JP2677685B2 - Continuous toner manufacturing method - Google Patents
Continuous toner manufacturing methodInfo
- Publication number
- JP2677685B2 JP2677685B2 JP1289162A JP28916289A JP2677685B2 JP 2677685 B2 JP2677685 B2 JP 2677685B2 JP 1289162 A JP1289162 A JP 1289162A JP 28916289 A JP28916289 A JP 28916289A JP 2677685 B2 JP2677685 B2 JP 2677685B2
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- resin
- material supply
- kneading
- supply port
- 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 - Fee Related
Links
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はトナーの連続製造方法及び該製造方法により
得られるトナーに関する詳しくは、トナー製造工程中で
の原料樹脂と、着色剤等の添加剤との溶融混練工程にお
いて、樹脂中への添加剤の分散性を向上させると同時
に、樹脂の分子切断を抑制することにより、優れたトナ
ー品質を付与し、しかも生産効率を向上させたトナーの
連続製造方法及び該製造方法により得られるトナーに関
するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of use] The present invention relates to a method for continuously producing a toner and a toner obtained by the method, more specifically, a raw material resin in a toner production process and an additive such as a colorant. In the melt-kneading process with and, while improving the dispersibility of the additive in the resin, at the same time by suppressing the molecular cleavage of the resin, excellent toner quality is imparted, and the continuous production of toner with improved production efficiency. The present invention relates to a manufacturing method and a toner obtained by the manufacturing method.
混練装置による、樹脂中への添加剤の分散あるいは複
数の樹脂どうしの分散はトナーを一例とする機能性材料
あるいは複合樹脂等の開発、生産に見られるように従来
から広く行われており、その製造法については文献等に
多数報告されている。これらの方法はいずれも、分散能
力を向上させるために、混練原料に分散剤を加える、混
練機の操作条件で対応する、混練機中のスクリューを変
更する、あるいは最初に原料樹脂の一部と添加剤の一部
又は全部とを混練した後、この混練物を冷却、固化、粉
砕し、この粉砕品と残りの樹脂及び添加剤を混合した
後、再度混練するいわゆるマスターバッチ法を採用する
等の工夫をしている。Dispersion of the additive in the resin or dispersion of a plurality of resins by a kneading device has been widely performed from the past as seen in the development and production of functional materials or composite resins such as toner. Many manufacturing methods have been reported in the literature. In any of these methods, in order to improve the dispersibility, a dispersant is added to the kneading raw material, corresponding to the operating conditions of the kneading machine, the screw in the kneading machine is changed, or first a part of the raw material resin is used. After kneading a part or all of the additives, this kneaded product is cooled, solidified, crushed, the crushed product is mixed with the rest of the resin and additives, and then kneaded again. Is devising.
しかしこれらの従来法では、分散剤を加えることによ
り分散能力を向上させる方法では、分散剤が製品物性上
好ましくない場合には、目的とする製品物性を得ること
ができないという問題点があり、また混練機の操作条件
やスクリューを変更することにより分散能力を向上させ
る方法では、高い剪断力あるいは高温度による樹脂の劣
化等の現象により製品物性を損なうという問題がある。
またマスターバッチ法では、混練工程を２回に分割する
ことにより、１回目の混練ではある程度の樹脂の分子切
断が起こるものの、供給原料中の添加剤濃度が高いため
充分な分散が可能となり、２回目の混練では１回目の混
練によって得られた添加剤が充分に分散した高濃度樹脂
を１回目の混練より小さな剪断力で希釈混練すればよい
ことから、樹脂の分子切断による物性の低下を抑制する
ことができ、分子切断の比較的少ない、分散性の良好な
混練物を得ることができるが、この方法では１種類の製
品を得るにも混練工程が２回必要であり、またこの方法
は１回目の混練終了後、冷却、固化、粉砕工程が必要で
あり、さらにはこの粉砕物と残りの混練原料との混合工
程が必要であるといった理由から生産効率が低いという
問題がある。However, in these conventional methods, the method of improving the dispersing ability by adding a dispersant has a problem that the desired product physical properties cannot be obtained when the dispersant is not preferable in terms of product physical properties, and The method of improving the dispersing ability by changing the operating conditions of the kneader and the screw has a problem that the physical properties of the product are impaired due to phenomena such as deterioration of the resin due to high shearing force or high temperature.
Further, in the masterbatch method, by dividing the kneading step into two parts, although molecular cutting of the resin occurs to some extent in the first kneading, the additive concentration in the feed material is high, so that sufficient dispersion is possible. In the first kneading, the high-concentration resin in which the additive obtained in the first kneading is sufficiently dispersed may be diluted and kneaded with a smaller shearing force than that in the first kneading, so that the deterioration of the physical properties due to the resin molecular cutting is suppressed It is possible to obtain a kneaded product with relatively low molecular cleavage and good dispersibility, but this method requires two kneading steps to obtain one type of product, and this method There is a problem that the production efficiency is low because the cooling, solidification and crushing steps are required after the first kneading and the mixing step of the crushed material and the remaining kneading raw material is necessary.
本発明者らは上述のような従来技術の状況に鑑み、分
散能力に優れ生産効率の高いトナーの連続製造方法を見
出すべく鋭意研究の結果、本発明を完成するに到った。The present inventors have completed the present invention as a result of earnest research in order to find a method for continuously producing a toner having excellent dispersion ability and high production efficiency, in view of the above-mentioned state of the art.
即ち、本発明は、樹脂及び添加剤からなる組成物を溶
融混練し、冷却、固化、粉砕し、分級してトナーを製造
する方法において、押し出し流れ性を有するバレル長さ
Ｌの混練押し出し機の入口側から0.3L以内の位置に設け
られた少なくとも１個所の原料供給口から樹脂中の添加
剤濃度（以下前半部添加剤濃度という）が10〜50重量％
の混合原料を連続的に供給し、入口側から0.3L〜0.9Lの
位置に設けられた１〜５個所の原料供給口から樹脂単独
もしくは樹脂中の添加剤濃度が20重量％以下でかつ上記
前半部添加剤濃度より低い濃度の原料を連続的に供給
し、かつ0.3L以内の位置の原料供給口に供給する原料と
0.3L〜0.9Lの位置の原料供給口に供給する原料との供給
流量の比を10:1〜1:5（重量比）にすると共に、混練押
し出し機出口から混練物を連続的に取り出すことを特徴
とするトナーの連続製造方法、及び該製造方法により得
られたトナーを提供するものである。That is, the present invention relates to a method for producing a toner by melt-kneading a composition comprising a resin and an additive, cooling, solidifying, pulverizing, and classifying the composition, and a kneading extruder having a barrel length L having an extrusion flow property. The additive concentration in the resin (hereinafter referred to as the first half additive concentration) is 10 to 50% by weight from at least one raw material supply port provided within 0.3 L from the inlet side.
Of the mixed raw material is continuously supplied, and the resin alone or the additive concentration in the resin is 20% by weight or less from 1 to 5 raw material supply ports provided at positions 0.3L to 0.9L from the inlet side, and The raw material with a concentration lower than the first half additive concentration is continuously supplied, and the raw material is supplied to the raw material supply port within 0.3L.
The ratio of the supply flow rate of the raw material supplied to the raw material supply port at the position of 0.3L to 0.9L is set to 10: 1 to 1: 5 (weight ratio), and the kneaded material is continuously taken out from the kneading extruder outlet. The present invention also provides a method for continuously producing a toner, and a toner obtained by the method.
本発明のトナーの連続製造方法を図面に基づいて詳細
に説明する。The continuous toner manufacturing method of the present invention will be described in detail with reference to the drawings.
第１図は本発明のトナーの連続製造方法の一例を示す
フローシートであり、１は原料計量器、２は予備混合
機、３は原料供給装置、４はバレル長さＬに対して入口
側から0.3L以内の位置に設けられた原料供給口、４′は
入口側から0.3L〜0.9Lの位置に設けられた原料供給口、
５は混練押し出し機、６は混練押し出し機外筒部冷却装
置、７は混練物冷却機、８は粉砕・分級機である。FIG. 1 is a flow sheet showing an example of the continuous toner production method of the present invention, in which 1 is a raw material meter, 2 is a premixer, 3 is a raw material supply device, and 4 is an inlet side with respect to a barrel length L. From the inlet side, 4'is a raw material supply port provided at a position within 0.3L to 0.9L,
Reference numeral 5 is a kneading extruder, 6 is a kneading extruder outer cylinder cooling device, 7 is a kneading material cooler, and 8 is a crushing / classifying machine.
本発明に用いられる混練押し出し機５は、流れ方向に
対しては実質的に混合能力がなく、半径方向に対して混
合能力を有し、流れ方向に平行なスクリューを備えた混
練押し出し機であればどの様な形式でもよいが、連続二
軸押し出し機が好ましい。また混練時の発熱による樹脂
の熱劣化を抑制するため、バレル（混練押し出し機外筒
部）及び／又はスクリューには、適当な方法による冷却
装置６を設けることが好ましい。The kneading extruder 5 used in the present invention may be a kneading extruder having substantially no mixing ability in the flow direction, a mixing ability in the radial direction, and a screw parallel to the flow direction. Any form may be used, but a continuous twin-screw extruder is preferred. Further, in order to suppress heat deterioration of the resin due to heat generation during kneading, it is preferable to provide the barrel (kneading extruder outer cylinder portion) and / or the screw with a cooling device 6 by an appropriate method.
また本発明に用いられる混練押し出し機５には、バレ
ル長さＬに対して入口側から0.3L以内の位置に少なくと
も１個所の原料供給口４、入口側から0.3L〜0.9Lの位置
に１〜５個所の原料供給口４′が設けられ、混練押し出
し機内のスクリューは、各原料供給部分において原料あ
るいは混練物の移送に優れ、次の原料の供給口に至るま
でに、分散能力に優れるように構成されるのが好まし
い。このために原料供給口はバレル内径Ｄの少なくとも
２〜３倍以上の距離をおいて配設される。また混練押し
出し機のバレル長さＬとバレル内径Ｄの比L/Dは20〜7
0、バレル長さＬは0.5〜7m、バレル内径Ｄは20〜150mm
のものが通常用いられる。The kneading extruder 5 used in the present invention has at least one raw material supply port 4 at a position within 0.3L from the inlet side with respect to the barrel length L, and 1 at a position 0.3L to 0.9L from the inlet side. ~ 5 raw material supply ports 4'are provided, and the screw in the kneading extruder is excellent in transferring the raw material or the kneaded material in each raw material supply part, and has excellent dispersion ability until reaching the next raw material supply port. Preferably, For this reason, the raw material supply port is arranged at a distance of at least 2-3 times the inner diameter D of the barrel. The ratio L / D of barrel length L and barrel inner diameter D of the kneading extruder is 20 to 7
0, barrel length L is 0.5 to 7 m, barrel inner diameter D is 20 to 150 mm
What is usually used.
本発明に用いられる混練押し出し機の好ましい実施態
様を第２図に示す。A preferred embodiment of the kneading extruder used in the present invention is shown in FIG.
第２図に示す混練押し出し機５は二軸押し出し機であ
り、バレル長さＬに対して入口側から0.3L以内の位置に
１個所の原料供給口４を、また入口側から0.3L〜0.9Lの
位置に２個所の原料供給口４′が設けられている。また
原料供給口４′の周りにはジャケット９、原料供給口
４′の手前には脱気孔10が設けられている。更にバレル
には冷却装置６が設けられている。第２図の二軸押し出
し機のＡ−Ａ線断面図を第３図に示す。第３図におい
て、11はバレル、12はスクリュー、13はスクリュー谷
部、14はスクリュー山部である。またＤはバレル内径で
ある。The kneading extruder 5 shown in FIG. 2 is a twin-screw extruder, and has one raw material supply port 4 at a position within 0.3 L from the inlet side with respect to the barrel length L, and 0.3 L to 0.9 L from the inlet side. Two raw material supply ports 4'are provided at the L position. A jacket 9 is provided around the raw material supply port 4 ', and a deaeration hole 10 is provided in front of the raw material supply port 4'. Further, the barrel is provided with a cooling device 6. A sectional view taken along the line AA of the twin-screw extruder shown in FIG. 2 is shown in FIG. In FIG. 3, 11 is a barrel, 12 is a screw, 13 is a screw trough, and 14 is a screw crest. D is the barrel inner diameter.
本発明において、混練押し出し機に供給される原料樹
脂はトナーのバインダー樹脂であれば特に限定されず、
例えばポリエチレン及びポリプロピレンの如きポリオレ
フィン類を含む熱可塑性樹脂類、ポリブタジエン、ポリ
イソブチレン及びポリクロロプレンの如きジエン類から
誘導した重合体類、ポリスチレン、ポリエチルアクリレ
ート、スチレン−ブチルメタクリレート共重合体類、ス
チレン−アクリロニトリル共重合体類、アクリロニトリ
ル−ブタジエン−スチレン三元共重合体類、ポリメチル
メタクリレート、ポリアクリレート類、ポリビニルアル
コール、ポリ塩化ビニル、ポリビニルカルバゾール、ポ
リビニルエーテル類及びポリビニルケトン類の如きビニ
ル及びビニリデン重合体類並びにその共重合体類：ポリ
テトラフルオロエチレン及びポリ弗化ビニリデンの如き
フルオロカーボン重合体類：ポリアミド類、ポリエステ
ル類、ポリウレタン類、ポリペプチド類、カゼイン、ポ
リグリコール類、ポリスルファイド類及びポリカーボネ
ート類の如きヘテロ・チェイン（hetero chain）系熱可
塑性樹脂類、並びに再生セルロース、酢酸セルロース及
び硝酸セルロースの如きセルロース系共重合体類等が挙
げられる。また混練、冷却後の粉砕・分級工程で得られ
るトナー粒径規定外の回収微粉も原料樹脂として混練押
し出し機に供給してもよい。本発明でいう原料樹脂は上
記各種原料樹脂のみでなく、該回収微粉も意味する。In the present invention, the raw material resin supplied to the kneading extruder is not particularly limited as long as it is a binder resin for the toner,
Thermoplastic resins containing polyolefins such as polyethylene and polypropylene, polymers derived from dienes such as polybutadiene, polyisobutylene and polychloroprene, polystyrene, polyethyl acrylate, styrene-butyl methacrylate copolymers, styrene- Vinyl and vinylidene polymers such as acrylonitrile copolymers, acrylonitrile-butadiene-styrene terpolymers, polymethylmethacrylate, polyacrylates, polyvinyl alcohol, polyvinyl chloride, polyvinylcarbazole, polyvinyl ethers and polyvinyl ketones. And their copolymers: Fluorocarbon polymers such as polytetrafluoroethylene and polyvinylidene fluoride: Polyamides, polyesters, polyurethanes Chain, hetero chain thermoplastic resins such as compounds, polypeptides, casein, polyglycols, polysulfides and polycarbonates, and cellulosic copolymers such as regenerated cellulose, cellulose acetate and cellulose nitrate And the like. Further, recovered fine powder having a toner particle size not specified, which is obtained in the pulverization / classification step after kneading and cooling, may be supplied to the kneading extruder as a raw material resin. The raw material resin in the present invention means not only the above various raw material resins but also the recovered fine powder.
また本発明で用いられる添加剤はトナーの製造に用い
られる従来公知の添加剤であり、例えば染顔料、荷電制
御剤、カーボンブラック、磁性粉、ワックス等が挙げら
れる。The additive used in the present invention is a conventionally known additive used in the production of toner, and examples thereof include dyes and pigments, charge control agents, carbon black, magnetic powder, and wax.
上記の如き原料樹脂及び添加剤は、各々一種単独で使
用しても、二種以上併用してもよい。また原料の供給
は、樹脂と添加剤を予備混合機２で予備混合した後、混
練押し出し機５に設置された入口側から0.3L以内の位置
に設けられた少なくとも１個所の供給口４から定量的に
供給し、残りの樹脂及び添加剤の混合物又は樹脂のみを
0.3L〜0.9Lの位置に設けられた１〜５個の供給口４′か
ら定量的に供給する。0.3L以内の位置に設けられた原料
供給口４から供給される原料は樹脂中の添加剤濃度が10
〜50重量％のものであり、0.3L〜0.9Lの位置に設けられ
た原料供給口４′から供給される原料は樹脂単独もしく
は樹脂中の添加剤濃度が20重量％以下、好ましくは10重
量％以下でかつ前半部添加剤濃度より低いものである。
原料供給口４に供給される原料の組成が上記範囲を外れ
て、添加剤が多すぎても少なすぎても添加剤の樹脂中へ
の分散が不十分となる。また原料供給口４′に供給され
る原料の組成が上記範囲を外れると分散不良が生ずる。
更に0.3L以内の位置の原料供給口に供給する原料と0.3L
〜0.9Lの位置の原料供給口に供給する原料との供給流量
の比は10:1〜1:5（重量比）、好ましくは3:1〜1:3であ
り、供給流量比が10:1より大きくなると希釈効果が減少
し、1:5より小さくなると装置効率が悪くなる。The above raw material resins and additives may be used alone or in combination of two or more. In addition, the raw materials are supplied by pre-mixing the resin and the additive in the pre-mixer 2, and then quantitatively from at least one supply port 4 provided within 0.3 L from the inlet side installed in the kneading extruder 5. Of the remaining resin and additives or only the resin
It is quantitatively supplied from 1 to 5 supply ports 4'provided at positions of 0.3L to 0.9L. The raw material supplied from the raw material supply port 4 provided at a position within 0.3L has an additive concentration of 10 in the resin.
˜50 wt%, and the raw material supplied from the raw material supply port 4 ′ provided at a position of 0.3 L to 0.9 L has a resin alone or an additive concentration in the resin of 20% by weight or less, preferably 10% by weight. % Or less and lower than the concentration of the additive in the first half.
If the composition of the raw material supplied to the raw material supply port 4 is out of the above range and the amount of the additive is too large or too small, the additive will not be sufficiently dispersed in the resin. Further, if the composition of the raw material supplied to the raw material supply port 4'is out of the above range, poor dispersion occurs.
Furthermore, the raw material supplied to the raw material supply port located within 0.3L and 0.3L
The ratio of the supply flow rate of the raw material supplied to the raw material supply port at a position of ~ 0.9L is 10: 1 to 1: 5 (weight ratio), preferably 3: 1 to 1: 3, and the supply flow rate ratio is 10: When it is larger than 1, the dilution effect is reduced, and when it is smaller than 1: 5, the efficiency of the apparatus is deteriorated.
原料供給口４は入口側から0.3L以内であれば樹脂中へ
の添加剤の分散が十分に達成されるが、0.3L以降では滞
留時間が少なくなり分散が不十分となるため好ましくな
い。該原料供給口４は少なくとも１個所設けられるが、
１もしくは２個所が好ましい。また0.3L〜0.9Lの位置に
配設される原料供給口４′の数は１〜５個所であり、６
個所以上設けても設備が複雑になるだけで実質的に効果
がない。When the raw material supply port 4 is within 0.3 L from the inlet side, the additive can be sufficiently dispersed in the resin, but after 0.3 L, the residence time becomes short and the dispersion becomes insufficient, which is not preferable. At least one raw material supply port 4 is provided,
One or two locations are preferred. Further, the number of raw material supply ports 4'disposed at the position of 0.3L to 0.9L is 1 to 5 and 6
Even if it is provided in more than one place, the equipment becomes complicated and practically ineffective.
本発明において、混練押し出し機中の原料の滞留時間
20秒〜600秒が好ましく、50秒〜500秒が更に好ましい。
滞留時間が上記範囲より短いと分散不良となり、また長
いと樹脂が劣化する。混練押し出し機の混練温度は樹脂
の軟化点より70℃低い温度〜樹脂の軟化点より50℃高い
温度の範囲が好ましく、樹脂の軟化点より40℃低い温度
〜樹脂の軟化点より10℃低い温度の範囲が更に好まし
い。混練温度が上記範囲より低いと樹脂の溶融状態が悪
く分散不良を生じ、高いと樹脂の劣化及び樹脂の粘度低
下により分散不良が生じる。また混練物の出口温度は樹
脂の軟化点より５℃高い温度〜樹脂の軟化点より100℃
高い温度の範囲が好ましく、樹脂の軟化点より30℃高い
温度〜樹脂の軟化点より70℃高い温度の範囲が更に好ま
しい。出口温度が上記範囲より低いと樹脂の溶融状態が
悪く分散不良を生じ、高いと樹脂の劣化及び樹脂の粘度
低下により分散不良が生じる。In the present invention, the residence time of the raw material in the kneading extruder
20 seconds to 600 seconds are preferable, and 50 seconds to 500 seconds are more preferable.
If the residence time is shorter than the above range, poor dispersion will result, and if it is long, the resin will deteriorate. The kneading temperature of the kneading extruder is preferably in the range of 70 ° C lower than the softening point of the resin to 50 ° C higher than the softening point of the resin, 40 ° C lower than the softening point of the resin to 10 ° C lower than the softening point of the resin. Is more preferable. If the kneading temperature is lower than the above range, the molten state of the resin will be poor, resulting in poor dispersion. The temperature of the kneaded product is 5 ° C higher than the softening point of the resin to 100 ° C higher than the softening point of the resin.
A high temperature range is preferable, and a temperature range of 30 ° C. higher than the softening point of the resin to 70 ° C. higher than the softening point of the resin is more preferable. If the outlet temperature is lower than the above range, the molten state of the resin will be poor and poor dispersion will occur. If it is high, the poor resin will cause deterioration of the viscosity of the resin, resulting in poor dispersion.
上記の如き本発明のトナーの連続製造方法により、樹
脂中への添加剤の分散性が優れ、しかも樹脂の分子切断
の少ない、品質の優れたトナーを得ることができるが、
この理由は、入口側から0.3L以内の位置（以下前半部と
略記する）の原料供給口と0.3L〜0.9Lの位置（以下後半
部と略記する）の原料供給口から供給される原料中の樹
脂含有量の差、及び原料供給流量及び原料供給量の分配
比率を制御することによる混練押し出し機内滞留時間の
差による。By the continuous production method of the toner of the present invention as described above, it is possible to obtain a high-quality toner having excellent dispersibility of the additive in the resin and having less resin molecular cleavage,
The reason for this is that in the raw material supplied from the raw material supply port at a position within 0.3L from the inlet side (hereinafter abbreviated as the first half part) and the raw material supply port at 0.3L to 0.9L position (hereinafter abbreviated as the second half part). Of the resin content and the difference of the residence time in the kneading extruder by controlling the raw material supply flow rate and the distribution ratio of the raw material supply amount.
即ち前半部から供給される原料は樹脂含有量が低く、
溶融しにくいため混練押し出し機内で高い剪断力を受け
ることが出来、優れた分散能力を付与することが可能で
ある。しかしこの状態のままで後半部の供給口から原料
を供給しなければ、前半部から供給された原料は小流量
であることから非常に滞留時間が長くなってしまうた
め、混練押し出し機の出口方向に進むにしたがって、樹
脂の分子切断は著しいものとなってしまう。そこで後半
部から樹脂含有量の高い原料が供給されるが、前半部で
充分分散した、添加剤を高濃度に含む樹脂は、この後半
部から供給される原料で希釈効果を受けることによっ
て、必要以上の剪断力による分子切断を免れることが可
能となる。That is, the raw material supplied from the first half has a low resin content,
Since it is difficult to melt, it can be subjected to a high shearing force in the kneading extruder, and it is possible to impart excellent dispersing ability. However, if the raw material is not supplied from the supply port of the latter half in this state, the raw material supplied from the first half has a small flow rate and the residence time becomes very long. The molecular breakage of the resin becomes remarkable as the process proceeds to. Therefore, a raw material with a high resin content is supplied from the latter half, but the resin that is sufficiently dispersed in the first half and contains a high concentration of additives is required by the raw material supplied from this latter half to undergo a dilution effect. It becomes possible to avoid the molecular cutting by the above shearing force.
一方、後半部から供給される原料は、樹脂含有量が高
いため、前半部から供給される原料に比べ溶融し易い。
さらに前半部から移送される混練物が溶融状態であるこ
とから、一層溶融しやすく、機内滞留時間が短くても充
分な混練が可能となる。またこのことは樹脂の分子切断
を少なくする上で非常に効果がある。On the other hand, since the raw material supplied from the latter half has a high resin content, it is easier to melt than the raw material supplied from the first half.
Further, since the kneaded product transferred from the first half portion is in a molten state, it is more easily melted, and sufficient kneading can be performed even when the residence time in the machine is short. This is also very effective in reducing the molecular breakage of the resin.
このように前半部と後半部から供給する原料の樹脂含
有量の比率を制御し、また各々の原料の機内滞留時間を
制御することにより、前半部では分散を主とする混練
が、また後半部では物性の劣化を抑制する混練が可能と
なり、優れた品質を有するトナーを高い生産効率で製造
することが可能となる。In this way, by controlling the ratio of the resin content of the raw materials supplied from the first half and the second half, and by controlling the residence time of each raw material in the machine, kneading mainly for dispersion in the first half, and again in the second half. With this, kneading that suppresses deterioration of physical properties becomes possible, and it becomes possible to manufacture a toner having excellent quality with high production efficiency.
本発明において用いられる原料は、粉体のみでなく、
必要に応じて液体原料を供給してもよい。また製品の品
質をさらに向上させるため、必要に応じて減圧による脱
気処理を行うことも好ましい。The raw material used in the present invention is not limited to powder,
You may supply a liquid raw material as needed. Moreover, in order to further improve the quality of the product, it is also preferable to perform degassing treatment under reduced pressure, if necessary.
以下、実施例により本発明を更に詳細に説明するが、
本発明はこれらの実施例に限定されるものではない。Hereinafter, the present invention will be described in more detail by examples,
The present invention is not limited to these examples.
尚、例中の部は重量基準である。 The parts in the examples are based on weight.
実施例 １ 軟化点が138℃であるポリエステル樹脂100部と、該ポ
リエステル樹脂100部に対してカーボンブラック８部、
電荷制御剤２部及びワックス３部の原料粉体と、上記原
料100部に対して10部の次工程の粉砕・分級工程で得ら
れる回収微粉を溶融混練してトナー用混練物を得た。用
いた混練押し出し機は、混練部分の全長1560mm、スクリ
ュー径42mm、バレル内径43mmの同方向回転二軸押し出し
機であり、原料供給口が３箇所設置されている。Example 1 100 parts of a polyester resin having a softening point of 138 ° C., and 8 parts of carbon black based on 100 parts of the polyester resin,
A raw material powder consisting of 2 parts of the charge control agent and 3 parts of wax and 10 parts of the fine powder collected in the subsequent pulverization / classification step of 100 parts of the raw material were melt-kneaded to obtain a kneaded product for toner. The kneading extruder used is a co-rotating twin-screw extruder having a total kneading portion length of 1560 mm, a screw diameter of 42 mm, and a barrel inner diameter of 43 mm, and three raw material supply ports are provided.
各々の原料供給口の位置は、第１の原料供給口の中心
が混練部分の端面から進行方向に向かって75mmの位置で
あり、第２の原料供給口の中心が第１の原料供給口の中
から620mmの位置であり、第３の原料供給口の中心が第
１の原料供給口の中心から1100mmの位置である。The position of each raw material supply port is such that the center of the first raw material supply port is 75 mm from the end face of the kneading part in the traveling direction, and the center of the second raw material supply port is the first raw material supply port. The position is 620 mm from the center, and the center of the third raw material supply port is 1100 mm from the center of the first raw material supply port.
該混練押し出し機の第１の原料供給口から、ポリエス
テル樹脂35部と、カーボンブラック８部、電荷制御剤２
部及びワックス３部の粉体原料を予備混合した後、定量
的に供給し、第２の原料供給口からポリエステル樹脂65
部を定量的に供給し、第３の原料供給口から回収微粉10
部を定量的に供給することにより連続混練を行った。From the first raw material supply port of the kneading extruder, 35 parts of polyester resin, 8 parts of carbon black, charge control agent 2
Parts of powder and 3 parts of wax are premixed and then quantitatively supplied, and the polyester resin 65 is supplied through the second material supply port.
Part is quantitatively supplied, and fine powder recovered from the third raw material supply port 10
Continuous kneading was performed by quantitatively supplying parts.
この混練時の操作条件は、バレル（混練押し出し機外
筒部）の設定温度は100℃、スクリュー回転数は200rpm
であり、原料供給量は第１の原料供給口へは19.3kg/H
r、第２の原料供給口へは26.2kg/Hr、第３の原料供給口
へは4.5kg/Hrであり、合計50kg/Hrであった。The operating conditions during this kneading are as follows: barrel temperature (outer cylinder of kneading extruder) 100 ° C, screw speed 200 rpm
The raw material supply rate is 19.3kg / H to the first raw material supply port.
r, 26.2 kg / Hr to the second raw material supply port, and 4.5 kg / Hr to the third raw material supply port, for a total of 50 kg / Hr.
また、この混練による樹脂出口温度は187℃であっ
た。The resin outlet temperature by this kneading was 187 ° C.
この結果得られた混練物を冷却、固化した後、粉砕、
分級し、目的とする粒径の粉体に所定の処理を施しトナ
ー性能を評価したところ、樹脂の軟化点は129℃であ
り、樹脂の分子切断の程度を表す混練前後での軟化点の
差は９℃と小さく、しかも樹脂中への添加剤の分散も良
好な優れたトナーが得られた。The kneaded product obtained as a result is cooled and solidified, and then pulverized,
When the toner performance was evaluated by classifying and subjecting the powder having the target particle diameter to the predetermined treatment, the softening point of the resin was 129 ° C., and the difference in the softening point before and after the kneading, which represents the degree of resin molecular cutting, was shown. Was as low as 9 ° C., and an excellent toner having a good dispersion of the additive in the resin was obtained.
ここで軟化点とは、高化式フローテスター（CFT−50
0;島津製作所製）を用い、ダイスの細孔の径約1mm、長
さ1mm、荷重20kg/cm2G、昇温速度６℃／分の条件下で1c
m3の試料を溶融流出させたときの流出開始点から流出終
了点の高さの1/2に相当する温度を軟化点とする時の値
である。Here, the softening point is a Koka type flow tester (CFT-50
0; made by Shimadzu), the diameter of the die pores is about 1 mm, the length is 1 mm, the load is 20 kg / cm 2 G, and the heating rate is 6 ° C / min.
It is the value when the softening point is the temperature corresponding to 1/2 of the height from the outflow start point to the outflow end point when the m 3 sample is melted and outflowed.
実施例 ２ 実施例１と同一の装置を用いて、軟化点が132℃であ
るポリスチレン樹脂100部と、該ポリスチレン樹脂100部
に対してカーボンブラック７部、電荷制御剤2.5部及び
ワックス３部の原料粉体と、上記原料100部に対して10
部の次工程の粉砕・分級工程で得られる回収微粉を溶融
混練してトナー用混練物を得た。Example 2 Using the same apparatus as in Example 1, 100 parts of a polystyrene resin having a softening point of 132 ° C., and 7 parts of carbon black, 2.5 parts of a charge control agent and 3 parts of wax per 100 parts of the polystyrene resin were used. Raw material powder and 10 for 100 parts of the above raw material
Part fine powder obtained in the pulverization / classification step as the next step was melt-kneaded to obtain a kneaded product for toner.
本混練において、連続押し出し機の第１の原料供給口
から、ポリスチレン樹脂40部と、カーボンブラック７
部、電荷制御剤2.5部及びワックス３部の粉体原料を予
備混合した後、定量的に供給し、第２の原料供給口から
ポリスチレン樹脂60部を定量的に供給し、第３の原料供
給口から回収微粉10部を定量的に供給することにより連
続混練を行った。In the main kneading, 40 parts of polystyrene resin and carbon black 7 were supplied from the first raw material supply port of the continuous extruder.
Parts, 2.5 parts of charge control agent and 3 parts of wax are pre-mixed, and then quantitatively supplied, and 60 parts of polystyrene resin is quantitatively supplied from the second material supply port, and third material is supplied. Continuous kneading was carried out by quantitatively supplying 10 parts of the recovered fine powder from the mouth.
この混練時の操作条件は、バレルの設定温度は100
℃、スクリュー回転数は200rpmであり、原料供給量は第
１の原料供給口へは19.1kg/Hr、第２の原料供給口へは2
1.8kg/Hr、第３の原料供給口へは4.1kg/Hrであり、合計
45kg/Hrであった。The operating conditions during this kneading are that the barrel set temperature is 100
℃, the screw rotation speed is 200 rpm, the raw material supply rate is 19.1kg / Hr to the first raw material supply port, 2 to the second raw material supply port.
1.8 kg / Hr, 4.1 kg / Hr to the third raw material supply port, total
It was 45 kg / Hr.
また、この混練による樹脂出口温度は195℃であっ
た。The resin outlet temperature by this kneading was 195 ° C.
この結果得られた混練物を冷却、固化した後、粉砕、
分級し、目的とする粒径の粉体に所定の処理を施しトナ
ー性能を評価したところ、樹脂の軟化点は125℃であ
り、樹脂の分子切断の程度を表す混練前後での軟化点の
差は７℃と小さく、しかも樹脂中への添加剤の分散も良
好な優れたトナーが得られた。The kneaded product obtained as a result is cooled and solidified, and then pulverized,
When the toner performance was evaluated by classifying and subjecting the powder having the target particle diameter to the predetermined treatment, the softening point of the resin was 125 ° C., which represents the degree of resin molecular cutting, and the difference in the softening point before and after kneading. Was as low as 7 ° C., and an excellent toner was obtained in which the additives were well dispersed in the resin.
比較例 １ 実施例１と同様に、軟化点が138℃であるポリエステ
ル樹脂100部と、該ポリエステル樹脂100部に対してカー
ボンブラック８部、電荷制御剤２部及びワックス３部の
原料粉体と、上記原料100部に対して10部の次工程の粉
砕・分級工程で得られる回収微粉を、実施例と同一の混
練押し出し機を用いて上記原料粉体を分配供給すること
なく、全量を予備混合した後、第１の原料供給口から定
量的に供給し、溶融混練を行い、トナー用混練物を得
た。Comparative Example 1 Similar to Example 1, 100 parts of a polyester resin having a softening point of 138 ° C., and 8 parts of carbon black, 2 parts of a charge control agent, and 3 parts of a wax with respect to 100 parts of the polyester resin were used as raw material powders. With respect to 100 parts of the raw material, 10 parts of the recovered fine powder obtained in the crushing / classifying step of the next step is used to prepare the entire amount of the raw material powder without distributing the raw material powder by using the same kneading extruder as in the example. After mixing, they were quantitatively supplied from the first raw material supply port and melt-kneaded to obtain a kneaded product for toner.
この混練時の操作条件は、実施例１と同様にバレルの
設定温度は100℃、スクリュー回転数は200rpmであり、
原料供給量は50kg/Hrであり、この混練による樹脂の出
口温度は205℃であった。The operating conditions during this kneading were that the barrel temperature was 100 ° C. and the screw rotation speed was 200 rpm, as in Example 1.
The raw material supply rate was 50 kg / Hr, and the exit temperature of the resin by this kneading was 205 ° C.
本比較例で得られた混練物を冷却、固化した後、粉
砕、分級し、目的とする粒径の粉体に所定の処理を施し
トナー性能を評価したところ、樹脂の軟化点は118℃で
あり、樹脂の分子切断の程度を表す混練前後での軟化点
の差は20℃と実施例に比べて大きく、樹脂中への添加剤
の分散も不良であり、トナーとして好ましくないもので
あった。The kneaded product obtained in this Comparative Example was cooled and solidified, then pulverized and classified, and the powder having a target particle diameter was subjected to a predetermined treatment to evaluate the toner performance, and the softening point of the resin was 118 ° C. The difference in the softening point before and after kneading, which represents the degree of molecular cleavage of the resin, was 20 ° C., which was large compared to the examples, and the additive was not well dispersed in the resin, which was not preferable as a toner. .
比較例 ２ 実施例２と同一の装置を用いて、軟化点が132℃であ
るポリスチレン樹脂100部と、該ポリスチレン樹脂100部
に対してカーボンブラック７部、電荷制御剤2.5部及び
ワックス３部の原料粉体と、上記原料100部に対して10
部の次工程の粉砕・分級工程で得られる回収微粉を溶融
混練してトナー用混練物を得た。Comparative Example 2 Using the same apparatus as in Example 2, 100 parts of a polystyrene resin having a softening point of 132 ° C., and 7 parts of carbon black, 2.5 parts of a charge control agent and 3 parts of wax per 100 parts of the polystyrene resin were used. Raw material powder and 10 for 100 parts of the above raw material
Part fine powder obtained in the pulverization / classification step as the next step was melt-kneaded to obtain a kneaded product for toner.
本混練において、連続押し出し機の第１の原料供給口
から、ポリスチレン樹脂60部と、電荷制御剤2.5部及び
ワックス３部の粉体原料を予備混合した後、定量的に供
給し、第２の原料供給口からポリスチレン樹脂60部とカ
ーボンブラック７部の粉体原料を予備混合した後、定量
的に供給し、第３の原料供給口から回収微粉10部を定量
的に供給することにより連続混練を行った。In this kneading, 60 parts of the polystyrene resin, 2.5 parts of the charge control agent and 3 parts of the wax were pre-mixed from the first material supply port of the continuous extruder and then quantitatively supplied to the second material. 60 parts polystyrene resin and 7 parts carbon black powder raw materials are premixed from the raw material supply port, then quantitatively supplied, and 10 parts of recovered fine powder are quantitatively supplied from the third raw material supply port to continuously knead. I went.
この混練時の操作条件は、バレルの設定温度は100
℃、スクリュー回転数は200rpmであり、原料供給量は第
１の原料供給口へは23.8kg/Hr、第２の原料供給口へは1
7.1kg/Hr、第３の原料供給口へは4.1kg/Hrであり、合計
45kg/Hrであった。The operating conditions during this kneading are that the barrel set temperature is 100
℃, the screw rotation speed is 200 rpm, the raw material supply rate is 23.8kg / Hr to the first raw material supply port, 1 to the second raw material supply port
7.1 kg / Hr, 4.1 kg / Hr to the third raw material supply port, total
It was 45 kg / Hr.
また、この混練による樹脂出口温度は198℃であっ
た。The resin outlet temperature by this kneading was 198 ° C.
この結果得られた混練物を冷却、固化した後、粉砕、
分級し、目的とする粒径の粉体に所定の処理を施しトナ
ー性能を評価したところ、樹脂の軟化点は123℃であ
り、樹脂の分子切断の程度を表す混練前後での軟化点の
差は９℃と小さいが、樹脂中への添加剤の分散が不良で
ありトナーとして好ましくないものであった。The kneaded product obtained as a result is cooled and solidified, and then pulverized,
When the toner performance was evaluated by classifying and subjecting the powder having the target particle diameter to a predetermined treatment, the softening point of the resin was 123 ° C., and the difference in the softening point before and after the kneading showing the degree of molecular breakage of the resin was shown. Was as small as 9 ° C., but the dispersion of the additive in the resin was poor, which was not preferable as a toner.
第１図は本発明のトナーの連続製造方法の一例を示すフ
ローシートであり、第２図は本発明に用いられる混練押
し出し機の一例を示す断面略示図、第３図は第２図の２
軸押し出し機のＡ−Ａ線断面図である。 １……原料計量器 ２……予備混合機 ３……原料供給装置 ４……入口側から0.3L以内の位置に設けられた原料供給
口 ４′……入口側から0.3L〜0.9Lの位置に設けられた原料
供給口 ５……混練押し出し機 ６……混練押し出し機外筒部冷却装置 ７……混練物冷却機 ８……粉砕・分級機 ９……ジャケット 10……脱気孔 11……バレル 12……スクリュー 13……スクリュー谷部 14……スクリュー山部FIG. 1 is a flow sheet showing an example of the toner continuous production method of the present invention, FIG. 2 is a schematic sectional view showing an example of a kneading extruder used in the present invention, and FIG. Two
It is the sectional view on the AA line of an axial extruder. 1 ... Raw material meter 2 ... Preliminary mixer 3 ... Raw material supply device 4 ... Raw material supply port provided within 0.3L from inlet side 4 '... Position from 0.3L to 0.9L from inlet side Raw material supply port 5 …… Kneading extruder 6 …… Kneading extruder External cylinder cooling device 7 …… Kneading material cooler 8 …… Grinding / classifying machine 9 …… Jacket 10 …… Deaeration hole 11 …… Barrel 12 …… Screw 13 …… Screw trough 14 …… Screw crest
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭62−78570（ＪＰ，Ａ) 特開 昭62−30259（ＪＰ，Ａ) 特開 昭61−50624（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of front page (56) References JP 62-78570 (JP, A) JP 62-30259 (JP, A) JP 61-50624 (JP, A)
Claims (2)
し、冷却、固化、粉砕し、分級してトナーを製造する方
法において、押し出し流れ性を有するバレル長さＬの混
練押し出し機の入口側から0.3L以内の位置に設けられた
少なくとも１個所の原料供給口から樹脂中の添加剤濃度
（以下前半部添加剤濃度という）が10〜50重量％の混合
原料を連続的に供給し、入口側から0.3L〜0.9Lの位置に
設けられた１〜５個所の原料供給口から樹脂単独もしく
は樹脂中の添加剤濃度が20重量％以下でかつ上記前半部
添加剤濃度より低い濃度の原料を連続的に供給し、かつ
0.3L以内の位置の原料供給口に供給する原料と0.3L〜0.
9Lの位置の原料供給口に供給する原料との供給流量の比
を10:1〜1:5（重量比）にすると共に、混練押し出し機
出口から混練物を連続的に取り出すことを特徴とするト
ナーの連続製造方法。1. A method for producing a toner by melt-kneading a composition comprising a resin and an additive, cooling, solidifying, pulverizing and classifying the composition, and an inlet of a kneading extruder having a barrel length L and having extrusion flowability. From at least one raw material supply port provided at a position within 0.3L from the side, the mixed raw material having an additive concentration in the resin (hereinafter referred to as the first half additive concentration) of 10 to 50 wt% is continuously supplied, Raw material having a concentration of 20% by weight or less of the resin alone or a concentration lower than the concentration of the above-mentioned first half additive from 1 to 5 raw material supply ports provided at positions 0.3L to 0.9L from the inlet side Continuously supplied, and
Raw material supplied to the raw material supply port located within 0.3L and 0.3L ~ 0.
The ratio of the supply flow rate to the raw material supplied to the raw material supply port at the 9L position is set to 10: 1 to 1: 5 (weight ratio), and the kneaded product is continuously taken out from the kneading extruder outlet. Continuous toner manufacturing method.
し、冷却、固化、粉砕し、分級してなるトナーであっ
て、押し出し流れ性を有するバレル長さＬの混練押し出
し機の入口側から0.3L以内の位置に設けられた少なくと
も１個所の原料供給口から樹脂中の添加剤濃度（以下前
半部添加剤濃度という）が10〜50重量％の混合原料を連
続的に供給し、入口側から0.3L〜0.9Lの位置に設けられ
た１〜５個所の原料供給口から樹脂単独もしくは樹脂中
の添加剤濃度が20重量％以下でかつ上記前半部添加剤濃
度より低い濃度の原料を連続的に供給し、かつ0.3L以内
の位置の原料供給口に供給する原料と0.3L〜0.9Lの位置
の原料供給口に供給する原料との供給流量の比を10:1〜
1:5（重量比）にすると共に、混練押し出し機出口から
混練物を連続的に取り出し、冷却、固化、粉砕し、分級
してなることを特徴とするトナー。2. A toner obtained by melt-kneading a composition comprising a resin and an additive, cooling, solidifying, crushing, and classifying the composition, which is an inlet side of a kneading extruder having a barrel length L and having extrusion flowability. At least one raw material supply port provided within 0.3 L from the above continuously supplies the mixed raw material with the additive concentration in the resin (hereinafter referred to as the first half additive concentration) of 10 to 50% by weight to the inlet. From 1 to 5 raw material supply ports provided at positions of 0.3L to 0.9L from the side, a raw material having a concentration of 20% by weight or less of the resin alone or a concentration lower than the concentration of the additive in the first half is supplied. The ratio of the supply flow rate between the raw material supplied to the raw material supply port located within 0.3L and the raw material supplied to the raw material supply port located within 0.3L to 0.9L is 10: 1 to
A toner characterized in that the kneaded product is continuously taken out from the kneading extruder outlet, cooled, solidified, pulverized, and classified while being set to 1: 5 (weight ratio).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1289162A JP2677685B2 (en) | 1989-11-07 | 1989-11-07 | Continuous toner manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1289162A JP2677685B2 (en) | 1989-11-07 | 1989-11-07 | Continuous toner manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03149567A JPH03149567A (en) | 1991-06-26 |
| JP2677685B2 true JP2677685B2 (en) | 1997-11-17 |
Family
ID=17739563
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1289162A Expired - Fee Related JP2677685B2 (en) | 1989-11-07 | 1989-11-07 | Continuous toner manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2677685B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150013636A (en) | 2012-05-02 | 2015-02-05 | 가부시키가이샤 리코 | Particles and method for producing particles |
| US9611376B2 (en) | 2012-11-13 | 2017-04-04 | Ricoh Company, Ltd. | Method for producing particles and apparatus for producing particles |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6232030B1 (en) | 1998-09-01 | 2001-05-15 | Kao Corporation | Toner manufacturing method |
| JP2010055019A (en) * | 2008-08-29 | 2010-03-11 | Sanyo Chem Ind Ltd | Toner composition |
| US8524437B2 (en) | 2011-03-04 | 2013-09-03 | Ricoh Company, Ltd. | Particle producing method, particle, toner, developer, process cartridge, image forming method, image forming apparatus, and particle producing method |
| JP6205116B2 (en) * | 2012-10-25 | 2017-09-27 | 花王株式会社 | Method for producing toner for developing electrostatic image |
| JP6256094B2 (en) * | 2013-03-25 | 2018-01-10 | 三菱ケミカル株式会社 | Method for producing toner for developing electrostatic image |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4973439A (en) * | 1984-07-13 | 1990-11-27 | Xerox Corporation | Process for preparing toner particles |
| JPS6230259A (en) * | 1985-07-31 | 1987-02-09 | Mita Ind Co Ltd | Manufacture of toner |
| JPS6278570A (en) * | 1985-10-01 | 1987-04-10 | Hitachi Chem Co Ltd | Production of toner for developing electrostatic charge image |
-
1989
- 1989-11-07 JP JP1289162A patent/JP2677685B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150013636A (en) | 2012-05-02 | 2015-02-05 | 가부시키가이샤 리코 | Particles and method for producing particles |
| US9669565B2 (en) | 2012-05-02 | 2017-06-06 | Ricoh Company, Ltd. | Particles and method for producing particles |
| US9611376B2 (en) | 2012-11-13 | 2017-04-04 | Ricoh Company, Ltd. | Method for producing particles and apparatus for producing particles |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03149567A (en) | 1991-06-26 |
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