JPS6335621A - Production of polycarbonate resin powder - Google Patents
Production of polycarbonate resin powderInfo
- Publication number
- JPS6335621A JPS6335621A JP17877586A JP17877586A JPS6335621A JP S6335621 A JPS6335621 A JP S6335621A JP 17877586 A JP17877586 A JP 17877586A JP 17877586 A JP17877586 A JP 17877586A JP S6335621 A JPS6335621 A JP S6335621A
- Authority
- JP
- Japan
- Prior art keywords
- polycarbonate resin
- amount
- resin powder
- methylene chloride
- powder
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 48
- 229920005668 polycarbonate resin Polymers 0.000 title claims abstract description 45
- 239000004431 polycarbonate resin Substances 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000013557 residual solvent Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000748 compression moulding Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 238000005507 spraying Methods 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims abstract 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 abstract description 3
- 239000004417 polycarbonate Substances 0.000 abstract description 3
- 238000010528 free radical solution polymerization reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000008187 granular material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 238000005453 pelletization Methods 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000006136 alcoholysis reaction Methods 0.000 description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 1
- 238000012696 Interfacial polycondensation Methods 0.000 description 1
- 238000012695 Interfacial polymerization Methods 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 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 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002362 mulch Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、ポリカーボネート樹脂粉状体の製造法に係わ
り、公知の溶液法によって得られるポリカーボネート樹
脂粉粒状体から塩化メチレンその他の溶媒の残存量が少
なく、かつ、微粉が少なく、高い嵩密度を有するポリカ
ーボネート樹脂粉状体の製造法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing polycarbonate resin powder, and the present invention relates to a method for producing polycarbonate resin powder, and the remaining amount of methylene chloride and other solvents from polycarbonate resin powder and granules obtained by a known solution method. The present invention relates to a method for producing a polycarbonate resin powder having a high bulk density and a small amount of fine powder.
ビスフェノール頚とホスゲンとの反応により得られるポ
リカーボネート樹脂の一般的な製法は、塩化メチレンと
アルカリ水系との界面重縮合反応による方法である。そ
のため、重縮合反応並びに精製終了後、樹脂は塩化メチ
レン溶液として取り出される。そして溶液のままでは輸
送等の取り扱いにも不都合であり、更には、安定剤、染
顔料、充填剤等各種の添加剤を混合する操作の便利さの
ため、通常、この溶液からポリカーボネート樹脂を粉状
体として単離する。この粉体に安定剤、染顔料、充填剤
等各種の添加剤を混合し、最終的には溶融押出しによる
ペレット状体とし、このペレットが射出成形その他の用
に供せられる。A general method for producing polycarbonate resin obtained by the reaction of bisphenol neck and phosgene is an interfacial polycondensation reaction between methylene chloride and an aqueous alkaline system. Therefore, after the polycondensation reaction and purification are completed, the resin is taken out as a methylene chloride solution. It is inconvenient to transport and handle the polycarbonate resin as a solution.Furthermore, for the convenience of mixing various additives such as stabilizers, dyes and pigments, and fillers, polycarbonate resin is usually powdered from this solution. It is isolated as a solid. This powder is mixed with various additives such as stabilizers, dyes and pigments, and fillers, and finally formed into pellets by melt extrusion, and these pellets are used for injection molding and other purposes.
ポリカーボネート樹脂の塩化メチレン溶液から樹脂を単
離する方法としては、既に多くの方法が提案されている
が、例えば、特公昭４６−３７４２４号公報に開示され
ている塩化メチレン溶液自体を濃縮し、最終的に塩化メ
チレンを数千〜数百ｐｐｍ含有する粉状体とする方法と
、例えば、特公昭５３−１３７２９７号公報に開示され
る塩化メチレン溶液にポリカーボネート樹脂の非溶媒を
添加し、これを濃縮し、最終的に非溶媒を数千ｐｐｍ含
有する粉状体とする方法とによって代表される。Many methods have already been proposed for isolating a polycarbonate resin from a methylene chloride solution. For example, the method disclosed in Japanese Patent Publication No. 53-137297 involves adding a non-solvent of polycarbonate resin to a methylene chloride solution and concentrating it. This is typified by the method of finally producing a powder containing several thousand ppm of non-solvent.
前者の方法によって塩化メチレン溶液自体から得た粉状
体には、乾煙後においても、前述の通り、数千〜数百ｐ
ｐｍの塩化メチレンが残存するため、これを溶融押出し
した場合には、塩化メチレンの熱分解により樹脂が著し
く着色する。一方、貧溶媒を用いる後者の方法では、非
溶媒の種類により、その影山が異なるが、例えば、アル
コール類を用いた場合には、残存アルコールによる熱時
のアルコリシスによって樹脂の分解が起こり、好ましく
ない。そのため、一般には脂肪族炭化水素類もしくは芳
香族炭化水素類等の不活性溶媒が多く用いられている。As mentioned above, the powder obtained from the methylene chloride solution itself by the former method contains several thousand to several hundred parts even after drying.
Since methylene chloride of pm remains, when this is melt-extruded, the resin is significantly colored due to thermal decomposition of the methylene chloride. On the other hand, in the latter method using a poor solvent, the effects differ depending on the type of non-solvent, but for example, when alcohols are used, the resin decomposes due to alcoholysis due to residual alcohol when heated, which is undesirable. . Therefore, inert solvents such as aliphatic hydrocarbons or aromatic hydrocarbons are generally used.
しかし、これらの溶媒は、溶融押出時にも樹脂から完全
には離脱せず、最終成形品にまで残存し、実使用下での
応力亀裂の発生による著しい強度低下の原因となる。However, these solvents do not completely separate from the resin during melt extrusion and remain in the final molded product, causing stress cracks to occur during actual use and resulting in a significant decrease in strength.
以上のように、ポリカーボネート樹脂粉状体中の残存溶
媒は極力少なくすることが、耐熱性ならびに耐久性に優
れたポリカーボネート樹脂成形品を製造するための必要
条件である。As described above, minimizing the amount of residual solvent in the polycarbonate resin powder is a necessary condition for producing polycarbonate resin molded products with excellent heat resistance and durability.
さて、少量の有機溶媒を包含する粉状体より有機溶媒を
除去するために、その粉状体をさらに微粉化し、乾愚す
る試みは、当業者が当然に想起するところであるが、微
粉とするために要する装置、動力を考えた場合、この方
法は必ずしも経済的に有利な方法ではない。また、係る
微粉体は、乾繰、種々の添加剤その他との混合などの作
業において、粉塵の飛故による環境悪化等の取り扱い上
の問題、およびスクリュー押出機によるペレット化の際
にスクリューへの食い込み不良によりサージングを生じ
たりして生産量が低下するという問題の原因となる。な
お、嵩密度の高いポリカーボネート樹脂粉状体とするこ
とは、粉末計量、輸送及び貯蔵等の粉状体取り扱い上、
極めて重要なことである。Now, in order to remove the organic solvent from a powder containing a small amount of organic solvent, attempts have been made to further pulverize the powder and dry it, as those skilled in the art will naturally recall. Considering the equipment and power required for this, this method is not necessarily economically advantageous. In addition, such fine powders pose handling problems such as environmental deterioration due to flying dust during operations such as drying and mixing with various additives, etc., and when pelletizing using a screw extruder. This causes problems such as surging due to poor biting and a decrease in production. In addition, the use of polycarbonate resin powder with a high bulk density makes handling of the powder such as powder measurement, transportation, and storage difficult.
This is extremely important.
本発明者らは、上記粉状体の微粉化による不都合を避け
、乾燥後に粒度分布の整った嵩密度の高いポリカーボネ
ート樹脂粉状体を得る方法について鋭意検討した結果、
極めて簡単に、しかも、２０〜４０メツシュが粒度分布
の主体となり、微粉体を含まず、嵩密度が０．５〜０．
７ｇ／ｃＪであるポリカーボネート樹脂粉状体を得るこ
とに成功し、本発明を完成させた。The present inventors have conducted intensive studies on a method for obtaining a polycarbonate resin powder with a uniform particle size distribution and high bulk density after drying, avoiding the inconvenience caused by the pulverization of the powder.
Very easily, the particle size distribution mainly consists of 20 to 40 mesh, does not contain fine powder, and has a bulk density of 0.5 to 0.
We succeeded in obtaining polycarbonate resin powder having a weight of 7 g/cJ, and completed the present invention.
すなわち、本発明は、その全量の９０％以上が１６メツ
シュの篩を通過せず、乾燥後の残存塩化メチレンの量が
１１００ｐｐ以下であり、かつ、その他の残存溶媒の量
が５００ｐｐｍ以下であるポリカーボネート樹脂粉粒状
体を乾式圧縮成形し、次いで、得られた成形物を破砕す
ることからなる残存溶媒量が少なく、かつ、嵩密度が高
いポリカーボネート樹脂粉状体の製造法である。That is, the present invention provides polycarbonate in which 90% or more of the total amount does not pass through a 16-mesh sieve, the amount of residual methylene chloride after drying is 1100 ppm or less, and the amount of other residual solvents is 500 ppm or less. This is a method for producing a polycarbonate resin powder with a small amount of residual solvent and a high bulk density, which comprises dry compression molding a resin powder granule and then crushing the resulting molded product.
以下、本発明の構成について説明する。The configuration of the present invention will be explained below.
まず、本発明のその全量の９０％以上が１６メツシュの
篩を通過せず、乾爆後の残存塩化メチレンの量が１１０
０ｐｐ以下であり、かつ、その他の残存溶媒の量が５０
０ｐｐｍ以下であるポリカーボネート樹脂粉粒状体とは
、界面重合法により得られたポリカーボネート樹脂の塩
化メチレン溶液にポリカーボネ−１・樹脂の非溶媒、例
えば、ｎ−ヘプタン、ｎ−ヘキサン、シクロヘキサン、
ベンゼン、クロルベンゼン、トルエンなどを沈澱物が生
成しない程度の量だけ添加混合し、この混合液を約４５
〜１００℃に保持した温熱水中に滴下もしくは噴霧して
、塩化メチレンおよび添加非溶媒を蒸発せしめポリカー
ボネート樹脂固体状物を得、その後、その全量の９０％
以上が１６メツシュの篩を通過しない粒度になるように
湿式粉砕もしくは乾燥粉砕してなるものである。First, more than 90% of the total amount of the present invention does not pass through a 16-mesh sieve, and the amount of methylene chloride remaining after dry explosion is 110%.
0 pp or less, and the amount of other residual solvent is 50
A polycarbonate resin powder having a concentration of 0 ppm or less is a methylene chloride solution of a polycarbonate resin obtained by an interfacial polymerization method, and a polycarbonate resin non-solvent such as n-heptane, n-hexane, cyclohexane,
Benzene, chlorobenzene, toluene, etc. are added and mixed in an amount that does not form a precipitate.
Methylene chloride and the added non-solvent are evaporated by dropping or spraying into hot water maintained at ~100°C to obtain a polycarbonate resin solid, and then 90% of the total amount
The above particles are wet-pulverized or dry-pulverized to a particle size that does not pass through a 16-mesh sieve.
ここに、ポリカーボネート樹脂の塩化メチレン溶液に添
加する非溶媒の添加量が、少なすぎると緻密な粉粒状体
となり乾燥が困難となり、多すぎると溶媒蒸発時に微粉
化してしまいその後の取り扱いが、例えば、水との分離
の際、槙布の目を通過するとか、目づまりするとか、總
過分離機では微粉が水側に排出されるなどの不都合があ
り、極めて困難となる。Here, if the amount of non-solvent added to the methylene chloride solution of polycarbonate resin is too small, it will become a dense granular material that will be difficult to dry, and if it is too large, it will become fine powder when the solvent evaporates, making subsequent handling difficult, for example. Separation from water is extremely difficult due to inconveniences such as passing through the mesh of the mulch cloth, clogging, and fine powder being discharged to the water side in a filtration separator.
非溶媒のうちで、アルコール系、エーテル系等は、上記
で説明した如く、加熱時アルコリシス等による樹脂の分
解が起こり易いので不適当であり、好ましいものは、前
記に例示した脂肪族炭化水素や芳香族炭化水素類である
。Among non-solvents, alcohol-based, ether-based, etc. are unsuitable as they tend to cause decomposition of the resin due to alcoholysis when heated, as explained above, and preferred ones are aliphatic hydrocarbons and ethers as exemplified above. They are aromatic hydrocarbons.
非溶媒の添加量は、ポリカーボネート樹脂のＳＰ値と非
溶媒のＳＰ値との差、およびポリカーボネート樹脂溶液
の濃度により適宜選択されるものであり、上記に例示し
た非溶媒のなかで、例えば、ポリカーボネート樹脂溶液
の濃度が１５〜２５重量％の場合、ＳＰ値の差が約２．
３である叶へブタンでは樹脂液の好ましくは、０．１５
〜０．５８蚤倍であり、ＳＰ値の差が約１．５５である
シクロヘキサンでは樹脂液の０．３〜０．６容量倍、Ｓ
Ｐ値の差が約０．９であるトルエンでは樹脂液の０．５
〜０．８容量倍の範囲より適宜選択されるが、非溶媒の
使用量およびポリカーボネート樹脂粉粒状体の安定した
生成からは、ｎ−ヘプタンが最も好ましい。The amount of the nonsolvent added is appropriately selected depending on the difference between the SP value of the polycarbonate resin and the SP value of the nonsolvent, and the concentration of the polycarbonate resin solution. Among the nonsolvents listed above, for example, polycarbonate When the concentration of the resin solution is 15 to 25% by weight, the difference in SP value is about 2.
3, the resin liquid is preferably 0.15
In cyclohexane, the difference in SP value is about 1.55, it is 0.3 to 0.6 times the volume of the resin liquid, S
In toluene, where the difference in P value is approximately 0.9, the difference in P value is 0.5 of the resin liquid.
Although it is appropriately selected from the range of 0.8 to 0.8 times the volume, n-heptane is most preferred in terms of the amount of nonsolvent used and stable production of polycarbonate resin powder.
上記で調製した混合液を４５〜１００℃の水中に滴下も
しくは噴霧し、溶媒および非溶媒を蒸発線速度が好まし
くは２０ ｃ＋ｎ／ｓｅｃ以下となるように蒸発させて
ポリカーボネート樹脂粉粒状体とし、そのままもしくは
水を分離した後、粉砕する。蒸発線速度が、２０ ｃｍ
／ｓｅｃより高くなる条件で滴下もしくは噴霧した場合
には、気液界面での泡立ち現象が激しくなり、蒸発溶媒
への樹脂の同伴や気液界面でブロック状の樹脂塊が生じ
たりしがちであり好ましくない。The liquid mixture prepared above is dropped or sprayed into water at 45 to 100°C, and the solvent and nonsolvent are evaporated so that the linear evaporation velocity is preferably 20 c+n/sec or less to obtain polycarbonate resin powder and granules, and then Or, after separating the water, crush it. Evaporation linear velocity is 20 cm
If dripping or spraying is carried out at a temperature higher than /sec, the bubbling phenomenon at the gas-liquid interface becomes more intense, and the resin tends to be entrained in the evaporated solvent and block-shaped resin lumps occur at the gas-liquid interface. Undesirable.
以上の方法により通常５ｍｍ〜１０ｍｍ程度の粒子径で
、乾燥後の嵩密度が０．２５〜０．４５程度のポリカー
ボネート樹脂の固体状物が得られる。By the above method, a solid polycarbonate resin having a particle size of about 5 mm to 10 mm and a bulk density of about 0.25 to 0.45 after drying can be obtained.
この固体状物はそのままでは乾燥速度が不充分であるの
で、水懸濁液のままもしくは埴過後、粉砕し乾燥する。Since the drying rate of this solid substance is insufficient as it is, it is pulverized and dried either as an aqueous suspension or after passing through clay.
粉砕は、上記の如く、その全量の９０％以上が１６メツ
シュの篩を通過しない粒度になるよう行い、ついで、こ
の粉粒状体を通常、温度１２０〜１５０℃で１．０〜１
０．０時間乾燥し、乾燥後の残存塩化メチレンの量が１
１００ｐｐ以下であり、かつ、その他の残存溶媒の量が
５００ｐｐｍ以下であるポリカーボネート樹脂粉粒状体
とする。ここに、粉体の粒子径が小さい程、乾燥は容易
となり、かつ、乾燥温度も高い程乾繰時間が短くてよい
と考えられるが、粉体の高温による固結や乾煙時の劣化
などの点から、粒度、嵩密度および乾燥温度が上記のご
とくに選択されるものである。As mentioned above, pulverization is performed so that 90% or more of the total amount does not pass through a 16-mesh sieve, and then this powder is usually sieved at a temperature of 1.0 to 1.
After drying for 0.0 hours, the amount of residual methylene chloride after drying is 1
The polycarbonate resin powder has a content of 100 ppm or less and an amount of other residual solvents of 500 ppm or less. Here, it is thought that the smaller the particle size of the powder, the easier it is to dry, and the higher the drying temperature, the shorter the drying time. from which the particle size, bulk density and drying temperature are selected as described above.
以上の方法で調製したポリカーボネート樹脂粉粒状体は
、そのままでは嵩密度が低く、貯蔵、運搬の際、さらに
は溶融ペレット化時の生産能力が低下するなどの不都合
かあるので、乾式圧縮成形し粉砕することにより、嵩密
度のより高い粉状体とする。The polycarbonate resin powder prepared by the above method has a low bulk density as it is, which causes disadvantages such as a decrease in production capacity during storage and transportation, and even during melt pelletization, so it is dry compression molded and pulverized. By doing so, a powder having a higher bulk density is obtained.
圧縮成形は、室温〜１７０℃程度の範囲で、圧力５ｋｇ
／ ｃｉ以上で適宜選択することにより、粉砕可能な
高嵩密度の板状体とすることによる。例えば、室温で圧
縮圧力１２００ ｋｇ／ｃｎｆと１７０℃で５ｋｇ／ｃ
ｌの条件で得た板状体を、粉状体の粒度分布の主成分が
２０〜４０メツシュとなるように粉砕したものの嵩密度
は、前者で０．５８ｇ ／ ｃｃ 、後者で０．６ｇ／
ＣＣであった。Compression molding is performed at a pressure of 5 kg at a temperature ranging from room temperature to 170°C.
By appropriately selecting a value of /ci or more, a plate-like body having a high bulk density that can be crushed can be obtained. For example, the compression pressure is 1200 kg/cnf at room temperature and 5 kg/cnf at 170°C.
The bulk density of the plate obtained under the conditions of 1 was pulverized so that the main component of the particle size distribution of the powder was 20 to 40 mesh, the former was 0.58 g / cc, and the latter was 0.6 g / cc.
It was CC.
圧縮成形温度が１７０℃を越えると、僅かの加圧により
得られる板状体は高強度のものとなり粉砕が困難となる
。また、圧縮成形後の粉砕粉状体の粒度は、粉砕機の機
種、条件その他により任意に選択することが可能である
が、押出ペレット化時などに種々の添加物を均一に混合
するため、あるいは粉塵の発生による障害を無くするこ
となどのため、２０〜４０メツシュとなるように粉砕す
るのが好ましい。When the compression molding temperature exceeds 170° C., the plate-like material obtained by slight pressure becomes so strong that it becomes difficult to crush it. In addition, the particle size of the pulverized powder after compression molding can be arbitrarily selected depending on the type of pulverizer, conditions, etc., but in order to uniformly mix various additives during extrusion pelletization, etc. Alternatively, in order to eliminate problems caused by the generation of dust, it is preferable to grind the material into 20 to 40 meshes.
以上の方法により得た本発明のポリカーボネート樹脂粉
状体は、通常、押出ベレット化し、成形に用いる。The polycarbonate resin powder of the present invention obtained by the above method is usually formed into extrusion pellets and used for molding.
以下、本発明を実施例により説明する。The present invention will be explained below with reference to Examples.
実施例−１
攪拌機、排出口、滴下ノズル、脱気口の付いた７５ Ａ
のジャケット付き容器に水を４０ Ａ入れ、攪拌しなが
ら水温を５５℃に昇温した。別に準備した樹脂濃度２５
重量％、分子ｆｆ１２．５Ｘ１０’のポリカーボネート
樹脂のメチレンクロライド溶液２０１とｎ−ヘプタン５
１を均一に混合した混合液を、強攪拌下の上記水に、約
１時間で滴下した。滴下中の容器内の温度は５５℃に維
持した。滴下終了後、直ちに容器内温度を９５℃以上に
昇温し、残余の溶媒を約３０分かかって蒸発除去した。Example-1 75 A with a stirrer, discharge port, dripping nozzle, and deaeration port
40 A of water was put into a jacketed container, and the water temperature was raised to 55° C. while stirring. Separately prepared resin concentration 25
Weight %, methylene chloride solution of polycarbonate resin with molecules ff 12.5 x 10' 201 and n-heptane 5
A uniformly mixed solution of 1 was added dropwise to the above water under strong stirring over about 1 hour. The temperature inside the container was maintained at 55° C. during the dropping. Immediately after the dropwise addition was completed, the temperature inside the container was raised to 95° C. or higher, and the remaining solvent was evaporated off over a period of about 30 minutes.
ついで、容器内のポリカーボネート樹脂水懸濁液を取り
出し、濾過分離し水切りをした。このようにして得たポ
リカーボネート樹脂粉粒状体は直径５ｍｍ〜１０ｍｍ程
度の大きさであった。Then, the aqueous polycarbonate resin suspension in the container was taken out, filtered and drained. The polycarbonate resin powder thus obtained had a diameter of about 5 mm to 10 mm.
この粉粒状体を粉砕機（ターボ工業■製、ターボミルＴ
−４００−４−Ｊ型）を用い、９０％以上が１６メツシ
ュの篩を通過しない程度の大きさまで粉砕し、この粉砕
品を１４０℃で３時間熱風循環乾繰機で乾煙した。乾燥
後の樹脂粉状体品中のメチレンクロライドは１０ｐｐｍ
以下、ｎ−ヘプタンは１５０ｐｐｍ 、嵩密度は０．３
２ｇ ／ ｃｃであった。This powder and granule material is processed using a pulverizer (Turbo Kogyo ■, Turbo Mill T).
-400-4-J type) to a size such that 90% or more did not pass through a 16-mesh sieve, and the pulverized product was dried and smoked in a hot air circulation dryer at 140°C for 3 hours. Methylene chloride in the resin powder product after drying is 10 ppm.
Below, n-heptane is 150 ppm, bulk density is 0.3
It was 2g/cc.
この乾燥粉状体を圧縮造粒機（不二パウダル０菊製、Ｉ
ＩＭ−１６００Ｓ ＩＩ ｒｉ型）を用い、常温で圧縮
圧力２０００ ｋｇ／ ｃｎｌで圧縮し、板状晶とし、
粗粉砕後、更に、粉砕機を用いて粉砕し、粒度分布が１
０〜３０メツシュア０％、３０メツシュ以下３０％で、
嵩密度０、５９０のポリカーボネート樹脂粉状体を得た
。This dry powder was processed using a compression granulator (manufactured by Fuji Powdal 0 Kiku, I
IM-1600S II ri type) at room temperature with a compression pressure of 2000 kg/cnl to form plate crystals.
After coarse pulverization, further pulverization is performed using a pulverizer until the particle size distribution is 1.
0 to 30 mesh 0%, 30 mesh or less 30%,
A polycarbonate resin powder having a bulk density of 0.590 was obtained.
以上、発明の詳細な説明および実施例から明白な如く、
本発明の方法によれば、容易に粒子径が揃い、かつ残存
溶媒の少ない粉体が得られるものであり、熱安定性、そ
の他の優れた高品質のポリカーボネート樹脂が？昇られ
るものであり、１重々の用途に極めて好適に利用出来る
ものである。As is clear from the detailed description and examples of the invention,
According to the method of the present invention, it is possible to easily obtain a powder with a uniform particle size and a small amount of residual solvent, and to obtain a high-quality polycarbonate resin with excellent thermal stability and other properties. It can be used very suitably for multiple purposes.
Claims (1)
ず、乾燥後の残存塩化メチレンの量が１００ｐｐｍ以下
であり、かつ、その他の残存溶媒の量が５００ｐｐｍ以
下であるポリカーボネート樹脂粉粒状体を乾式圧縮成形
し、次いで、得られた成形物を破砕することからなる残
存溶媒量が少なく、かつ、嵩密度が高いポリカーボネー
ト樹脂粉状体の製造法 ２ 該ポリカーボネート樹脂粉粒状体が、ポリカーボネ
ート樹脂の塩化メチレン溶液にポリカーボネート樹脂の
非溶媒を沈澱物が生じない程度の量で加え、得られた混
合液を４５〜１００℃に保たれた熱水中に滴下あるいは
噴霧することによって得られるものである範囲第１項記
載の製造法。 ３ ポリカーボネート樹脂の非溶媒がノルマルへプタン
（ｎ−ヘプタン）である特許請求の範囲第２項記載の製
造法。 ４ 樹脂量が１５〜２５重量％の濃度になるように予め
濃縮されたポリカーボネート樹脂の塩化メチレン溶液に
容量比で０．１５〜０．５となる量のｎ−ヘプタンを加
え、均一になるまで攪拌混合して得られる混合液を用い
る特許請求の範囲第３項記載の製造法。 ５ 室温ないし１７０℃の温度で成形圧力５ｋｇ／ｃｍ
＾２以上で乾式圧縮成形する特許請求の範囲第１項記載
の製造法。[Claims] 1. 90% or more of the total amount does not pass through a 16 mesh sieve, the amount of methylene chloride remaining after drying is 100 ppm or less, and the amount of other residual solvents is 500 ppm or less Method 2 for producing a polycarbonate resin powder with a small amount of residual solvent and a high bulk density, which comprises dry compression molding a polycarbonate resin powder and then crushing the obtained molded product. The process involves adding a non-solvent for polycarbonate resin to a methylene chloride solution of polycarbonate resin in an amount that does not cause precipitation, and dropping or spraying the resulting mixture into hot water maintained at 45 to 100°C. The manufacturing method according to item 1, which is obtained by. 3. The manufacturing method according to claim 2, wherein the non-solvent of the polycarbonate resin is normal heptane (n-heptane). 4 Add n-heptane in an amount of 0.15 to 0.5 by volume to a methylene chloride solution of polycarbonate resin that has been concentrated in advance so that the resin amount is 15 to 25% by weight, and mix until uniform. The manufacturing method according to claim 3, which uses a liquid mixture obtained by stirring and mixing. 5 Molding pressure 5kg/cm at a temperature between room temperature and 170℃
The manufacturing method according to claim 1, which comprises dry compression molding at a temperature of ^2 or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17877586A JPS6335621A (en) | 1986-07-31 | 1986-07-31 | Production of polycarbonate resin powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17877586A JPS6335621A (en) | 1986-07-31 | 1986-07-31 | Production of polycarbonate resin powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6335621A true JPS6335621A (en) | 1988-02-16 |
| JPH0512371B2 JPH0512371B2 (en) | 1993-02-17 |
Family
ID=16054409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17877586A Granted JPS6335621A (en) | 1986-07-31 | 1986-07-31 | Production of polycarbonate resin powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6335621A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0300485A2 (en) * | 1987-07-21 | 1989-01-25 | Mitsubishi Gas Chemical Company, Inc. | Process for producing polycarbonate resin molding material with low particle content |
| WO1994005722A1 (en) * | 1992-08-31 | 1994-03-17 | Mitsubishi Rayon Co., Ltd. | Process for producing powdery thermoplastic copolymer |
| WO1995008585A1 (en) * | 1993-09-21 | 1995-03-30 | Teijin Chemicals Ltd. | Aromatic polycarbonate resin particulate and process for producing the same |
| US5760160A (en) * | 1993-09-21 | 1998-06-02 | Teijin Chemicals Ltd. | Aromatic polycarbonate resin granule |
| WO2019188953A1 (en) * | 2018-03-30 | 2019-10-03 | 株式会社Adeka | Granular ultraviolet absorber and resin composition |
| JPWO2018216516A1 (en) * | 2017-05-24 | 2020-04-02 | 三菱瓦斯化学株式会社 | Sheet made of carbon fiber reinforced thermoplastic resin and method for producing the sheet |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112322015B (en) * | 2020-10-16 | 2022-06-24 | 金发科技股份有限公司 | Polycarbonate/polystyrene alloy and preparation method and application thereof |
-
1986
- 1986-07-31 JP JP17877586A patent/JPS6335621A/en active Granted
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0300485A2 (en) * | 1987-07-21 | 1989-01-25 | Mitsubishi Gas Chemical Company, Inc. | Process for producing polycarbonate resin molding material with low particle content |
| WO1994005722A1 (en) * | 1992-08-31 | 1994-03-17 | Mitsubishi Rayon Co., Ltd. | Process for producing powdery thermoplastic copolymer |
| US5521231A (en) * | 1992-08-31 | 1996-05-28 | Mitsubishi Rayon Co., Ltd. | Process for producing thermoplastic copolymer powder |
| WO1995008585A1 (en) * | 1993-09-21 | 1995-03-30 | Teijin Chemicals Ltd. | Aromatic polycarbonate resin particulate and process for producing the same |
| US5663277A (en) * | 1993-09-21 | 1997-09-02 | Teijin Chemicals, Ltd. | Aromatic polycarbonate resin granule and process for the production thereof |
| US5760160A (en) * | 1993-09-21 | 1998-06-02 | Teijin Chemicals Ltd. | Aromatic polycarbonate resin granule |
| US11365298B2 (en) | 2017-05-24 | 2022-06-21 | Mitsubishi Gas Chemical Company, Inc. | Sheet formed from carbon fiber reinforced thermoplastic resin, and production method of said sheet |
| JPWO2018216516A1 (en) * | 2017-05-24 | 2020-04-02 | 三菱瓦斯化学株式会社 | Sheet made of carbon fiber reinforced thermoplastic resin and method for producing the sheet |
| WO2019188953A1 (en) * | 2018-03-30 | 2019-10-03 | 株式会社Adeka | Granular ultraviolet absorber and resin composition |
| CN112105704A (en) * | 2018-03-30 | 2020-12-18 | 株式会社艾迪科 | Particulate ultraviolet absorber and resin composition |
| JP2021050345A (en) * | 2018-03-30 | 2021-04-01 | 株式会社Adeka | Granular ultraviolet absorber and resin composition |
| JPWO2019188953A1 (en) * | 2018-03-30 | 2020-04-30 | 株式会社Adeka | Granular ultraviolet absorber and resin composition |
| CN112105704B (en) * | 2018-03-30 | 2023-08-22 | 株式会社艾迪科 | Particulate ultraviolet absorber and resin composition |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0512371B2 (en) | 1993-02-17 |
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