CN106431828A - 卤代物水解方法及专用设备 - Google Patents

卤代物水解方法及专用设备 Download PDF

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CN106431828A
CN106431828A CN201610814535.1A CN201610814535A CN106431828A CN 106431828 A CN106431828 A CN 106431828A CN 201610814535 A CN201610814535 A CN 201610814535A CN 106431828 A CN106431828 A CN 106431828A
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hydrolysis
halides
strengthening
temperature
flow reactor
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李珣珣
朱建军
康登海
周新基
陈俊明
吴小强
王金建
于天鹏
宗小波
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NANTONG TIANSHI CHEMICAL CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/42Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by hydrolysis
    • C07C45/43Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by hydrolysis of >CX2 groups, X being halogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/126Microwaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/09Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
    • C07C29/12Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids
    • C07C29/124Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids of halides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids

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Abstract

本发明公开了一种卤代物水解方法及专用设备,水解过程采用强化水解手段,水解水进料温度是室温到220℃,卤代物进料温度从室温到220℃。采用平推流反应器,且平推流反应器带有可以换热和耐压性能的外壁。本发明效率高、投资省、能耗低。

Description

卤代物水解方法及专用设备
背景技术
卤代物水解制备醇或同一碳原子上的的二卤代物水解制备醛是经典的反应。一般的卤烷都可以由醇制得,因此水解卤烷制备醇似乎没有价值。但是实际上在一些比较复杂的分子中要引入一个羟基常常比引入卤原子困难很多。因此在合成中经常先引入卤原子再水解制备相应的醇。工业上不少产品是利用这个方法制备的,比如采用苄叉二氯水解制备苯甲醛;再比如一氯戊烷的各种异构体混合物通过水解制得戊醇的各种异构体混合物,以作工业溶剂。
卤代烷水解在通常情况下都很缓慢,往往需要加温或加碱来促进反应,实际上在升温和加碱的条件下水解速率也未必就十分理想。往往分子结构和所用溶剂的差异会导致很大的不同。
发明内容
本发明的目的在于提供一种效率高、投资省、能耗低的卤代物水解方法及专用设备。
本发明的技术解决方案是:
一种卤代物水解方法,其特征是:水解过程采用强化水解手段,水解水进料温度是室温到220℃,卤代物进料温度从室温到220℃。
所述强化手段为微波强化、超声波强化、高温强化、高压强化、电磁场强化中的一种或几种的组合。
水的mol量为卤素mol量的1~50倍。
所述微波强化,微波通过导波原件直接传送到反应器中,不需要穿透反应器壁,减少损失。
所述超声波强化,超声波通过平推流反应器外壁穿透进入反应介质。
所述高温、高压强化,反应设备采用平推流反应器,平推流反应器出料端设置减压阀,控制反应器内部始终处于高温高压状态。
所述卤代物水解方法是苄叉二氯制备苯甲醛的方法或一氯戊烷制备戊醇的方法。
采用平推流反应器,且平推流反应器带有可以换热和耐压性能的外壁。
平推流反应器内部设置有导流板或填料;导流板为防腐材料或涂有耐腐涂料的材料。
导流板的结构是SK、SV、SX、SL、SH静态混合器内部导流板的一种或几种组合。
本发明效率高、投资省、能耗低。
下面结合实施例对本发明作进一步说明。
具体实施方式
实施例1:
一种卤代物水解方法,水解过程采用强化水解手段,水解水进料温度是室温到220℃,卤代物进料温度从室温到220℃。
所述强化手段为微波强化、超声波强化、高温强化、高压强化、电磁场强化中的一种或几种的组合。
水的mol量为卤素mol量的1~50倍。
所述微波强化,微波通过导波原件直接传送到反应器中,不需要穿透反应器壁,减少损失。
所述超声波强化,超声波通过平推流反应器外壁穿透进入反应介质。
所述高温、高压强化,反应设备采用平推流反应器,平推流反应器出料端设置减压阀,控制反应器内部始终处于高温高压状态。
所述卤代物水解方法是苄叉二氯制备苯甲醛的方法或一氯戊烷制备戊醇的方法。
采用平推流反应器,且平推流反应器带有可以换热和耐压性能的外壁。
平推流反应器内部设置有导流板或填料;导流板为防腐材料或涂有耐腐涂料的材料。
导流板的结构是SK、SV、SX、SL、SH静态混合器内部导流板的一种或几种组合。
实施例2:
苄叉二氯超声波强化管式反应器(SV型填料)水解,水和苄叉二氯mol比例是10:1,反应时间20分钟,反应温度104℃,转化率98.9%,选择性99.5%。其余同实施例1。
实施例3:
苄叉二氯高温高压强化管式反应器(SK型填料)水解,水和苄叉二氯mol比例是5:1,反应时间10分钟,反应温度145℃,反应压力4MPa,转化率99.9%,选择性99.6%。其余同实施例1。

Claims (10)

1.一种卤代物水解方法,其特征是:水解过程采用强化水解手段,水解水进料温度是室温到220℃,卤代物进料温度从室温到220℃。
2.根据权利要求1所述的卤代物水解方法,其特征是:所述强化手段为微波强化、超声波强化、高温强化、高压强化、电磁场强化中的一种或几种的组合。
3.根据权利要求1所述的卤代物水解方法,其特征是:水的mol量为卤素mol量的1~50倍。
4.根据权利要求1、2或3所述的卤代物水解方法,其特征是:所述微波强化,微波通过导波原件直接传送到反应器中,不需要穿透反应器壁,减少损失。
5.根据权利要求1、2或3所述的卤代物水解方法,其特征是:所述超声波强化,超声波通过平推流反应器外壁穿透进入反应介质。
6.根据权利要求1、2或3所述的卤代物水解方法,其特征是:所述高温、高压强化,反应设备采用平推流反应器,平推流反应器出料端设置减压阀,控制反应器内部始终处于高温高压状态。
7.根据权利要求1、2或3所述的卤代物水解方法,其特征是:所述卤代物水解方法是苄叉二氯制备苯甲醛的方法或一氯戊烷制备戊醇的方法。
8.一种权利要求1所述的卤代物水解方法的专用设备,其特征是:采用平推流反应器,且平推流反应器带有可以换热和耐压性能的外壁。
9.根据权利要求8所述的卤代物水解方法的专用设备,其特征是:平推流反应器内部设置有导流板或填料;导流板为防腐材料或涂有耐腐涂料的材料。
10.根据权利要求8所述的卤代物水解方法的专用设备,其特征是:导流板的结构是SK、SV、SX、SL、SH静态混合器内部导流板的一种或几种组合。
CN201610814535.1A 2016-09-12 2016-09-12 卤代物水解方法及专用设备 Pending CN106431828A (zh)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4229379A (en) * 1977-11-25 1980-10-21 Bayer Aktiengesellschaft Process for the preparation of benzaldehyde
RO94833B1 (ro) * 1986-07-26 1988-07-31 Institutul De Cercetari Procedeu de preparare a alcoolilor amilici lineari
JP2007186440A (ja) * 2006-01-12 2007-07-26 Nippon Steel Chem Co Ltd 芳香族クロロメチル化合物の加水分解方法
CN102066423A (zh) * 2008-05-22 2011-05-18 T·C·刘易斯 自包容式、高效率纤维素生物质处理设备
CN105482045A (zh) * 2015-12-14 2016-04-13 北方华锦化学工业集团有限公司 一种耐热本体abs树脂的制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4229379A (en) * 1977-11-25 1980-10-21 Bayer Aktiengesellschaft Process for the preparation of benzaldehyde
RO94833B1 (ro) * 1986-07-26 1988-07-31 Institutul De Cercetari Procedeu de preparare a alcoolilor amilici lineari
JP2007186440A (ja) * 2006-01-12 2007-07-26 Nippon Steel Chem Co Ltd 芳香族クロロメチル化合物の加水分解方法
CN102066423A (zh) * 2008-05-22 2011-05-18 T·C·刘易斯 自包容式、高效率纤维素生物质处理设备
CN105482045A (zh) * 2015-12-14 2016-04-13 北方华锦化学工业集团有限公司 一种耐热本体abs树脂的制备方法

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Title
吴谋成: "《生物柴油》", 31 December 2008 *
姜华: "《酶工程技术及应用探析》", 31 December 2015 *
张旭之: "《乙烯衍生物工学》", 31 December 1995 *

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