JP2009134141A - 二軸押出型混練装置の洗浄方法 - Google Patents
二軸押出型混練装置の洗浄方法 Download PDFInfo
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- JP2009134141A JP2009134141A JP2007310996A JP2007310996A JP2009134141A JP 2009134141 A JP2009134141 A JP 2009134141A JP 2007310996 A JP2007310996 A JP 2007310996A JP 2007310996 A JP2007310996 A JP 2007310996A JP 2009134141 A JP2009134141 A JP 2009134141A
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- Prior art keywords
- cleaning
- resin composition
- washing
- kneading apparatus
- elastic modulus
- Prior art date
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Abstract
【解決手段】結着樹脂及び着色剤を含むトナー原料を溶融混練するための二軸押出型混練装置の洗浄方法であって、180℃における貯蔵弾性率が1.0×104〜4.0×104Paである洗浄樹脂組成物を用いて混練装置内を洗浄する第1洗浄工程、及び第1洗浄工程後、第1洗浄工程で用いた洗浄樹脂組成物より貯蔵弾性率の高い洗浄樹脂組成物を用いて混練装置内を洗浄する第2洗浄工程を含む、二軸押出型混練装置の洗浄方法。
【選択図】なし
Description
で表されるビスフェノールのアルキレンオキサイド付加物等の芳香族ジオール、エチレングリコール、1,2-プロパンジオール、1,3-プロパンジオール、1,4-ブタンジオール、1,5-ペンタンジオール、1,6-ヘキサンジオール、1,4-ブテンジオール、1,3-ブタンジオール、ネオペンチルグリコール等の脂肪族ジオール、グリセリン等の3価以上の多価アルコール等が挙げられる。
フローテスター(島津製作所、CFT-500D)を用い、1gの試料を昇温速度6℃/分で加熱しながら、プランジャーにより1.96MPaの荷重を与え、直径1mm、長さ1mmのノズルから押出する。温度に対し、フローテスターのプランジャー降下量をプロットし、試料の半量が流出した温度を軟化点とする。
示差走査熱量計「DSC210」(セイコー電子工業(株)製)を用いて200℃まで昇温し、その温度から降温速度10℃/分で0℃まで冷却したサンプルを昇温速度10℃/分で昇温し、吸熱の最高ピーク温度以下のベースラインの延長線とピークの立ち上がり部分からピークの頂点までの最大傾斜を示す接線との交点の温度とする。
JIS K0070の方法に基づき測定する。但し、測定溶媒のみJIS K0070の規定のエタノールとエーテルの混合溶媒から、アセトンとトルエンの混合溶媒(アセトン:トルエン=1:1(容量比))に変更した。
粘弾性測定装置(レオメーター)ARES(TA社製)を用いて測定を行う。測定装置の条件については下記の通り設定する。
Diameter = 25.0 [mm]
Gap = 1.5〜2.5 [mm]
Read Test Fixture Gap = On
Tool Serial Num = 0000
Tool Inertia = 58.0 [g・cm2]
Change Gap to Match Tool Thermal Expansion = Off
Tool Thermal Expansion Coefficient = 2.3 [μm/℃]
Fluid Density = 1.0 [g/cm3]
Fixture Compliance = 0.524 [μrad/g-cm]
------------------------------------
Test Type = Dynamic Temperature Ramp (DTempRamp)
Frequency = 6.28 [rad/s]
Initial Temp. = 200.0 [℃]
Final Temp. = 150.0, 200.0, 0.0, 0.0, 0.0, 0.0, 0.0, 0.0 [℃]
Ramp Rate = 20.0, 5.0, 0.0, 0.0, 0.0, 0.0, 0.0, 0.0 [℃/min.]
Computed Ramp Time = 2:30, 10:00, 0, 0, 0, 0, 0, 0 [h:m:s]
Soak Time After Ramp = 300, 0, 0, 0, 0, 0, 0, 0 [s or h:m:s]
Time Per Measure = 24, 12, 0, 0, 0, 0, 0, 0 [s or h:m:s]
Strain = 0.05, 0.05, 0.0, 0.0, 0.0, 0.0, 0.0, 0.0 [%]
Computed Test Duration = 17:30 [h:m:s]
Zone Time = 450, 10:00, 0, 0, 0, 0, 0, 0 [s or h:m:s]
Options = ElectroRheology
Steady PreShear = Off
PreShear Mode = Preshear Off
Delay Before Test = Off
Automatically start test when on Temperature = Off
AutoTension Adjustment = On
Mode = Apply Constant Static Force
AutoTension Direction = Compression
Initial Static Force = 10.0 [g]
AutoTension Sensitivity = 10.0 [g]
When Sample Modulus < = 100.0 [Pa]
AutoTension Limits = Default
Max Autotension Displacement = 3.0 [mm]
Max Autotension Rate = 0.01 [mm/s]
AutoStrain = On
Max Applied Strain = 20.0 [%]
Max Allowed Torque = 300.0 [g-cm]
Min Allowed Torque = 1.0 [g-cm]
Strain Adjustment = 20.0 [% of Current Strain]
Strain Amplitude Control = Default Behavior
Limit Minimum Dynamic Force Used = No
Minimum Applied Dynamic Force = 1.0 [gmf]
Measurement Options = Default Delay Settings
Cycles = 0.5
Time = 3 [s or h:m:s]
Correlation: One Cycle Correlate = Off
ElectroRheology Mode = Off
Turn OFF Motor = No
Turn Hold ON = Yes
Turn OFF Temp Controller = No
Set End of Test Temp = Yes
Set End of Test Temp to: = 200.0 [℃]
Oven Air/N2 Switch = Force Air
Dielectric Testing = Off
Steady Stress on Dynamic = 0.0 [Pa]
Analog Data Collection = Off
External Correlation = Off
Measurement Time = 1.0 [s]
Correlation Cycles = 1
Enable External Trigger = Off
Delay before initial trigger = 5.0 [s]
Trigger On Time = 2.0 [s]
Trigger Off Time = 2.0 [s]
Number of On/Off Cycles = 1
ポリオキシプロピレン(2.2)-2,2-ビス(4-ヒドロキシフェニル)プロパン1040g、ポリオキシエチレン(2.0)-2,2-ビス(4-ヒドロキシフェニル)プロパン10g、テレフタル酸199g、及び酸化ジブチル錫(エステル化触媒)4gを窒素雰囲気下、常圧、230℃で5時間反応させた後、さらに減圧下(70kPa)で反応させた。温度を210℃に冷却し、フマル酸209g及びハイドロキノン1gを加え、5時間反応した後にさらに減圧下(70kPa)で反応させて樹脂Aを得た。得られた樹脂の軟化点は107.5℃、酸価は21.3mgKOH/g、ガラス転移点は64.4℃であった。
結着樹脂として樹脂A 100重量部、荷電制御剤「ボントロン E-81」(オリエント化学社製)1重量部、シアン顔料「ECB-301」(大日精化工業社製、銅フタロシアニン顔料)5重量部及びポリプロピレンワックス「NP-055」(三井化学社製)2重量部をヘンシェルミキサーにて60秒間混合し、シアントナー原料混合物を得た。
着色剤として、シアン顔料の代わりに、イエロー顔料「Toner Yellow HG」(クラリアント社製)5重量部を使用した以外は、シアントナー原料混合物と同様にしてイエロートナー原料混合物を得た。
シアントナー原料混合物40kgを、押出機の温度を100℃、スクリューの回転数を100r/minに設定した二軸押出機「PCM-43」(池貝社製)に供給し、溶融混練した。
2)励起条件
ターゲット:Rh
管電流:50mA
管電圧:50mV
一次フィルタ:OUT
3)光学系条件
アテネーター:1/1
スリット:COARSE
分光結晶:LiF
検出器:SC
試料マスク径:30mmφ
4)スキャン条件
スペクトル:Cu-Kα
ピーク(deg):45.0
開始(deg):43
終了(deg):47
ステップ(deg):0.02
スキャン速度(deg/min):30
シアントナー原料混合物の溶融混練と、押出機内の乾拭きとの間に、表1に示す洗浄樹脂組成物を使用した洗浄工程を行った以外は、実施例1と同様にして、二軸押出機を洗浄し、イエロートナー原料混合物の溶融混練物中の銅の含有量を測定した。結果を表1に示す。
Claims (5)
- 結着樹脂及び着色剤を含むトナー原料を溶融混練するための二軸押出型混練装置の洗浄方法であって、180℃における貯蔵弾性率が1.0×104〜4.0×104Paである洗浄樹脂組成物を用いて混練装置内を洗浄する第1洗浄工程、及び第1洗浄工程後、第1洗浄工程で用いた洗浄樹脂組成物より貯蔵弾性率の高い洗浄樹脂組成物を用いて混練装置内を洗浄する第2洗浄工程を含む、二軸押出型混練装置の洗浄方法。
- 第2洗浄工程で用いる洗浄樹脂組成物と第1洗浄工程で用いる洗浄樹脂組成物の180℃における貯蔵弾性率の比(第2洗浄工程で用いる洗浄樹脂組成物の180℃における貯蔵弾性率/第1洗浄工程で用いる洗浄樹脂組成物の180℃における貯蔵弾性率)が、1.1〜20である、請求項1記載の洗浄方法。
- 第2洗浄工程後、さらに、第2洗浄工程で用いる洗浄樹脂組成物より貯蔵弾性率の低い洗浄樹脂組成物を用いて混練装置内を洗浄する第3洗浄工程を含む、請求項1又は2記載の洗浄方法。
- 結着樹脂がポリエステルを含有する、請求項1〜3いずれか記載の洗浄方法。
- 各洗浄工程における二軸押出型混練装置の設定温度が160〜210℃である、請求項1〜4いずれか記載の洗浄方法。
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