obtained in the same manner as in Example 33 by using the apparatus shown in FIG. As shown in Table 6, the amount of steam introduced into the mixing nozzle 61 (= 25 kg / hr) is 1 / 7.5 times the weight of MC in PCMC introduced into the mixing nozzle 61. This value is obtained in Example 3.

Same as 3.

Example 36 (Method IV; Combination with Method I B)

A PCMC having a PC concentration of 25 wt% was used, and the amount of PCMC introduced into the mixing nozzle 61 was set to 250 kgZhr. A high bulk density PC powder was obtained. As shown in Table 6, the amount of steam introduced into the mixing nozzle 61 (= 25 kg / hr) was 1 Z 7.5 times the weight of MC in PCMC introduced into the mixing nozzle 61. Yes, this value is the same as in Example 33.

Example 37 (Method IV; Combination with Method I B)

In the same manner as in Example 33 except that the blade tip speed was set to about 110 minutes (900 rpm) and the dynamic mixer 71 was used, a high bulk density was obtained by the apparatus shown in FIG. PC powder was obtained.

Bulk density and residual MC of high bulk density PC powder obtained The amounts are shown in Table 6.

Example 38 (Method IV; Combination with Method I B)

In the same manner as in Example 33 except that the blade tip speed was set to about 126 m (l OOO rpm) and the dynamic mixer 71 was used, high bulk density PC powder was obtained using the apparatus shown in Fig. 6. I got

The bulk density and residual MC weight of the obtained high bulk density PC powder are not shown in Table 6.

Example 39 (Method IV; Combination with Method I)

A static mixer, a Sulza complete static mixer [mixing element used and the number of used: 10 SMV type of Sumitomo Heavy Industries, Ltd.] was added to the dynamic mixer 71 in Example 33. A high bulk density PC powder was obtained in the same manner as in Example 33 except that the powder was used instead. At this time, the flow path length 1 from the mixing nozzle 61 to the static mixer was 0.5 m, the flow path length L from the mixing nozzle 61 to the cyclone 73 was 1 m, and LZ 1 Is 20.

Example 40 (Method IV; Combination with Conventional Method B)

A high bulk density PC powder was obtained using the apparatus shown in FIG. 6 in the same manner as in Example 33, except that the amount of PCM introduced into the mixing nozzle 61 was 57.5 kg / hr. As shown in Table 6, following the change in the amount of PCMC introduced, The amount of steam introduced into the mixing nozzle 61 (= 25 kg / hr) was 1/2 times the weight of MC in PCMC introduced into the mixing nozzle 61.

Reference Examples 5 to 8 (Method I)

This is shown in Fig. 6 except that the mixing nozzle 61 and the cyclone 73 were directly connected with a stainless steel pipe with an inner diameter of 10 mm and a length of 10 m without using the dynamic mixer 71. PC powder (one of high bulk density PC powders by method I) was obtained in the same manner as in Example 33, Example 34, Example 35 or Example 36, using the same apparatus as the apparatus. .

Table 6 shows the bulk density and the amount of residual MC of the obtained PC powder.

Comparative Example 14 (conventional method)

Except that the dynamic mixer 71 was not used, the mixing nozzle 61 and the cyclone 73 were connected directly with a stainless steel pipe with an inner diameter of 10 mm and a length of 1 Om. A PC powder (one of conventional PC powders) was obtained in the same manner as in Example 40 using the same apparatus.

Table 6 shows the bulk density and residual MC amount of the obtained PC powder.

* 1: Indicates the i degree of PC in PCMC.

* 2: The value in [] indicates the ratio (unit: times) of the amount of introduced steam to the introduced AS of MC introduced into the mixing nozzle.

As can be seen from Table 6, the bulk density of each of the high bulk density PC powders obtained in Examples 33 to 39 using the mixer in combination with Method I based on Method I was 0.53 to 0.6. 5 g / cc. These values are the values of the bulk density of PC powders obtained in Reference Examples 5 to 8 which are examples of Method I (0.47 to 0. 55 g / cc. See Table 6.) Larger than. Further, the bulk density of the high bulk density PC powder obtained in Example 40 using a mixer in combination with the conventional method is 0.37 g / cc. This value is much larger than the bulk density (0.25 g Zcc) of the PC powder obtained in Comparative Example 14 which is an example of the conventional method.

Furthermore, the residual MC amount of each of the high bulk density PC powders obtained in Examples: 33 to 40 was as small as 90 to: LO Owtppm, and these values are as in Reference Examples 5 to 8 and It is substantially equivalent to the residual MC amount (90 to 100 wtppm) of each PC powder obtained in Comparative Example 14.

As described above, in any of the methods I to IV, the polycarbonate powder having a higher bulk density than the conventional polycarbonate powder can be easily prepared without increasing the amount of residual solvent. Can be obtained.

The high bulk density polycarbonate powder obtained by these methods can improve the volumetric efficiency of the processing equipment used for post-processing such as drying or storage, and can achieve a high density. Easy molding into pellets -5-It is possible.

Therefore, by implementing the present invention, it is possible to improve the productivity of high quality polycarbonate products.

Further, according to the method (2), it is possible to easily obtain a polycarbonate powder having a high bulk density and a small amount of a residual solvent, and to obtain even a case where the processing amount of the organic solvent solution of the polycarbonate varies. Changes in properties of polycarbonate powder are small. Therefore, the polycarbonate carbonate powder obtained by the method (1) can improve the volumetric efficiency of the processing equipment when performing post-processing such as drying, storage, granulation, and molding, and can also perform post-processing. In this respect, it is possible to improve the productivity of polycarbonate products because they can be applied stably.

Claims

1. Polycarbonate organic solvent solution and steam are introduced into the mixing nozzle, and the polycarbonate is recovered as a powder from the mixture injected from the mixing nozzle. In the production method, the organic solvent π medium is used as a solution, and the concentration of polycarbonate 靑

Wherein the ratio of the weight of the steam at the time of introduction to the weight of the organic solvent in the organic solvent solution is 1Ζ10〜1Ζ5. Method for producing high bulk density polycarbonate powder.

2. W _c / Wo 1/8: The method according to claim 1, wherein to L Zeta 6.

3. The method according to claim 1, wherein a solution of polycarbonate in methylene chloride is used as the organic solvent solution.

4. The method according to claim 1, wherein a polycarbonate organic solvent solution obtained in the process of producing polycarbonate by an interfacial polycondensation reaction is used as the organic solvent solution.

5. As steam, the pressure when introducing the mixing nozzle is 1 ~

The method according to claim 1, wherein a steam at 100 kg / cm ² and a temperature of 100 to 310 ° C. is used.

6. The mixture sprayed from the mixing nozzle is D is 5 mn! ~ 25cm, L length 50! !! ~ 1 000 m, ratio of pipe length L to inside diameter D (L / D) is 100 ~; 1 000 2. The method according to claim 1, wherein the powder is introduced into a gas-solid separator through a pipe of No. 0, and the polycarbonate powder is separated by the gas-solid separator.

7. A mixture of an organic solvent solution having a concentration of polycarbonate of 3 to 45% by weight and steam having a weight of 1 to 20 to 1 to 8 times the weight of the organic solvent in the organic solvent solution. Introduced to

The mixture sprayed from the mixing nozzle is mixed with a steam having a weight of lZSOOOlZl times the weight of the organic solvent in the organic solvent solution after a residence time of 1 to 1 second. To obtain a mixture of

Recovering the polycarbonate as a powder from this second mixture

Particularly, a method for producing a high bulk density polycarbonate powder.

8. The second mixture is obtained by introducing the mixture injected from the mixing nozzle into the second mixing nozzle through a pipe and introducing steam into the second mixing nozzle. The method described in.

9. The method according to claim 7, wherein a solution of polycarbonate in methylene chloride is used as the organic solvent solution.

10. The method according to claim 7, wherein as the organic solvent solution, a polycarbonate organic solvent solution obtained in the process of producing polycarbonate by an interfacial polycondensation reaction is used. .

1. The method according to claim 7, wherein a steam having a pressure of 1 to 100 kg / cm ² at the time of introducing the mixing table nozzle is used as the steam.

2. An organic solvent solution having a polycarbonate concentration of 3 to 45% by weight, steam and polycarbonate powder are introduced into a mixing nozzle, and the mixture injected from the mixing nozzle is used to polish the mixture. A method for producing high bulk density polycarbonate powder, comprising recovering the carbonate as powder.

1 3. When introducing the organic solvent solution, steam, and polycarbonate powder into the mixing nozzle, the steam and the polycarbonate powder are mixed and then introduced into the mixing nozzle. 12. The method described in 2.

14. The amount of steam introduced into the mixing nozzle is set to 1Z10 to 1/1 times the weight of the organic solvent in the organic solvent solution introduced into the mixing nozzle, and the polycarbonate powder to the mixing nozzle is used. 13. The method according to claim 12, wherein the amount of phenol introduced is 5 to 20% of the weight of the polycarbonate in the organic solvent solution introduced into the mixing nozzle.

1 5. The method according to claim 12, wherein a polycarbonate powder having a particle size of 8 mesh or less and 200 mesh or more is used as the polycarbonate powder introduced into the mixing nozzle. Method. 6. The method according to claim 12, wherein a solution of polycarbonate in methylene chloride is used as the organic solvent solution. 7. The method according to claim 12, wherein a polycarbonate organic solvent solution obtained in the process of producing polycarbonate by an interfacial polycondensation reaction is used as the organic solvent solution.

8. a steam-pressure during mixing nozzle introduced 1 1 0 0 kg Roh cm 0 temperature 1 ² 0-3 1 0. 13. The method according to claim 12, wherein the C stream is used.

9. The mixture ejected from the mixing nozzle has an inner diameter D of 5 mn! ~ 25 cm, tube length L force 50 cn! 100 m, the ratio of the pipe length L to the inner diameter D (LZD) force is introduced to the gas-solid separator through a pipe with a force of 100 to 100000, and the polycarbonate is 13. The method according to claim 12, wherein said powder is separated.

0. An organic solvent solution having a concentration of polycarbonate of 3 to 45% by weight and steam are introduced into a mixing nozzle, and the mixture injected from the mixing nozzle is directly injected from the mixing nozzle or connected to a pipe. Characterized in that the mixture discharged from the mixer is introduced into a gas-solid separator through a pipe, and the polyethylene-solid separator is recovered by the gas-solid separator. The method for producing polycarbonate powder.

1. Flow length from mixing nozzle to gas-solid separator (L) and flow length from mixing nozzle to mixer (^) 22. The method according to claim 20, wherein the mixer is arranged with a ratio (LZJ?) Of 5 or more.

22. The method according to claim 20, wherein a dynamic mixer is used as the mixer, a blade tip speed of 50 to 250 m / min.

23. The method according to claim 20, wherein a solution of polycarbonate in methylene chloride is used as the organic solvent solution.

24. The method according to claim 20, wherein an organic solvent solution of a poly-carbonate obtained in a process of producing a polycarbonate by an interfacial polycondensation reaction is used as the organic solvent solution.

2 5. As steam, the pressure when introducing the mixing nozzle is 1 to 100 kgZcm ² and the temperature is 100 to 310. 20. The method according to claim 20, wherein a C-form is used.

26. The method according to claim 20, wherein the amount of steam introduced into the mixing nozzle is 110 to 11 times the weight of the organic solvent in the organic solvent solution guided to the mixing nozzle. the method of.

2 7. The mixing nozzle and mixer, and the mixer and gas-solid separator, have an inner diameter D of 5 mn! ~ 25 cm, length L is 50 cn! 20. The method according to claim 20, wherein the pipes are connected by pipes having a length of (L / D) <100-: L0000, respectively.