JPH041767B2 - - Google Patents
Info
- Publication number
- JPH041767B2 JPH041767B2 JP59058324A JP5832484A JPH041767B2 JP H041767 B2 JPH041767 B2 JP H041767B2 JP 59058324 A JP59058324 A JP 59058324A JP 5832484 A JP5832484 A JP 5832484A JP H041767 B2 JPH041767 B2 JP H041767B2
- Authority
- JP
- Japan
- Prior art keywords
- polycarbonate
- hydroxyphenyl
- bis
- kneader
- methylene chloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 75
- 229920000515 polycarbonate Polymers 0.000 claims description 43
- 239000004417 polycarbonate Substances 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000008187 granular material Substances 0.000 claims description 17
- 238000009835 boiling Methods 0.000 claims description 8
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 5
- ODJUOZPKKHIEOZ-UHFFFAOYSA-N 4-[2-(4-hydroxy-3,5-dimethylphenyl)propan-2-yl]-2,6-dimethylphenol Chemical compound CC1=C(O)C(C)=CC(C(C)(C)C=2C=C(C)C(O)=C(C)C=2)=C1 ODJUOZPKKHIEOZ-UHFFFAOYSA-N 0.000 claims description 3
- HCNHNBLSNVSJTJ-UHFFFAOYSA-N 1,1-Bis(4-hydroxyphenyl)ethane Chemical group C=1C=C(O)C=CC=1C(C)C1=CC=C(O)C=C1 HCNHNBLSNVSJTJ-UHFFFAOYSA-N 0.000 claims description 2
- YMTYZTXUZLQUSF-UHFFFAOYSA-N 3,3'-Dimethylbisphenol A Chemical compound C1=C(O)C(C)=CC(C(C)(C)C=2C=C(C)C(O)=CC=2)=C1 YMTYZTXUZLQUSF-UHFFFAOYSA-N 0.000 claims description 2
- VOWWYDCFAISREI-UHFFFAOYSA-N Bisphenol AP Chemical compound C=1C=C(O)C=CC=1C(C=1C=CC(O)=CC=1)(C)C1=CC=CC=C1 VOWWYDCFAISREI-UHFFFAOYSA-N 0.000 claims description 2
- SDDLEVPIDBLVHC-UHFFFAOYSA-N Bisphenol Z Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)CCCCC1 SDDLEVPIDBLVHC-UHFFFAOYSA-N 0.000 claims 1
- 238000004807 desolvation Methods 0.000 claims 1
- 229920001519 homopolymer Polymers 0.000 claims 1
- 239000000243 solution Substances 0.000 description 32
- 238000000034 method Methods 0.000 description 20
- 239000002904 solvent Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 238000004898 kneading Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 150000002989 phenols Chemical class 0.000 description 4
- 125000004203 4-hydroxyphenyl group Chemical group [H]OC1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- GXDIDDARPBFKNG-UHFFFAOYSA-N 4,4'-(Butane-1,1-diyl)diphenol Chemical compound C=1C=C(O)C=CC=1C(CCC)C1=CC=C(O)C=C1 GXDIDDARPBFKNG-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 2
- -1 aliphatic alcohols Chemical class 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 description 1
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical class C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 1
- VWGKEVWFBOUAND-UHFFFAOYSA-N 4,4'-thiodiphenol Chemical compound C1=CC(O)=CC=C1SC1=CC=C(O)C=C1 VWGKEVWFBOUAND-UHFFFAOYSA-N 0.000 description 1
- NZGQHKSLKRFZFL-UHFFFAOYSA-N 4-(4-hydroxyphenoxy)phenol Chemical compound C1=CC(O)=CC=C1OC1=CC=C(O)C=C1 NZGQHKSLKRFZFL-UHFFFAOYSA-N 0.000 description 1
- RQCACQIALULDSK-UHFFFAOYSA-N 4-(4-hydroxyphenyl)sulfinylphenol Chemical compound C1=CC(O)=CC=C1S(=O)C1=CC=C(O)C=C1 RQCACQIALULDSK-UHFFFAOYSA-N 0.000 description 1
- AZZWZMUXHALBCQ-UHFFFAOYSA-N 4-[(4-hydroxy-3,5-dimethylphenyl)methyl]-2,6-dimethylphenol Chemical compound CC1=C(O)C(C)=CC(CC=2C=C(C)C(O)=C(C)C=2)=C1 AZZWZMUXHALBCQ-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000001175 rotational moulding Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明はポリカーボネート粒状体の製造方法に
関し、詳しくは塩化メチレン溶液の濃縮によつて
はゲル化しない単独重合型或は共重合型ポリカー
ボネートの塩化メチレン溶液から嵩密度の大き
い、粒子径の揃つたポリカーボネート粒状体を効
率よく製造する方法に係わる。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing polycarbonate granules, and more specifically, the present invention relates to a method for producing polycarbonate granules, and more specifically, a process for chlorinating homopolymerized or copolymerized polycarbonate that does not gel by concentrating a methylene chloride solution. The present invention relates to a method for efficiently producing polycarbonate granules having a high bulk density and uniform particle size from a methylene solution.
［従来技術］
ポリカーボネートを有機溶媒と水の存在下で製
造する方法は種々知られているが、いずれの方法
においても反応終了時にはポリカーボネートは有
機溶媒に溶けた溶液として得られる。ポリカーボ
ネートは押出成形、射出成形、回転成形等の成形
に用いるためにも、またキヤステイングフイルム
として用いるにも、その運搬、貯蔵面から粒状物
が好ましいので、上記溶液から固形物として回収
する必要がある。この回収法として多数の提案が
ある。[Prior Art] Various methods are known for producing polycarbonate in the presence of an organic solvent and water, but in any method, upon completion of the reaction, polycarbonate is obtained as a solution dissolved in an organic solvent. For polycarbonate to be used in extrusion molding, injection molding, rotary molding, etc., and also for use as a casting film, it is preferable to use granular materials from the viewpoint of transportation and storage, so it is necessary to recover the polycarbonate from the solution as a solid material. be. There are many proposals for this collection method.
それらの提案の第１の方法はポリカーボネート
の有機溶媒溶液にアルコール類やケトン類のよう
な非溶媒を混合して、ポリカーボネートを沈澱回
収する、所謂非溶剤沈澱法である（特公昭36−
22447、同36−22448、同37−7000、同38−16347
号公報参照）。 The first method proposed by them is the so-called non-solvent precipitation method, in which a non-solvent such as alcohol or ketone is mixed with an organic solvent solution of polycarbonate to collect the polycarbonate by precipitation.
22447, 36-22448, 37-7000, 38-16347
(see publication).
第２の方法はポリカーボネート溶液を熱水中或
いは水蒸気流中或いは熱風中に噴出させて固形ポ
リカーボネートを得る、所謂噴霧法である（特公
昭36−11231、同40−3533、同40−9843号公報参
照）。 The second method is the so-called spraying method in which solid polycarbonate is obtained by spraying a polycarbonate solution into hot water, steam flow, or hot air (Japanese Patent Publications Nos. 36-11231, 40-3533, and 40-9843). reference).
第３の方法はポリカーボネート溶液を濃縮し、
ゲル化させ粉砕する、所謂ゲル化法である（特公
昭36−21033、同44−11031、同45−9875号公報参
照）。 The third method is to concentrate the polycarbonate solution and
This is a so-called gelling method in which gelation and pulverization are performed (see Japanese Patent Publications No. 36-21033, No. 44-11031, and No. 45-9875).
これらの方法のうち、第１と第２の方法では得
られる固形物は嵩密度が低いため、取扱い上に難
点があり、さらに、第１の方法では２種以上の溶
媒を回収する不利がある。従つて、得られる固形
物の嵩密度が大きく、操作も簡単な第３のゲル化
法が優れている。しかしながら、本発明で対象と
するポリカーボネートはゲル化しないために第３
の方法では粒状体は得られない。 Among these methods, the solids obtained by the first and second methods have a low bulk density, making them difficult to handle, and the first method has the disadvantage of recovering two or more types of solvents. . Therefore, the third gelation method is superior because it provides a solid product with a high bulk density and is easy to operate. However, since the polycarbonate targeted by the present invention does not gel, it
Granules cannot be obtained using this method.
このようなゲル化しない共重合型ポリカーボネ
ートの粒状化方法として、ポリカーボネート溶液
に脂肪族炭化水素、脂肪族アルコール及び脂肪族
ケトンの中から選ばれた少くとも１種の沈澱剤を
加え、特定の剪断力のもとに混合する方法が特開
昭51−123265号公報に開示されている。しかし、
この方法も２種の溶媒を使用するために、各々の
溶剤を分離回収しなければならず工業上有利な方
法ではない。 As a method for granulating copolymerized polycarbonate that does not gel, at least one precipitant selected from aliphatic hydrocarbons, aliphatic alcohols, and aliphatic ketones is added to a polycarbonate solution, and a specific shear A method of mixing under force is disclosed in JP-A-51-123265. but,
Since this method also uses two types of solvents, each solvent must be separated and recovered, which is not an industrially advantageous method.
［発明の目的］
塩化メチレン溶液の濃縮によつてはゲル化しな
い単独重合型或は共重合型のポリカーボネートの
塩化メチレン溶液から、嵩密度の高い、粒度の揃
つた粒状体を、効率よく製造する方法を提供する
ことにある。[Objective of the invention] To efficiently produce granules with high bulk density and uniform particle size from a methylene chloride solution of a homopolymerized or copolymerized polycarbonate that does not gel by concentrating the methylene chloride solution. The purpose is to provide a method.
［発明の構成］
本発明は塩化メチレン溶液の濃縮によつてはゲ
ル化しないポリカーボネートの塩化メチレン溶液
を、塩化メチレンの沸点以上の温度に維持した熱
水を貯留した粉砕機構を有する混練機に供給し、
これを混練してポリカーボネートが黐（もち）状
になつた時点で粉砕機構が駆動できる程度にまで
熱水を除去し、続いて混練機内を塩化メチレンの
沸点以上の温度に維持して混練することにより脱
溶媒、粉砕を同時に行うことを特徴とするポリカ
ーボネート粒状体の製造方法である。[Structure of the Invention] The present invention supplies a methylene chloride solution of polycarbonate, which does not gel by concentrating the methylene chloride solution, to a kneader having a pulverizing mechanism that stores hot water maintained at a temperature equal to or higher than the boiling point of methylene chloride. death,
When this is kneaded and the polycarbonate becomes sticky, the hot water is removed to the extent that the crushing mechanism can be driven, and then the inside of the kneader is maintained at a temperature higher than the boiling point of methylene chloride and kneaded. This is a method for producing polycarbonate granules, characterized in that solvent removal and pulverization are performed simultaneously.
本発明で対象とするポリカーボネートは、一般
には酸受容体、水、有機溶媒および分子量調整剤
の存在下、２価フエノールとホスゲン等のカーボ
ネート前駆体との反応によつて製造される。ここ
で単独重合型ポリカーボネートの原料である２価
フエノールとしては、１，１−ビス（４−ヒドロ
キシフエニル）エタン、１，１−ビス（４−ヒド
ロキシフエニル）ブタン、１，１−ビス（４−ヒ
ドロキシフエニル）シクロヘキサン、２，２−ビ
ス（３−メチル−４−ヒドロキシフエニル）プロ
パン、２，２−ビス（３，５−ジメチル−４−ヒ
ドロキシフエニル）プロパン、１，１−ビス
（３，５−ジメチル−４−ヒドロキシフエニル）
メタン、１−フエニル−１，１−ビス（４−ヒド
ロキシフエニル）エタンなどが用いられる。ま
た、共重合型ポリカーボネートの原料である２価
フエノールとしては、上記の２価フエノール以外
にも２，２−ビス（４−ヒドロキシフエニル）プ
ロパン、ビス（４−ヒドロキシフエニル）スルフ
イツド、ビス（４−ヒドロキシフエニル）スルホ
ン、ビス（４−ヒドロキシフエニル）スルホキシ
ド、ビス（４−ヒドロキシフエニル）エーテル、
ビス（４−ヒドロキシフエニル）の如き化合物ま
たはビス（３，５−ジブロモ−４−ヒドロキシフ
エニル）プロパンの如きハロゲン化ビスフエノー
ル類が用いられる。 The polycarbonates of interest in the present invention are generally produced by reacting divalent phenols with carbonate precursors such as phosgene in the presence of an acid acceptor, water, an organic solvent, and a molecular weight modifier. Examples of divalent phenols that are raw materials for the homopolymerized polycarbonate include 1,1-bis(4-hydroxyphenyl)ethane, 1,1-bis(4-hydroxyphenyl)butane, and 1,1-bis(4-hydroxyphenyl)butane. 4-hydroxyphenyl)cyclohexane, 2,2-bis(3-methyl-4-hydroxyphenyl)propane, 2,2-bis(3,5-dimethyl-4-hydroxyphenyl)propane, 1,1- Bis(3,5-dimethyl-4-hydroxyphenyl)
Methane, 1-phenyl-1,1-bis(4-hydroxyphenyl)ethane, etc. are used. In addition to the divalent phenols mentioned above, examples of divalent phenols that are raw materials for copolymerized polycarbonate include 2,2-bis(4-hydroxyphenyl)propane, bis(4-hydroxyphenyl)sulfide, and bis(4-hydroxyphenyl)propane. 4-hydroxyphenyl) sulfone, bis(4-hydroxyphenyl) sulfoxide, bis(4-hydroxyphenyl) ether,
Compounds such as bis(4-hydroxyphenyl) or halogenated bisphenols such as bis(3,5-dibromo-4-hydroxyphenyl)propane are used.
本発明においてはかかる非晶性ポリカーボネー
トを塩化メチレン溶液として処理する。この溶液
の濃度は特に制限されるものではないが、好まし
い濃度としては３〜30重量％である。また、本発
明においては、かかるポリカーボネートの塩化メ
チレン溶液を熱水の入つた粉砕機構を有する混練
機中に供給し、脱溶媒を行なうので混練機中の熱
水の温度は塩化メチレンの沸点より高い温度、好
ましくは10〜30°程度高い温度とする。 In the present invention, such amorphous polycarbonate is treated as a methylene chloride solution. The concentration of this solution is not particularly limited, but the preferred concentration is 3 to 30% by weight. Furthermore, in the present invention, the methylene chloride solution of polycarbonate is fed into a kneader having a grinding mechanism containing hot water to remove the solvent, so that the temperature of the hot water in the kneader is higher than the boiling point of methylene chloride. The temperature is preferably about 10 to 30 degrees higher.
本発明に用いる粉砕機構を有する混練機の一例
を図面に示す。第１図は双腕形ニーダの簡略化し
た断面図であり、第２図はそのシグマ型翼の簡略
化した側面図である。このニーダは平行に設置し
たシグマ型翼１とこれを収納するジヤケツト付の
バレル２から成り、翼の回転により混練を行な
う。更に、このニーダには、第１図に示す如く、
バレルの長手方向に突条３を設けるとともにシグ
マ型翼１の周縁には鋸歯状突起４を設けてある。
鋸歯状突起４は第３図に示す如き形状であり、バ
レル２内面に形成した突条３の形状は第４図に示
す如き断面を有するものである。バレル２内面に
形成する凹凸としては第１図、第４図に示した突
条３に変えて、第５図に示す如く、多数の突起３
ａを突設せしめてもよい。このような粉砕用の突
条、突起としては、そのピツチが３〜20ｍ／ｍ程
度が良く、また翼とバレルのクリアランスは１〜
50ｍ／ｍが好ましい。 An example of a kneader having a crushing mechanism used in the present invention is shown in the drawings. FIG. 1 is a simplified cross-sectional view of a double-arm kneader, and FIG. 2 is a simplified side view of its sigma-type blade. This kneader consists of sigma type blades 1 installed in parallel and a barrel 2 with a jacket for housing the blades, and kneading is carried out by the rotation of the blades. Furthermore, as shown in Fig. 1, this kneader has
A protrusion 3 is provided in the longitudinal direction of the barrel, and a serrated protrusion 4 is provided on the periphery of the sigma-type blade 1.
The serrated projection 4 has a shape as shown in FIG. 3, and the shape of the protrusion 3 formed on the inner surface of the barrel 2 has a cross section as shown in FIG. As for the unevenness formed on the inner surface of the barrel 2, instead of the protrusions 3 shown in Figs. 1 and 4, there are many protrusions 3 as shown in Fig. 5.
A may be provided in a protruding manner. The pitch of such protrusions and protrusions for crushing should be about 3 to 20 m/m, and the clearance between the blade and the barrel should be about 1 to 20 m/m.
50m/m is preferred.
かかるニーダを用いる本発明について具体的に
説明する。 The present invention using such a kneader will be specifically explained.
まず、ニーダのバレル内に塩化メチレンの沸点
より高い温度の熱水を注入しこれをジヤケツトで
加熱し所定の温度に維持しつつポリカーボネート
の塩化メチレン溶液を少量ずつ投入しつつ撹拌す
る。これによりカーボネート溶液と熱水との接触
は十分に行なわれ、溶液の投入と同時に塩化メチ
レンの急速な沸騰蒸発が起こり、気泡や水滴を多
量に包含したペースト状ないし黐（もち）状物に
なる。ポリカーボネート溶液の投入および塩化メ
チレンの蒸発につれて、内容物は徐々に粘性を失
い、高い稠度の黐状物になる。この時点で粉砕機
構が駆動できる程度にまで熱水の大部分を排出
し、混練機内の温度を塩化メチレンの沸点以上に
維持しながら脱溶媒を続ける。この間にニーダの
翼とバレルの内面の間で黐状物は切断作用などに
よつて粉砕されて粒度の揃つた粒状体になる。 First, hot water with a temperature higher than the boiling point of methylene chloride is injected into the barrel of a kneader, heated with a jacket, and maintained at a predetermined temperature, while a solution of polycarbonate in methylene chloride is added little by little and stirred. This ensures sufficient contact between the carbonate solution and the hot water, causing rapid boiling and evaporation of methylene chloride as soon as the solution is added, resulting in a paste-like or sticky substance containing a large amount of bubbles and water droplets. . As the polycarbonate solution is added and the methylene chloride evaporates, the contents gradually lose viscosity and become a thick consistency. At this point, most of the hot water is discharged to the extent that the crushing mechanism can be driven, and solvent removal is continued while maintaining the temperature inside the kneading machine above the boiling point of methylene chloride. During this time, between the blades of the kneader and the inner surface of the barrel, the slag is pulverized by a cutting action or the like to form granules with uniform particle size.
［実施例］
以下に実施例を掲げて本発明を更に具体的に説
明する。[Example] The present invention will be described in more detail with reference to Examples below.
実施例 １
第３図における歯の高さh1が10ｍ／ｍ、歯と歯
の間隔p1が20ｍ／ｍ、歯先のR1が５ｍ／ｍの鋸
歯状歯を設けたシグマ型翼とバレル内側に第４図
の高さh2が20ｍ／ｍ、間隔p2が20ｍ／ｍ、R2が
５ｍ／ｍの歯を設けたバレルをクリアランス３
ｍ／ｍに取付けた翼長1500ｍ／ｍ、翼径600ｍ／
ｍのジヤケツト付双腕形ニーダに熱水を入れた。
この中に、１，１−ビス（４−ヒドロキシフエニ
ル）エタンとホスゲンの反応から得たηsp0.43（0.7
ｇ／100ml塩化メチレン、20℃）のポリカーボネ
ートの10重量％塩化メチレン溶液を徐々に滴下し
た。ニーダは60r.p.m.で撹拌しながら、溶液を滴
下し、もち状物を得た。この間ジヤケツトから加
熱し、水温を約50℃に保つた。溶液を滴下し終え
ると、熱水を排出し、ニーダ内部の雰囲気温度を
約50℃に維持しながらかき混ぜ、脱溶媒と粉砕を
行なつた。Example 1 A sigma-type blade with serrated teeth in which the tooth height h 1 in Fig. 3 is 10 m/m, the tooth spacing p 1 is 20 m/m, and the tooth tip R 1 is 5 m/m. A barrel with teeth with a height h 2 of 20 m/m, a spacing p 2 of 20 m/m, and an R 2 of 5 m/m as shown in Figure 4 on the inside of the barrel has a clearance of 3.
Blade length 1500m/m installed on m/m, blade diameter 600m/
Hot water was poured into a double-arm kneader with a jacket.
Among these, η sp 0.43 (0.7
A 10% by weight solution of polycarbonate in methylene chloride (g/100ml methylene chloride, 20°C) was slowly added dropwise. While stirring the kneader at 60 rpm, the solution was added dropwise to obtain a glutinous material. During this time, the jacket was heated to maintain the water temperature at approximately 50°C. After dropping the solution, the hot water was discharged, and the mixture was stirred while maintaining the atmospheric temperature inside the kneader at approximately 50°C to remove the solvent and crush the mixture.
得られたポリカーボネート粒状体の粒径は１〜
５ｍ／ｍであり、120℃で12時間乾燥後に測定し
た嵩密度は0.33ｇ／cm3であつた。 The particle size of the obtained polycarbonate granules is 1-
The bulk density measured after drying at 120° C. for 12 hours was 0.33 g/cm 3 .
実施例 ２
実施例１と同じシグマ型翼とバレル内側に第５
図の高さh3が20ｍ／ｍ、間隔p3が20ｍ／ｍ、R3
が５ｍ／ｍの歯を設けたバレルをクリアランス３
ｍ／ｍで取付けた実施例１と同様のジヤケツト付
双腕形ニーダに50℃の熱水を入れた。この中に、
１，１−ビス（４−ヒドロキシフエニル）シクロ
ヘキサンとホスゲンの反応により得たηsp（0.7
ｇ／100ml）塩化メチレン溶液にて20℃で測定）
が0.41のポリカーボネートの10重量％塩化メチレ
ン溶液を徐々に滴下した。ニーダは60r.p.m.で撹
拌しながら、溶液を滴下し、もち状物を得た。こ
の間ジヤケツトから加熱し、水温を約50℃に保つ
た。溶液を滴下し終えると、熱水を排水し、ニー
ダ内部の雰囲気温度を約50℃に維持しながらかき
混ぜ、脱溶媒と粉砕を行なつた。Example 2 The same sigma-type blade as in Example 1 and a fifth blade inside the barrel.
The height of the figure h 3 is 20 m/m, the spacing p 3 is 20 m/m, R 3
The barrel with teeth of 5m/m has a clearance of 3
Hot water at 50° C. was poured into a double-arm kneader with a jacket similar to that in Example 1, which was installed at m/m. In this,
η sp (0.7
g/100ml) Measured at 20℃ in methylene chloride solution)
A 10% by weight methylene chloride solution of polycarbonate having a polycarbonate of 0.41 was gradually added dropwise. While stirring the kneader at 60 rpm, the solution was added dropwise to obtain a glutinous material. During this time, the jacket was heated to maintain the water temperature at approximately 50°C. After dropping the solution, the hot water was drained, and the mixture was stirred while maintaining the atmospheric temperature inside the kneader at approximately 50°C to remove the solvent and crush the mixture.
得られたポリカーボネート粒状体の粒径は0.5
〜３ｍ／ｍであり、120℃で12時間乾燥後に測定
した嵩密度は0.36ｇ／cm3であつた。 The particle size of the obtained polycarbonate granules is 0.5
~3 m/m, and the bulk density measured after drying at 120° C. for 12 hours was 0.36 g/cm 3 .
実施例 ３
60℃の熱水の入つた実施例２に用いたと同じニ
ーダ中に、２，２−ビス（４−ヒドロキシフエニ
ル）プロパン50重量％と、２，２−ビス（３，５
−ジメチル−４−ヒドロキシフエニル）プロパン
50重量％からなる２価フエノールとホスゲンとの
反応より得たηsp（0.7ｇ／100ml塩化メチレン溶液
にて20℃で測定）が0.47の共重合型ポリカーボネ
ートの10重量％塩化メチレン溶液を徐々に滴下し
た。ニーダは60r.p.m.で撹拌しながら、溶液を滴
下し、もち状物を得た。この間ジヤケツトから加
熱し、水温を約50℃に保つた。溶液を滴下し終え
ると、熱水を排出し、ニーダ、内部の雰囲気温度
を約50℃に維持しながらかきまぜ脱溶媒と粉砕と
行なつた。Example 3 In the same kneader used in Example 2 containing hot water at 60°C, 50% by weight of 2,2-bis(4-hydroxyphenyl)propane and 2,2-bis(3,5
-dimethyl-4-hydroxyphenyl)propane
A 10% by weight methylene chloride solution of a copolymerized polycarbonate with an η sp (measured at 20°C in a 0.7 g/100 ml methylene chloride solution) of 0.47 obtained by the reaction of 50% by weight divalent phenol with phosgene was gradually added. dripped. While stirring the kneader at 60 rpm, the solution was added dropwise to obtain a glutinous material. During this time, the jacket was heated to maintain the water temperature at approximately 50°C. After dropping the solution, the hot water was discharged, and the kneader was stirred to remove the solvent and pulverize while maintaining the ambient temperature inside the kneader at about 50°C.
得られた共重合型ポリカーボネート粒状体の粒
径は0.7〜５ｍ／ｍであり、120℃で12時間乾燥後
に測定した嵩密度は0.34ｇ／cm3であつた。 The particle size of the resulting copolymerized polycarbonate particles was 0.7 to 5 m/m, and the bulk density measured after drying at 120°C for 12 hours was 0.34 g/cm 3 .
比較例 １
翼にも、バレルにも歯のない以外は実施例１に
用いたと同様のジヤケツト付双腕形ニーダに50℃
の熱水を入れた。この中に実施例１に用いたと同
じポリカーボネート溶液を滴下し、もち状物を得
た。熱水排出後、雰囲気温度を約50℃に保ちなが
ら、撹拌を続けたところ、もち状物が大きな固い
塊となつて負荷が大きくなり撹拌不能となつた。Comparative Example 1 A double-arm kneader with a jacket similar to that used in Example 1 except that there were no teeth on either the blades or the barrel was heated at 50°C.
of hot water was added. The same polycarbonate solution used in Example 1 was dropped into this to obtain a glutinous material. After the hot water was discharged, stirring was continued while maintaining the ambient temperature at approximately 50°C, but the sticky material turned into a large solid lump and the load increased, making stirring impossible.
［発明の効果］
本発明の製造法で得られた非晶性ポリカーボネ
ート粒状体は粒度の揃つた嵩密度の高い粒状体で
あるので、そのままで押出成形、回転成形等の成
形に好適に用いられるし、輸送する際は嵩低く梱
包できる。また、粒状体は多孔質なので、溶媒に
溶け易くキヤステイングフイルム用に適してい
る。しかも、整備的には翼やバレルに溝又は突起
状の歯のついた粉砕機構を有する混練機一つで、
溶液から粒状体が得られ、その動力も粉砕機構を
有しない混練機にて助溶剤して得られる固い塊状
物を粉砕するような強力なものは不要であつて、
工業上極めて有利である。[Effects of the Invention] Since the amorphous polycarbonate granules obtained by the production method of the present invention are granules with uniform particle size and high bulk density, they can be suitably used as they are in extrusion molding, rotational molding, etc. However, when transporting it, it can be packed in a low-volume manner. Furthermore, since the granules are porous, they are easily soluble in solvents and are suitable for use in casting films. Moreover, in terms of maintenance, it is a single kneading machine that has a crushing mechanism with grooves or protruding teeth on the blades and barrel.
Granules are obtained from the solution, and there is no need for a powerful kneader that does not have a crushing mechanism to crush the hard lumps obtained by using a co-solvent.
It is extremely advantageous industrially.
第１図は本発明に用いる混練機の一例の簡略化
した断面図、第２図はその撹拌翼の簡略化した側
面図、第３図は撹拌翼に形成した鋸歯状歯の部分
側面図、第４図はバレルに形成した突条の部分側
面図、第５図はバレルに形成する突起の部分側面
図。
１は撹拌翼、２はバレル、３は撹拌翼周縁に形
成した鋸歯状歯、４はバレルに形成した突条。
FIG. 1 is a simplified sectional view of an example of a kneading machine used in the present invention, FIG. 2 is a simplified side view of its stirring blade, and FIG. 3 is a partial side view of serrated teeth formed on the stirring blade. FIG. 4 is a partial side view of a protrusion formed on the barrel, and FIG. 5 is a partial side view of a protrusion formed on the barrel. 1 is a stirring blade, 2 is a barrel, 3 is a serrated tooth formed on the periphery of the stirring blade, and 4 is a protrusion formed on the barrel.
Claims (1)
ないポリカーボネートの塩化メチレン溶液を、塩
化メチレンの沸点以上の温度に維持した熱水を貯
留した粉砕機構を有する混練機に供給し、これを
混練してポリカーボネートが黐（もち）状になつ
た時点で粉砕機構が駆動できる程度にまで熱水を
除去し、続いて混練機内を塩化メチレンの沸点以
上の温度に維持して混練することにより脱溶媒、
粉砕を同時に行うことを特徴とするポリカーボネ
ート粒状体の製造方法。 ２ 前記混練機として翼および／またはバレルに
溝又は突起状の歯を設けたニーダを用いる特許請
求の範囲第１項記載のポリカーボネート粒状体の
製造方法。 ３ 前記ポリカーボネートが１，１−ビス（４−
ヒドロキシフエニル）エタン、１，１−ビス（４
−ヒドロキシフエニル）シクロヘキサン、２，２
−ビス（３−メチル−４−ヒドロキシフエニル）
プロパン、２，２−ビス（３，５−ジメチル−４
−ヒドロキシフエニル）プロパン、１−フエニル
−１，１−ビス（４−ヒドロキシフエニル）エタ
ンの単独重合体或いは２，２−ビス（４−ヒドロ
キシフエニル）プロパンとの共重合型ポリカーボ
ネートである特許請求の範囲第１項若しくは第２
項記載のポリカーボネート粒状体の製造方法。[Claims] 1. A methylene chloride solution of polycarbonate that does not gel by concentrating the methylene chloride solution is supplied to a kneader having a pulverizing mechanism that stores hot water maintained at a temperature higher than the boiling point of methylene chloride. When this is kneaded and the polycarbonate becomes sticky, the hot water is removed to the extent that the crushing mechanism can be driven, and then the inside of the kneader is maintained at a temperature above the boiling point of methylene chloride and kneaded. By desolvation,
A method for producing polycarbonate granules, characterized by simultaneously performing pulverization. 2. The method for producing polycarbonate granules according to claim 1, wherein the kneader is a kneader having grooves or protruding teeth on its blades and/or barrel. 3 The polycarbonate is 1,1-bis(4-
hydroxyphenyl)ethane, 1,1-bis(4
-hydroxyphenyl)cyclohexane, 2,2
-bis(3-methyl-4-hydroxyphenyl)
Propane, 2,2-bis(3,5-dimethyl-4
- Hydroxyphenyl)propane, a homopolymer of 1-phenyl-1,1-bis(4-hydroxyphenyl)ethane, or a copolymerized polycarbonate with 2,2-bis(4-hydroxyphenyl)propane. Claim 1 or 2
A method for producing polycarbonate granules as described in Section 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5832484A JPS60202126A (en) | 1984-03-28 | 1984-03-28 | Production of polycarbonate particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5832484A JPS60202126A (en) | 1984-03-28 | 1984-03-28 | Production of polycarbonate particle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60202126A JPS60202126A (en) | 1985-10-12 |
| JPH041767B2 true JPH041767B2 (en) | 1992-01-14 |
Family
ID=13081103
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5832484A Granted JPS60202126A (en) | 1984-03-28 | 1984-03-28 | Production of polycarbonate particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60202126A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010053169A (en) * | 2008-08-26 | 2010-03-11 | Teijin Chem Ltd | Method for continuously producing polycarbonate granular material |
| JP2011026471A (en) * | 2009-07-27 | 2011-02-10 | Teijin Chem Ltd | Continuous production method for polycarbonate granules |
| JP2012025860A (en) * | 2010-07-23 | 2012-02-09 | Teijin Chem Ltd | Method for continuously producing polycarbonate granule |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR960000571B1 (en) * | 1991-01-24 | 1996-01-09 | 미쓰이 도오아쓰 가가쿠 가부시키가이샤 | Process for producing granules of polycarbonate and composition thereof |
| KR100316986B1 (en) * | 1993-09-21 | 2002-02-28 | 카지와라 마사쯔구 | Aromatic Polycarbonate Resin Powder and Manufacturing Method Thereof |
| US5760160A (en) * | 1993-09-21 | 1998-06-02 | Teijin Chemicals Ltd. | Aromatic polycarbonate resin granule |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59133228A (en) * | 1983-01-20 | 1984-07-31 | Mitsubishi Chem Ind Ltd | Production of polycarbonate resin particle |
-
1984
- 1984-03-28 JP JP5832484A patent/JPS60202126A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59133228A (en) * | 1983-01-20 | 1984-07-31 | Mitsubishi Chem Ind Ltd | Production of polycarbonate resin particle |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010053169A (en) * | 2008-08-26 | 2010-03-11 | Teijin Chem Ltd | Method for continuously producing polycarbonate granular material |
| JP2011026471A (en) * | 2009-07-27 | 2011-02-10 | Teijin Chem Ltd | Continuous production method for polycarbonate granules |
| JP2012025860A (en) * | 2010-07-23 | 2012-02-09 | Teijin Chem Ltd | Method for continuously producing polycarbonate granule |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60202126A (en) | 1985-10-12 |
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