CN1089026C - 一种设备及其用于氧氯化反应的用途 - Google Patents
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Abstract
在具有催化剂流化床下边界的反应器中由乙烯、氯化氢和氧或含氧的气体制备1,2-二氯乙烷(氧氯化反应),其中第一个气体入口管(分配管)(4)安装在边界上方和催化剂流化床中,其含有分布在整个反应器横截面上的喷嘴(5),喷嘴(5)开口于管(6)中,管(6)基本上以与流化催化剂的气流相反的方向引导所排出的气流,用于流化催化剂的气流通过边界下方的第二气体入口管(7)供给。
Description
“氧氯化”被理解为乙烯与氯化氢和氧气或含氧气体的反应,其中生成1, 2-二氯乙烷(EDC)。这里通常使用在EDC热裂解为氯乙烯时产生的氯化氢作为氯化氢。
此外,对于氧氯化使用在细粉末载体如氧化铝上含有金属卤化物,优选是氯化铜的催化剂。这里,催化剂颗粒的平均直径大约是50μm并且形成流化床,该流化床或者仅由反应气流(必要时含惰性气体组份)支持,或者另外还由循环气流支持。对于这种方法,反应热分布在流化床中和在一冷却面上被移去,这样可以在流化床反应器中得到均匀的温度分布。这里,催化剂颗粒必须具有高的耐磨性。通过载体材料基本上赋予这种性能,为此除了已经提到的氧化铝外;还使用硅酸、硅藻土或浮石。在耐磨性不足时,催化剂颗粒特别由气体入口装置喷射的气体磨碎,并且这样产生的催化剂载体粉尘通过向上流动的气体被排出氧氯化反应器。这不仅仅造成催化剂损失,而且提高了装置的磨耗。
另一方面,使用耐磨的载体材料伴随有气体导入设备的磨损增大,这样导致经常更换该设备,也意味着增加费用和附加的由生产中断造成的开支。
除了要使催化剂颗粒的稳定性和由此产生的磨损平衡外,还必须注意催化剂颗粒不能凝聚,因为由此造成的块结将导致流化床的破坏。结果是流化床中温度分布不均匀并伴随相应的不利的反应过程以及可能造成装置中狭窄部位的堵塞,例如在流化床上面的用于除尘的旋风分离器中或者用于将来自旋风分离器的灰尘再循环至流化床的垂直管中。除了催化剂的性质和其在催化剂载体上的分布外,结块的可能性特别与流化床中反应气体的浓度有关。
由W094/19099已知一种用于氧氯化的设备,其特征在于反应器1,用于流化床催化剂3的下边界2、包含喷嘴5的气体入口管(分配管)4和在边界2下面的气体入口管9,其中喷嘴5开口于管6中,管6使排出的气流在流动方向上具有水平的分支。
优选的实施例强调所提及的喷嘴开口于其中的管在端部包括具有流出口的转向装置,或者该管向上倾斜或在水平方向上或者向下倾斜和该管敞开着在催化剂床中终止,或者这些管或邻近的管的流出口这样布置,以使流出的喷射气体不会相互正面遭遇和/或不会碰到邻近的管。其它优选的实施例强调,管穿过边界,其中喷嘴布置在边界的下方,但在贯通的管的下端的上方,优选地该喷嘴安装在所涉及管的下半部,特别是从下端部到该喷嘴的距离大约为该管的直径。
EP-A-0446 379公开了用于制备α-β-不饱和腈的反应器,在反应器的较低部位设置了用于烯烃或叔丁醇的水平安置的气体进料管,在气体进料管的下侧设有许多喷嘴,还在下面与该气体进料管道平行设有另一用于含氧气体的进料管道。两个气体进料管道之间的距离为25-300mm。太短的距离会因不正常反应而引起熔化所造成的气体进料管的损坏,而距离太大则烯烃或叔丁醇未能与含氧气体充分混合,这导致降低腈的产率。
GB-A-1265770公开了用于流化床反应的反应器,在该反应器的较低部位设有分配板;在该板下设一气体进料管并且在反应器壳附近的外部区域在紧邻分配板之上设有另一气体进料管。该另一气体进料管防止催化剂在外部区域沉降。这一防护措施尤其用于防止催化剂减少。在流化床内可设置另一气体进料管,该进料管设在反应器较低部位以在流化床底部的反应物充分混合。
已经发现,在长期运转和高的通过量下,也是说在高的气流速度下,该已知设备表现出在气体入口设备中一定的磨损。另外令人惊奇地发现,如果喷嘴开口于其中的管以与保持催化剂为流化床形式的气流相反的方向引导排出气流,那么这种磨损不存在或仅在相对小的程度上发生。
因此,本发明涉及用于氧氯化的装置,其包括:
-反应器1,
-催化剂流化床3的下边界2
-在边界2上方和在催化剂流化床之内的气体入口管(分配管)4,该气体入口管包含分布在反应器1整个横截面上的喷嘴5,
-喷嘴5开口于管6中,该管6基本上以与使催化剂流化的气流逆流的方向引导排出的气流,以及
-气流入口管7在边界2的下方。
本发明的装置有利地是这样设计,即一定数目的管8与相同数目的管6相对并均匀分布在反应器横截面上。通过各管8和6的分别定位可以适中地分配来自于管8和6的相互反应气体的量。
在另一个本发明的设备的实施方案中,以交错的方式相对安装相同数目的管8和6。这种几何图形尽可能减小通过来自管8的上升气流对管6的磨损:此外,借助于这种布置可以实现,来自管8和6进入催化剂流化床3的反应产物立即与催化剂紧密地接触。因此,有利于所希望的朝着形成EDC的方向进行的反应和抑制了副反应,例如乙烯与氧的燃烧。
该设备的另一个实施方案对它的配置和结构允许有较大的自由度。其中管6的数目与管8的数目不同。然而,在这种情况下,重要的是这些管尽可能均匀地布置在反应器1的横截面上。这种形式产生这种可能性,即改变现存的反应器中的管6的数目,而不必同时调整管8,同时调整管8意味着高的费用。
在下面的实施例中进一步详细地说明本发明。
实施例
使用图1的装置。在直径2.8m和高26m的反应器1中加入气态的预热至160℃的反应物。5974kg/h的氯化氢和1417kg/h的氧气的混合物通过气体入口管4经过喷嘴5和管6进入催化剂流化床3。喷嘴5具有不同的尺寸,以使在所有喷嘴5上得到尽可能均匀的气体分布和由此在整个反应器1横截面上得到尽可能均匀的气体分布。为了补偿沿着气体入口管直到各自的喷嘴5的不同的压力损失,顺着气体入口管4的下流方向喷嘴5的直径从8.6mm增大到9.3mm和进一步增加到10mm。内径为40mm的管6的长度为300mm。2380kg/h的乙烯经过气体入口管7和带有喷嘴9的管8流过下边界2。在反应器1中,在氧化铝载体上的氯化铜(II)以催化剂流化床3的形式作为催化剂存在。将上面所提到的反应物加到流化床中。为了流化床的流化,使另外的8780kg/h的循环气流经过气体入口管7和管8流过下边界2进入反应器1中。管8的上端与下边界2齐平。下边界和管6下端的距离为400mm。在这区域中,反应物被分布在反应器整个横截面上,并且在单个反应物和催化剂之间形成混合区。乙烯和循环气体从下向上流入反应器中。在该方向上它与氯化氢和氧气相遇并在所存在的催化剂的共同作用下反应生成EDC和水。所形成的238.5kJ/mol的反应热经过催化剂流化床3转移到蛇形冷却管12中,在这里水在183℃被蒸发。在反应器中,在3.2巴的压力下反应温度为225℃。在反应器的上部由反应产物和循环气体组成的气流经过三个旋风分离器离开反应器1至进一步的加工步骤(图中没有示出)中。三个顺序连接的旋风分离器用于从催化剂流化床上方的反应器顶部的气流中分离出被夹带的催化剂尘粒。
Claims (8)
1.用于氧氯化的设备,其特征在于:
-反应器(1),
-催化剂流化床(3)的下边界(2),
-在边界(2)上面和催化剂流化床(3)内的气体入口管,即分配管(4),它包含分布在整个反应器(1)横截面上的喷嘴(5),
-其中,喷嘴(5)开口于管(6)中,管(6)基本上以与流化催化剂的气流逆流的方向引导所排出的气流和
-气体入口管(7)在边界(2)的下方,和
-管(8)穿过边界(2),
-在穿过边界(2)的管(8)上端和喷嘴(5)开口于其中的管(6)的下端之间的空间形成一个这么大的混合区,以使从这些管出来的反应物与催化剂在这里就已发生混合,25-300mm的混合区除外。
2.根据权利要求1的设备,其特征是在管(8)中喷嘴(9)安装在边界(2)的下方但在管(8)的下端的上方。
3.根据权利要求2的设备,其特征是,将喷嘴(9)布置在离管(8)的上端这样长的距离上,以便从喷嘴(9)喷射的气体向上的流动速度直到管(8)的上端在每个管(8)的各自的横截面上是均匀的。
4.根据权利要求3的设备,其特征是,喷嘴(9)安装在距离管(8)的下端大约为管(8)直径的地方。
5.根据权利要求1的设备,其特征是,管(6)的长度是这么长,以使从喷嘴(5)喷射的气体向下的流动速度直到管(6)的下端在每个管(6)各自的横截面上是均匀的。
6.根据权利要求1~5之任一项的设备,其特征是,喷嘴(5)具有不同的直径,以使通过气体入口管(4)导入的气体量均匀地分布在反应器(1)的横截面上。
7.根据权利要求1~5之任一项的设备,其特征是,在管(8)的上端和管(6)的下端之间的空间的尺寸这么大,以使不再导致管(4、6、8)以及下边界(2)的高的相互磨蚀应力。
8.根据权利要求1~7之任一项的设备的用途,用于乙烯与氯化氢和氧或一种含氧的气体反应得到1,2-二氯乙烷。
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DE19505664.7 | 1995-02-20 | ||
DE19505664A DE19505664C2 (de) | 1995-02-20 | 1995-02-20 | Vorrichtung und ihre Verwendung zur Oxichlorierung |
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CN1089026C true CN1089026C (zh) | 2002-08-14 |
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EP (1) | EP0810902B1 (zh) |
JP (1) | JPH11500062A (zh) |
KR (1) | KR100368512B1 (zh) |
CN (1) | CN1089026C (zh) |
AU (1) | AU702305B2 (zh) |
BG (1) | BG62436B1 (zh) |
BR (1) | BR9510383A (zh) |
CA (1) | CA2213446C (zh) |
CZ (1) | CZ289342B6 (zh) |
DE (2) | DE19505664C2 (zh) |
ES (1) | ES2126296T3 (zh) |
HU (1) | HU221883B1 (zh) |
IN (1) | IN188066B (zh) |
NO (1) | NO973714L (zh) |
PL (1) | PL180784B1 (zh) |
RO (1) | RO118119B1 (zh) |
RU (1) | RU2157726C2 (zh) |
SK (1) | SK282850B6 (zh) |
UA (1) | UA42056C2 (zh) |
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WO1994019099A1 (de) * | 1993-02-18 | 1994-09-01 | Hoechst Aktiengesellschaft | Vorrichtung zur oxichlorierung |
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GB1265770A (zh) * | 1969-07-01 | 1972-03-08 | ||
US4801731A (en) * | 1987-12-14 | 1989-01-31 | E. I. Du Pont De Nemours And Company | Preparation of acrylonitrile |
DE9116161U1 (zh) * | 1991-12-07 | 1992-03-26 | Hoechst Ag, 6230 Frankfurt, De |
-
1995
- 1995-02-20 DE DE19505664A patent/DE19505664C2/de not_active Expired - Fee Related
- 1995-05-17 BR BR9510383A patent/BR9510383A/pt not_active IP Right Cessation
- 1995-05-17 JP JP8525326A patent/JPH11500062A/ja not_active Ceased
- 1995-05-17 UA UA97094673A patent/UA42056C2/uk unknown
- 1995-05-17 KR KR1019970705738A patent/KR100368512B1/ko not_active IP Right Cessation
- 1995-05-17 RO RO97-01537A patent/RO118119B1/ro unknown
- 1995-05-17 ES ES95924203T patent/ES2126296T3/es not_active Expired - Lifetime
- 1995-05-17 DE DE59504023T patent/DE59504023D1/de not_active Expired - Fee Related
- 1995-05-17 AU AU28810/95A patent/AU702305B2/en not_active Ceased
- 1995-05-17 SK SK1134-97A patent/SK282850B6/sk unknown
- 1995-05-17 WO PCT/EP1995/001874 patent/WO1996026003A1/de active IP Right Grant
- 1995-05-17 HU HU9801625A patent/HU221883B1/hu not_active IP Right Cessation
- 1995-05-17 RU RU97116001/12A patent/RU2157726C2/ru not_active IP Right Cessation
- 1995-05-17 EP EP95924203A patent/EP0810902B1/de not_active Expired - Lifetime
- 1995-05-17 CZ CZ19972657A patent/CZ289342B6/cs not_active IP Right Cessation
- 1995-05-17 PL PL95321830A patent/PL180784B1/pl unknown
- 1995-05-17 CA CA002213446A patent/CA2213446C/en not_active Expired - Fee Related
- 1995-05-17 CN CN95197689A patent/CN1089026C/zh not_active Expired - Fee Related
-
1996
- 1996-01-29 IN IN143CA1996 patent/IN188066B/en unknown
- 1996-02-19 ZA ZA961278A patent/ZA961278B/xx unknown
-
1997
- 1997-07-04 BG BG101745A patent/BG62436B1/bg unknown
- 1997-08-12 NO NO973714A patent/NO973714L/no not_active Application Discontinuation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US4436507A (en) * | 1981-07-16 | 1984-03-13 | Foster Wheeler Energy Corporation | Fluidized bed reactor utilizing zonal fluidization and anti-mounding air distributors |
EP0446379A1 (en) * | 1989-10-04 | 1991-09-18 | Asahi Kasei Kogyo Kabushiki Kaisha | Apparatus for producing alpha-beta-unsaturated nitrile |
WO1994019099A1 (de) * | 1993-02-18 | 1994-09-01 | Hoechst Aktiengesellschaft | Vorrichtung zur oxichlorierung |
Cited By (1)
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CN100435928C (zh) * | 2006-09-20 | 2008-11-26 | 浙江大学 | 一种气体分布器 |
Also Published As
Publication number | Publication date |
---|---|
SK113497A3 (en) | 1998-01-14 |
CZ265797A3 (cs) | 1998-02-18 |
CZ289342B6 (cs) | 2002-01-16 |
HU221883B1 (hu) | 2003-02-28 |
KR19980702341A (ko) | 1998-07-15 |
NO973714D0 (no) | 1997-08-12 |
RO118119B1 (ro) | 2003-02-28 |
BG62436B1 (bg) | 1999-11-30 |
KR100368512B1 (ko) | 2003-03-26 |
EP0810902B1 (de) | 1998-10-21 |
ZA961278B (en) | 1996-08-27 |
DE19505664C2 (de) | 1996-12-12 |
SK282850B6 (sk) | 2002-12-03 |
DE59504023D1 (de) | 1998-11-26 |
BR9510383A (pt) | 1998-06-02 |
HUT77918A (hu) | 1998-10-28 |
WO1996026003A1 (de) | 1996-08-29 |
JPH11500062A (ja) | 1999-01-06 |
DE19505664A1 (de) | 1996-08-29 |
CA2213446A1 (en) | 1996-08-29 |
AU702305B2 (en) | 1999-02-18 |
PL180784B1 (pl) | 2001-04-30 |
CN1175219A (zh) | 1998-03-04 |
PL321830A1 (en) | 1997-12-22 |
IN188066B (zh) | 2002-08-17 |
BG101745A (en) | 1998-05-29 |
RU2157726C2 (ru) | 2000-10-20 |
EP0810902A1 (de) | 1997-12-10 |
AU2881095A (en) | 1996-09-11 |
CA2213446C (en) | 2002-01-29 |
UA42056C2 (uk) | 2001-10-15 |
ES2126296T3 (es) | 1999-03-16 |
NO973714L (no) | 1997-08-12 |
MX9706276A (es) | 1997-11-29 |
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