JP5836819B2 - 連続撹拌式槽型反応器 - Google Patents
連続撹拌式槽型反応器 Download PDFInfo
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- JP5836819B2 JP5836819B2 JP2012014227A JP2012014227A JP5836819B2 JP 5836819 B2 JP5836819 B2 JP 5836819B2 JP 2012014227 A JP2012014227 A JP 2012014227A JP 2012014227 A JP2012014227 A JP 2012014227A JP 5836819 B2 JP5836819 B2 JP 5836819B2
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- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000001508 potassium citrate Chemical class 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical class [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- 239000004224 potassium gluconate Chemical class 0.000 description 1
- 235000013926 potassium gluconate Nutrition 0.000 description 1
- 229960003189 potassium gluconate Drugs 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000012176 shellac wax Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229940087562 sodium acetate trihydrate Drugs 0.000 description 1
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 1
- 239000001509 sodium citrate Chemical class 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical class O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 229960001790 sodium citrate Drugs 0.000 description 1
- 235000011083 sodium citrates Nutrition 0.000 description 1
- 239000000176 sodium gluconate Chemical class 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- UZVUJVFQFNHRSY-OUTKXMMCSA-J tetrasodium;(2s)-2-[bis(carboxylatomethyl)amino]pentanedioate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CC[C@@H](C([O-])=O)N(CC([O-])=O)CC([O-])=O UZVUJVFQFNHRSY-OUTKXMMCSA-J 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
- GINSRDSEEGBTJO-UHFFFAOYSA-N thietane 1-oxide Chemical compound O=S1CCC1 GINSRDSEEGBTJO-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229940117957 triethanolamine hydrochloride Drugs 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/0802—Preparation methods
- G03G9/0804—Preparation methods whereby the components are brought together in a liquid dispersing medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/14—Treatment of polymer emulsions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/14—Treatment of polymer emulsions
- C08F6/18—Increasing the size of the dispersed particles
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Developing Agents For Electrophotography (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Colloid Chemistry (AREA)
Description
σp=mp/Vt
式中、mpは、乾燥トナー(生成物)の質量であり、Vは、反応器全体の容積であり、tは、反応器の合計滞留時間である。
式中、Rは、水素またはメチル基であってもよく、mおよびnは、コポリマーのランダム単位をあらわし、mは、2〜10であってもよく、nは、2〜10であってもよい。
式中、bは、5〜2000であり、dは、5〜2000である。
4リットルのプラスチックビーカーの中で、823グラムのアモルファスコアラテックス、140グラムの結晶性コアラテックス、2259グラムの脱イオン水(DIW)、3.2グラムのアルキルジフェニルオキシドジスルホネート界面活性剤(DOWFAXTM2A1、Dow Chemical Company製)、208グラムのシアン顔料(SUN製)、179グラムのポリエチレンワックス(IGI製)を混合した。次いで、このトナースラリーのpHを0.3M硝酸(HNO3)126グラムで4.2に調節した。この溶液を0℃まで冷却した。連続反応器への供給槽を満たすのに必要な場合、この様式でさらなる原料を作成した。
段階1:冷温添加
第1の段階10(冷温添加段階10としても知られる)において、第1の流れ2のAl2(SO4)3冷温供給物(0℃〜10℃)、第2の流れ4の種々の樹脂エマルション、ワックス分散物、着色剤分散物の混合物を連続反応器システム100にポンプで送り込んだ。反応器の壁面を、外側にある熱交換器(以下に記載)によって−10℃〜10℃の温度に維持した。この温度を5℃に設定した。第1の流れ2の材料および第2の流れ4の材料を反応器システム100にポンプで送り込むにつれて、これらの材料は、ある段階から次の段階へと、第1の段階と第2の段階(例えば、第1の凝集段階20)を分割しているオリフィス板6を通って上に移動した。オリフィス板6は、第1の段階10の材料と第2の段階20の材料が完全に混ざりあってしまうのを最低限にした。これにより、それぞれの段階が、確実に別個の連続撹拌式槽型反応器(CSTR)として作用した。それ以外の段階も、図1からわかるように、同様の様式でオリフィス板6によって分割されていた。冷温添加段階10において、軸330(図3を参照)を、毎分0〜600回転(rpm)の速度で回転させた。軸330には、第1の段階10で望ましい混合度を得るために必要なように設計変更されたインペラ310(図3を参照)が取り付けられた。
材料が第2の段階20(すなわち、第1の凝集段階)に入ると、外側にあるジャケットと、0℃〜50℃に設定された加熱浴22によって材料が加熱された。この温度を35℃に設定した。材料がこの反応器20に流れ込み、混ざりあっていくにつれて、対流および伝導による熱移動によって反応器の内壁からプロセス流に熱が移動した。この温度変化が引き金となってラテックスおよび分散物の凝集が始まり、平均直径が1μm〜20μmの粒子が生成した。
第2の段階20から出た材料は、オリフィス板6を通って第3の段階30(すなわち、第2の凝集段階30)へと流れ、この段階で、材料は、反応器ジャケットと接することによってさらに加熱され、第2の段階20の温度よりも1℃〜40℃高い温度が得られた。この温度を10℃高い温度である45℃に設定した。温度が高くなることによって、粒子が所定の大きさまでさらに成長した。
第3の段階30から出た材料は、オリフィス板6を通って第4の段階40(すなわち、シェル添加段階40)へと流れ、この段階で、新しいラテックス14がポンプで送り込まれ、前の段階10、20、30で生成した粒子の周りにシェルが生成した。第4の段階40のジャケット温度は、20〜60℃(45℃)であった。段階1から4の間、1個の軸330(図3を参照)が回転し、10、20、30、40のそれぞれの段階で内容物を撹拌した。インペラ310は、図3に示されているように、10、20、30、40のそれぞれの段階で望ましい撹拌が得られるように設計されていた。
第5の段階50において、水酸化ナトリウムまたは任意の他の適切な溶液(例えば、緩衝溶液24)をポンプで送り込み、粒子の成長を止めた。この水酸化ナトリウム溶液を、第4の段階40からオリフィス板6を通ってこの段階に入ってくる材料と混合した。凍結プロセスによって、最終的な用途にとって望ましい粒径が確実に得られた。この反応器のスラリー温度は、外側にあるジャケットおよび20〜60℃(45℃)に設定された加熱浴によって制御された。
第6の段階60において、キレート化溶液34を加え、粒子からイオンを除去した。このキレート化溶液は、エチレンジアミン四酢酸を含有する溶液および/またはコロイド状シリカを含有する溶液であった。キレート化溶液34を、第5の段階50からオリフィス板6を通ってこの段階に入ってくる材料と混合した。この反応器のスラリー温度は、外側にあるジャケットおよび20〜60℃(45℃)に設定された加熱浴32によって制御された。
第7の段階70において、ジャケットの温度は、外側にあるジャケットおよび加熱浴42によって制御され、40℃〜100℃(70℃)まで上昇し、第6の段階60および第7の段階70を分割しているオリフィス板6を通って入り込んでくる段階60のスラリーの温度が上がった。それに加えて、この反応器に水酸化ナトリウム溶液44を連続的に加え、pHを7〜9に制御した。
第8の段階80において、ジャケットの温度は、外側にあるジャケットおよび加熱浴52によって制御され、さらに50℃〜110℃(85℃)まで上昇し、第7の段階70および第8の段階80を分割しているオリフィス板6を通って入り込んでくるスラリーの温度が上がった。それに加えて、水酸化ナトリウム溶液または緩衝溶液54を加え、融着プロセスの速度を速めた。軸320(図3を参照)は、第5の段階50、第6の段階60、第7の段階70、第8の段階80で回転し、50、60、70、80のそれぞれの段階で内容物を撹拌した。
第8の段階80を出た材料は、槽90に集められ、その後に最終製品へと加工された。図2は、本開示の連続乳化凝集(EA)システムの三次元図200を示す。反応器システム100は、少なくとも2つの電動部210および少なくとも2つのポンプ220と動作可能なように連結していた。反応器システム200は、長さ方向に沿って、等距離の位置に複数の加熱ジャケット230を備えていた。さらに、反応器システム100は、複数のpHプローブ240を備えていた(図2および3を参照)。
Claims (8)
- 乳化凝集によって粒子を製造するための連続撹拌式槽型反応器であって、
凝集剤、樹脂エマルションを含む原材料供給槽と、
前記原材料供給槽から出た前記凝集剤及び前記樹脂エマルションの混合物を冷却するための少なくとも1つの第1反応器と、
前記第1反応器から出た混合物を加熱して、前記混合物を凝集させ、凝集粒子を形成するための少なくとも2つの第2反応器と、
前記第2反応器から出た混合物にラテックスを添加混合して、前記凝集粒子の周りにシェルを形成するための少なくとも1つの第3反応器と、
前記第3反応から出た混合物に緩衝液を添加混合して、前記凝集粒子の粒子成長を停止するための少なくとも1つの第4反応器と、
前記第4反応器から出た混合物にキレート化剤を添加混合するための少なくとも1つの第5反応器と、
前記第5反応器から出た混合物を加熱するための少なくとも1つの第6反応器と、
前記第6反応器から出た混合物をさらに加熱して、前記凝集粒子を融着させるための少なくとも1つの第7反応器と、を備え、
前記反応器が、直列の配置で連続的に整列され、隣接する反応器の間がオリフィス板で分割されている、連続撹拌式槽型反応器。 - 流体が、ポンプを用いることなく、正圧または負圧によって、ある反応器から次の反応器へと連続的に移動する、請求項1に記載の連続撹拌式槽型反応器。
- 各反応器は、外部から冷却デバイスまたは加熱デバイスを適用することによって温度が制御される、請求項1に記載の連続撹拌式槽型反応器。
- 粒径および粒径分布を制御するために、各反応器について独立した速度で材料を混合する、請求項1に記載の連続撹拌式槽型反応器。
- 反応器の温度が、材料が流れる方向に沿って段階的に高くなっている、請求項1に記載の連続撹拌式槽型反応器。
- 各反応器の滞留時間が0.5分〜60分である、請求項1に記載の連続撹拌式槽型反応器。
- 各反応器に塩基性溶液または酸性溶液を供給すると共に、前記塩基性溶液または前記酸性溶液を各反応器に供給する速度を変えることによって、各反応器でpHが制御され、前記pHが複数のpHプローブによって測定される、請求項1に記載の連続撹拌式槽型反応器。
- 各反応器が、前記反応器内の材料移動を助けるためのインペラを伴っている、請求項1に記載の連続撹拌式槽型反応器。
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US13/025,664 US8663565B2 (en) | 2011-02-11 | 2011-02-11 | Continuous emulsification—aggregation process for the production of particles |
US13/025,664 | 2011-02-11 |
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US20150104742A1 (en) * | 2013-10-11 | 2015-04-16 | Xerox Corporation | Emulsion aggregation toners |
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WO2015186710A1 (ja) * | 2014-06-04 | 2015-12-10 | 三菱化学株式会社 | 連続式反応装置及びトナーの製造装置 |
US10189004B2 (en) * | 2014-06-16 | 2019-01-29 | Bayer Aktiengesellschaft | Reaction chamber for a chemical reactor, and chemical reactor constructed therefrom |
US9464173B2 (en) * | 2014-12-16 | 2016-10-11 | Xerox Corporation | Latex preparation using an agitated reactor column |
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US8663565B2 (en) | 2014-03-04 |
EP2487544B1 (en) | 2016-01-20 |
KR20120092514A (ko) | 2012-08-21 |
CA2766716C (en) | 2016-05-24 |
MX2012001655A (es) | 2012-08-30 |
TW201238648A (en) | 2012-10-01 |
US20120208123A1 (en) | 2012-08-16 |
TWI561298B (en) | 2016-12-11 |
KR101798245B1 (ko) | 2017-11-15 |
JP2012166191A (ja) | 2012-09-06 |
BR102012003121B1 (pt) | 2019-10-29 |
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