JP5151119B2 - ビスフェノールaの製造方法 - Google Patents
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- JP5151119B2 JP5151119B2 JP2006312765A JP2006312765A JP5151119B2 JP 5151119 B2 JP5151119 B2 JP 5151119B2 JP 2006312765 A JP2006312765 A JP 2006312765A JP 2006312765 A JP2006312765 A JP 2006312765A JP 5151119 B2 JP5151119 B2 JP 5151119B2
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/11—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms
- C07C37/20—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms using aldehydes or ketones
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0242—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical
- B01J8/025—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical in a cylindrical shaped bed
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
- B01J8/40—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed subjected to vibrations or pulsations
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C39/00—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring
- C07C39/12—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring polycyclic with no unsaturation outside the aromatic rings
- C07C39/15—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a six-membered aromatic ring polycyclic with no unsaturation outside the aromatic rings with all hydroxy groups on non-condensed rings, e.g. phenylphenol
- C07C39/16—Bis-(hydroxyphenyl) alkanes; Tris-(hydroxyphenyl)alkanes
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00026—Controlling or regulating the heat exchange system
- B01J2208/00035—Controlling or regulating the heat exchange system involving measured parameters
- B01J2208/00044—Temperature measurement
- B01J2208/00061—Temperature measurement of the reactants
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00477—Controlling the temperature by thermal insulation means
- B01J2208/00495—Controlling the temperature by thermal insulation means using insulating materials or refractories
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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/0061—Controlling the level
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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00654—Controlling the process by measures relating to the particulate material
- B01J2208/00681—Agglomeration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00884—Means for supporting the bed of particles, e.g. grids, bars, perforated plates
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00191—Control algorithm
- B01J2219/00193—Sensing a parameter
- B01J2219/00195—Sensing a parameter of the reaction system
- B01J2219/00198—Sensing a parameter of the reaction system at the reactor inlet
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00191—Control algorithm
- B01J2219/00193—Sensing a parameter
- B01J2219/00195—Sensing a parameter of the reaction system
- B01J2219/002—Sensing a parameter of the reaction system inside the reactor
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00191—Control algorithm
- B01J2219/00193—Sensing a parameter
- B01J2219/00195—Sensing a parameter of the reaction system
- B01J2219/00202—Sensing a parameter of the reaction system at the reactor outlet
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00191—Control algorithm
- B01J2219/00222—Control algorithm taking actions
- B01J2219/00227—Control algorithm taking actions modifying the operating conditions
- B01J2219/00229—Control algorithm taking actions modifying the operating conditions of the reaction system
- B01J2219/00231—Control algorithm taking actions modifying the operating conditions of the reaction system at the reactor inlet
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/08—Ion-exchange resins
- B01J31/10—Ion-exchange resins sulfonated
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- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Description
図1に示す竪型固定床反応器を使用した。反応器1の底面の半径は2.8mで、触媒層高・が3.25m(触媒量:80m3)となる様に、スルホン酸基の15%が2−(4−ピリジル)エタンチオールで変性されたスルホン酸型陽イオン交換樹脂触媒を充填した。触媒層内には、熱電対温度計5を2箇所設置した。設置箇所は、図1に示す様に、触媒層の水平方向において、反応器の外周からの距離rが250cmの同じ位置であり、高さ方向に触媒層の最低面から15cm(触媒層の最低面から5%:測定点1=図中符号52)及び47cm(触媒層の最低面から14%:測定点2=図中符号53)であった。さらに、反応器の出口付近に熱電対温度計6を設置した(測定点0=図中符号51)。図1に示す様に、竪型固定床反応器1は、バルブ81〜84を使用して反応液の流通方向を逆転することが出来、最小流動化供給量は13.5t/hであった。
運転開始から12ヶ月経過した時点での反応の停止および触媒の流動操作を行わず、運転を継続した他は、実施例1と同様の操作を行った。最初に反応を開始してから24ヶ月経過した時点での測定点1の温度は71.9℃、測定点2の温度は71.9℃、反応器出口(測定点0)の温度は65.9℃であった。すなわち、測定点1と測定点0との温度差は6.0℃、測定点2と測定点0との温度差は6.0℃であった。この時点における。アセトン転化率は64.0%であった。
図1に示す竪型固定床反応器と基本的な構造が同一の反応器を使用した。反応器1の底面の半径は3.3mで、触媒層高・が3.2m(触媒量:110m3)となる様に、スルホン酸基の15%が2−(4−ピリジル)エタンチオールで変性されたスルホン酸型陽イオン交換樹脂触媒を充填した。触媒層内には、熱電対温度計5を2箇所設置した。設置箇所は、触媒層の水平方向において、反応器の外周からの距離rが300cmの同じ位置であり、高さ方向に触媒層の最低面から15cm(触媒層の最低面から5%:測定点1=図中符号52)及び47cm(触媒層の最低面から14%:測定点2=図中符号53)であった。竪型固定床反応器1は、バルブ81〜84を使用して反応液の流通方向を逆転することが出来、最小流動化供給量は18.8t/hであった。
運転開始から9ヶ月経過した時点での反応の停止および触媒の流動操作を行わず、運転を継続した他は、実施例2と同様の操作を行った。最初に反応を開始してから18ヶ月経過した時点での測定点1の温度は66.8℃、測定点2の温度は66.8℃、反応器出口(測定点0)の温度は72.4℃であった。すなわち、測定点1と測定点0との温度差は5.6℃、測定点2と測定点0との温度差は5.6℃であった。この時点における。アセトン転化率は61.0%であった。
2:断熱材
3:触媒支持部材
4:触媒層
5:熱電対
6:熱電対
7:ポンプ
51:測定点0
52:測定点1
53:測定点2
Claims (2)
- イオン交換樹脂触媒を充填した竪型固定床反応器にフェノ−ル原料とアセトン原料とを流通させ、ビスフェノールA含有反応液を得る反応工程を包含するビスフェノールAの製造方法であって、当該反応器内に形成されたイオン交換樹脂触媒層の出口から触媒層高20%以内の範囲にある何れかの位置における反応液の温度と、固定床反応器の出口における反応液の温度との温度差(ΔT)の絶対値が、1.0〜5.0℃である際に、イオン交換樹脂触媒の少なくとも一部を流動させることを特徴とするビスフェノールAの製造方法。
- 竪型固定床反応器に上昇流で流体を供給することによりイオン交換樹脂触媒の流動を行う請求項1に記載のビスフェノールAの製造方法。
Priority Applications (1)
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JP2006312765A JP5151119B2 (ja) | 2005-11-21 | 2006-11-20 | ビスフェノールaの製造方法 |
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JP2005335795 | 2005-11-21 | ||
JP2005335795 | 2005-11-21 | ||
JP2006312765A JP5151119B2 (ja) | 2005-11-21 | 2006-11-20 | ビスフェノールaの製造方法 |
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JP2007161709A JP2007161709A (ja) | 2007-06-28 |
JP5151119B2 true JP5151119B2 (ja) | 2013-02-27 |
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JP (1) | JP5151119B2 (ja) |
KR (1) | KR101095455B1 (ja) |
CN (1) | CN101309888B (ja) |
WO (1) | WO2007058234A1 (ja) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP5247184B2 (ja) * | 2008-02-21 | 2013-07-24 | 三井化学株式会社 | ビスフェノールaの製造方法 |
JP5559481B2 (ja) * | 2009-02-09 | 2014-07-23 | 川崎重工業株式会社 | カルマン渦による振動を利用したプロセス装置 |
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JP3350760B2 (ja) * | 1992-05-22 | 2002-11-25 | 月島機械株式会社 | 反応器およびビスフェノール類の製造法 |
CN1027638C (zh) * | 1993-02-17 | 1995-02-15 | 中国石油化工总公司 | 树脂法生产的2,2-二(4-羟基苯基)丙烷的方法 |
DE19957602A1 (de) * | 1999-11-30 | 2001-05-31 | Bayer Ag | Verfahren zur Inbetriebnahme eines Herstellungsverfahrens von 2,2-bis (4-hydroxyphenyl) propan |
PL201330B1 (pl) * | 2001-05-23 | 2009-03-31 | Edward Grzywa | Sposób otrzymywania bisfenolu A |
US6703530B2 (en) * | 2002-02-28 | 2004-03-09 | General Electric Company | Chemical reactor system and process |
US7141640B2 (en) * | 2002-10-08 | 2006-11-28 | General Electric Company | Process for producing dihydroxy compounds using upflow reactor system |
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2006
- 2006-11-16 WO PCT/JP2006/322817 patent/WO2007058234A1/ja active Application Filing
- 2006-11-16 CN CN200680043079XA patent/CN101309888B/zh active Active
- 2006-11-16 KR KR1020087011700A patent/KR101095455B1/ko active IP Right Grant
- 2006-11-20 JP JP2006312765A patent/JP5151119B2/ja active Active
Also Published As
Publication number | Publication date |
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CN101309888A (zh) | 2008-11-19 |
KR101095455B1 (ko) | 2011-12-19 |
JP2007161709A (ja) | 2007-06-28 |
WO2007058234A1 (ja) | 2007-05-24 |
KR20080069188A (ko) | 2008-07-25 |
CN101309888B (zh) | 2012-12-26 |
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