CN1406924A - 用于绝热硝基化的管式反应器 - Google Patents
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Abstract
本发明涉及一种经优化后的管式反应器,它用于芳香化合物、卤代芳香化合物以及卤代烃的绝热单硝基化。
Description
技术领域
本发明涉及一种经优化后的管式反应器,它用于芳香化合物、卤代芳香化合物以及卤代烃的绝热单硝基化。
背景技术
芳香化合物的硝基化在两个液相中进行。水相中包括用作催化剂的硫酸以及用作反应组分的硝酸,另外还可能有其它成分,例如磷酸,它在甲苯硝基化过程中起着影响所形成异构体的比率的作用。有机相中包括待硝化的芳香化合物,另外还包括在反应中生成的已硝化的芳香化合物部分。
例如,芳香化合物的硝化在恒温的环反应器中进行,而且在反应器中的一点或多点处,水相分散在有机相中或有机相分散在水相中。两相在离开反应器之前在回路反应器中进行多次循环。这个循环流及其与进料流量的比决定着这两相通过反应器中分散点的次数与时间频率。
芳香化合物的硝基化也可能在绝热的条件下进行。这一反应操作使得反应混合物在越来越快的转化过程中得到加热,反应时间也因高温引起反应加速而缩短。这一反应操作的另一优点是反应混合物的高温可用于蒸发反应过程中所产生的水。
通常情况下,绝热硝化在管式反应器中进行。由于没有回流或循环流,与回路反应器相比它具有更有利的浓度分布图,可提高这种反应器的时空产率。由于没有循环流,这种管式反应器的分散点必须连续排列。
EP 0 779 270 B1描述了一种可用于制备一种单硝基芳香化合物的管式反应器。这种管式反应器包括一种管,在其内部螺旋形、平片状的构件是按以下方式排列成一种序列:一个螺旋形、平片状的构件的一个前面边缘基本上垂直于前一构件的一个后面边缘。通常,一个反应器中有50个或50个以下这种螺旋形、平片状的构件,据报道其优选数量为4-12个。这种反应器的一个缺点是安在其中的螺旋形、平片状的构件具有特殊形状,必须为这种反应器专门制造。
EP0489211描述的是一种包括特殊内件的喷射冲击式反应器,用于进行单硝基化反应。这些内件由球体与半球体组成,其上有孔。这种反应器的目的在于使液相的优化混合顺利进行。所述反应器的缺点是它的制造成本高、不方便,而且上述的内件也需专门制造。
DE 44 10 417 A1与DE 44 11 064 A1描述甲苯或卤代苯的绝热硝基化过程。优先在带有可分散反应混合物的内件,例如多孔金属板的一个反应器中进硝基化反应。分散级数应为2-50。然而,以上提及的说明书并未声明这个反应器中需要多少内件,以及为使一个绝热硝化反应达到想得到的最终转化率所需提供的其他条件。
因而就需要有一种结构简单、能用来绝热制备一硝基化合物的管式反应器。该管式反应器的结构应使它具有足够的分散效果,使绝热硝化反应达到想得到的最终转化率。
令人惊讶的是,一种用于芳香化合物、卤代芳香化合物以及卤代烃的绝热单硝基化的管式反应器已经研制出来了,其特征是该管式反应器被隔板分隔成4-12个室,这种隔板有孔,并且每个隔板会产生0.5-4巴的压降。
研究表明,绝热单硝化方法想要达到的最终转化率取决于反应器的分散效果。为达到足够高的分散效果,该发明将带有合适开孔的板安置在反应器中,将反应器分隔成室。可以从绝热过程操作获得的高反应温度,以及具有腐蚀性的原料的进料对该隔板的材质提出了高的要求。优选使用在这些条件下呈惰性的材料,因而钽板就更被优选采用。因为这种材料贵,所以在硝化过程中使用尽量少的隔板数对其经济适用性就尤为重要。另一方面,为保证反应器中的理想的活塞流特性,反应器中又必须至少保证一定量的室,从而至少需要一定量的隔板。
本发明的反应器相应地用隔板分隔成4-12个室,优选6-12个,更优选7-11个。这些隔板起着分散器的作用。在该发明的反应器中,这些隔板上有孔,这些孔可以是槽形孔、冲压孔或钻孔。优选钻孔,因为它们容易制造。不过,其它形式的孔也可以选用。通常,为使质量流量为1t/h,一块隔板需10-25个孔,优先选择15-20个。
该发明的反应器优选在底部至少有一个反应物进料装置,在顶部至少有一个移出反应混合物的装置。该发明的一种优选实施方案有向反应器中个别室方便引进有机相与水相的进料装置。
除个别分散元件的数量与分隔方式外,分散能量对反应的分散效果并因此对最终转化率同样重要。分散能量一般应通过机械方式向反应混合物提供,而且同样应该越小越好,以节省操作费用。在采用隔板的情况下,在该发明中隔板有孔,一块隔板的分散效果就由通过该隔板的压降决定。从机械稳定性的角度考虑,压降决定了隔板的厚度,从而决定它的成本。
为使整个反应器都获得活塞式流动特性,避免在通过隔板时产生不期望的返流,该发明采用的隔板的压降为每板0.5-4巴。在芳香化合物的绝热单硝基化时,特别优选压降为0.5-3巴的隔板,更加优选0.8-2巴。
对于卤代芳香化合物与卤代烃的绝热单硝基化,优选采用压降为每板0.5-3巴的隔板,特别优选每板0.5-1.2巴的隔板。
优选使每板的压降尽可能地低,因为如果压降越高,例如就可能需要电功率越高的电泵,从而导致越高的总操作费用。
在该发明中,特别优选室数以及相应的隔板数尽可能少,因为例如,一块钽板的价格基本上取决于所采用的钽量,即隔板的厚度。当隔板数少时每块隔板的压降就必然增加,但这并不会对隔板的价格产生强烈的影响,因为隔板厚度仅仅与压降的平方根成比例。
在本发明的管式反应器中进行绝热单硝基化反应,所采用的反应物的组成范围在诸如US5,313,009,EP 0436 443 B1或DE 44 10417A1中已经作出了描述。然而,其它组成也可能适用。
卤代芳香化合物的单硝基化反应所采用的反应物的组成范围在US4,453,027或DE 44 11 064 A1已经作出了描述。在本申请中,其它组成也可能适用。
附图说明
图1显示的是本发明的一个特别优选实施方案。这是一个被有孔金属隔板(2)分隔成7个室的管式反应器(1)。在其底部安置了一个加入反应物(3)的装置。其它进料装置(4)可以用来直接向个别的室加料。反应器的顶部安置了一个引出反应混合物的排料装置(5)。具体实施方式
实施例
实施例1
约70重量%的硫酸以180kg/h的流量加入流量为8kg/h的约70重量%的硝酸中形成一种约3重量%的混合酸。它在一个热交换器中加热到约80℃。然后将9kg/h的甲苯通过一个分散元件与混合酸混合。此分散元件由哈司特镍合金制造,其结构如DE 199 05 572 A1所示。酸一侧的最窄流动截面面积为7mm2,甲苯侧为0.25mm2。酸侧的压降大约为0.5巴。分散元件安置在一个绝热管式反应器的入口处,该绝热管式反应器由搪瓷钢制造(直径50mm,高3255mm)。在管式反应器中,另有18个钽制的分散元件,呈1mm厚的碟形,每件上有4个直径1.4mm的钻孔,在整个高度实质上均匀分布。每板压降约为0.5巴。在反应器的下游终端,温度升至110℃并且所有的硝酸已经反应完全。反应分布曲线通过沿反应器轴线的温升来确定(见图2)。有机相与酸性水相于110℃在一个容器中分离。水相引入一个蒸发器中,在这里将反应中所产生的水在约90℃的温度下蒸发去除。从所形成的再浓缩酸中引出一排放流,代之以新鲜酸以防止副产品的积聚。酸流与硝酸又一次混合后返回反应器。
在图2,通过以百分率计算的转化率(1)与以秒计算的停留时间(2)作图表示出了实施例1的结果。
实施例2
将约70重量%的硫酸以252kg/h的流量加入流量为1 3kg/h的约68重量%的硝酸中形成一种约3重量%的混合酸。它在一个热交换器加热到约80℃。然后将13.9kg/h的甲苯通过一个分散元件(与实施例1中的分散元件类似)与混合酸混合。分散元件安置在一个绝热管式反应器的入口处,该绝热管式反应器由搪瓷钢制造(直径50mm,高3255mm)。在该管式反应器中,按实施例1所描述构成的4个分散元件分布于反应器中,分布在200,750,1300与1800mm的高度处。由于比实施例1的质量流量大,每板的压降约为1巴。在反应器的下游终端,温度升至110℃并且所有的硝酸已经反应完全。其它步骤以及实验装置与实施例1类似。
实施例3
将约70重量%的硫酸以180kg/h的流量加入流量为8.3kg/h的约68重量%的硝酸中形成一种约3重量%的混合酸。它在一个热交换器加热到约80℃。然后将8.1kg/h的甲苯通过一个与实施例1中的分散元件类似的分散元件与混合酸混合。分散元件安置在一个绝热管式反应器的入口处,该绝热管式反应器由搪瓷钢制造(直径50mm,高3255mm)。在管式反应器中,有6个呈1mm厚碟形的分散元件,每件上有3个直径1.36mm的钻孔,这些分散元件在反应器中分布于200,500,750,1000,1300与1800mm的高度处。每板的压降约为1巴。在反应器的下游终端,温度升至110℃并且所有的硝酸已经反应完全。其它步骤以及实验装置与实施例1类似。
实施例4
在随后的计算中用到了以下反应量:10t/h的甲苯;9.6t/h的68重量%的硝酸;208kg/h约70重量%的硫酸。
当钻孔直径与实施例1一样为1.4mm并且被钻孔横截面C所分流的质量流量保持恒定时,实施例1-3每例中隔板上都产生相同的压降。对于实施例1:
M实施例4/C实施例4=M实施例1/C实施例1 (方程式1)
C值由钻孔直径d和钻孔数量N计算而得:
C=л/4·d2·N (方程式2)
将方程式2代入方程式1中解出N实施例4:
N实施例4=N实施例1·d2 实施例1/d2 实施例4·M实施例4/M实施例1 (方程式3)
得到了如下钻孔数:
实施例1:
N=4·1.42/1.42·(10000+9600+208000)/(8+180+9)=4621个钻孔/板
实施例2:
N=4·1.42/1.42·(10000+9600+208000)/(13+252+13.9)=3264个钻孔/板
实施例3:
N=4·1.362/1.42·(10000+9600+208000)/(8.3+180+8.1)=3281个钻孔/板
当这个反应器有一个直径D=700mm的横截面积并且其钻孔以三角形方式定位,钻孔的分流s可以计算如下:
在例如DIN 28182所描述的三角形中,钻孔的中心就是以s为边长的等边三角形的顶点。因为在这样一个等边三角形中所有的角都是60°,则每一钻孔只有1/6在三角形中。将钻孔在三角形以内的面积总起来即为每个三角形3·1/6=1/2个钻孔面积。从而钻孔数N就等于反应器横截面能被分割成的等边三角形数量的一半。三角形的数量由反应器的横截面积与一个三角形的面积的比值而得:
π/4·D2/√3/4·s2=π/√3·D2/s2 (方程式4)
这样得到:
N=·π/√3·D2/s2 (方程式5)
解出s:
s=D·√[π/(2N√3)] (方程式6)
这样便给出了以下的钻孔分流:
对于实施例1:s=700·√[π/(2·4621√3)]=9.8mm
对于实施例2和3,可类似地解得分别为11.7mm和11.6mm。
隔板材料是依据VdTUV-Werkstoffblatt 382(German technicalsurveillance asociation的材料数据表)选用钽ES。根据表中数据,它在130℃时的0.2%拉伸极限为Rp0.2=94N/mm2。
为了计算隔板的必需厚度,使用ADMerkblatt B5(German code ofpractice)的第19式。安全系数设为S=1.5,计算系数设为C=0.4。忽略c1与c2的影响,下表中给出已计算得出的隔板厚度。
实施例编号 | 超过压 | 削弱系数 | 隔板厚度 | 隔板数 | 钽用量 |
1 | 0.5巴 | 0.86 | 8.5mm | 18 | 977kg |
2 | 1巴 | 0.88 | 11.9mm | 4 | 304kg |
3 | 1巴 | 0.88 | 11.9mm | 6 | 456kg |
Claims (6)
1.用于芳香化合物、卤代芳香化合物以及卤代烃的绝热单硝基化的管式反应器,其特征在于该管式反应器被隔板分隔成4-12个室,这些隔板上有孔,并产生0.5-4巴/板的压降。
2.权利要求1中的管式反应器,用于苯或甲苯的绝热单硝基化,其特征在于隔板上产生0.8-2巴/板的压降。
3.权利要求1中的管式反应器,用于氯苯或邻二氯苯的绝热单硝基化,其特征在于隔板上产生0.5-1.2巴/板的压降。
4.前述权利要求1至3中一项或多项所述的管式反应器,其特征在于孔是钻孔。
5.前述权利要求1至4中一项或多项所述的管式反应器,其特征在于隔板是钽板。
6.前述权利要求1至5中一项或多项所述的管式反应器,其特征在于它有有机相和水相的加入装置,这些装置便于向位于反应器中的各个室加料。
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DE10223483A DE10223483A1 (de) | 2001-09-10 | 2002-05-27 | Rohrreaktor zur adiabatischen Nitrierung |
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CN110546130A (zh) * | 2017-02-03 | 2019-12-06 | 约瑟夫·迈斯纳两合公司 | 用于芳香族化合物绝热硝化的方法及装置 |
CN113694858A (zh) * | 2020-05-26 | 2021-11-26 | 唐山金坤化工有限公司 | 苯环硝化的连续硝化反应装置及方法 |
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DE102004038555B3 (de) * | 2004-08-06 | 2005-08-04 | Plinke Gmbh | Modularer Mikroreaktor zur Nitrierung mit Mischsäure |
DE102007059513A1 (de) | 2007-12-11 | 2009-06-18 | Bayer Materialscience Ag | Verfahren zur Herstellung von Nitrobenzol durch adiabate Nitrierung |
DE102008048713A1 (de) | 2008-09-24 | 2010-03-25 | Bayer Materialscience Ag | Verfahren zur kontinuierlichen Herstellung von Nitrobenzol |
CN102216253B (zh) * | 2008-11-14 | 2015-01-14 | 诺拉姆国际公司 | 在单硝基苯生产过程中减少副产物二硝基苯形成的方法 |
DE102010006984A1 (de) * | 2010-02-05 | 2011-08-11 | Bayer MaterialScience AG, 51373 | Verfahren zur kontinuierlichen Herstellung von Nitrobenzol |
WO2013054180A1 (en) | 2011-10-14 | 2013-04-18 | Council Of Scientific & Industrial Research | Continuous modular reactor |
US8907144B2 (en) | 2012-03-22 | 2014-12-09 | Noram International Limited | Process for adiabatic production of mononitrotoluene |
EP2877442B1 (de) | 2012-07-27 | 2016-11-16 | Covestro Deutschland AG | Verfahren zur herstellung von nitrobenzol durch adiabate nitrierung |
CN104487413B (zh) | 2012-07-27 | 2017-03-29 | 科思创德国股份有限公司 | 通过绝热硝化制备硝基苯的方法 |
KR102066764B1 (ko) | 2012-07-27 | 2020-01-15 | 코베스트로 도이칠란드 아게 | 단열 니트로화에 의한 니트로벤젠의 제조방법 |
WO2014167506A1 (en) | 2013-04-10 | 2014-10-16 | Council Of Scientific & Industrial Research | Flow reactor with pinched pipe sections for mixing and heat transfer |
WO2014177450A1 (de) | 2013-04-29 | 2014-11-06 | Bayer Materialscience Ag | Verfahren zur herstellung von nitrobenzol durch adiabate nitrierung |
US10815189B2 (en) | 2017-03-07 | 2020-10-27 | Covestro Deutschland Ag | Method for producing nitrobenzene |
WO2020011817A1 (de) | 2018-07-12 | 2020-01-16 | Covestro Deutschland Ag | Verfahren zur herstellung von nitrobenzol durch adiabatisch betriebene nitrierung von benzol |
WO2020212334A1 (de) | 2019-04-17 | 2020-10-22 | Covestro Deutschland Ag | Verfahren und vorrichtung zur herstellung von nitrobenzol |
EP3956289A1 (de) | 2019-04-17 | 2022-02-23 | Covestro Deutschland AG | Verfahren zur kontinuierlichen herstellung von nitrobenzol |
WO2024003050A1 (en) | 2022-06-28 | 2024-01-04 | Basf Se | Process for producing nitrobenzene |
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US3576606A (en) * | 1968-05-24 | 1971-04-27 | Hercules Inc | Reactor for the manufacture of nitric oxide |
US4919541A (en) * | 1986-04-07 | 1990-04-24 | Sulzer Brothers Limited | Gas-liquid mass transfer apparatus and method |
CA2141886E (en) * | 1994-05-11 | 1999-10-12 | Federico Zardi | Reactor for two-phase reactions, in particular for urea synthesis at high pressure and temperature |
IL115063A0 (en) * | 1994-09-09 | 1995-12-08 | Urea Casale Sa | Method for in-situ modernization of a urea synthesis reactor |
PT1272268E (pt) * | 2000-03-02 | 2012-07-24 | Dow Global Technologies Llc | Reator tubular, processo de realização de reações multifásicas líquido/ líquido num reator tubular, e um processo de nitração cíclica de compostos aromáticos num reator tubular |
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CN110546130A (zh) * | 2017-02-03 | 2019-12-06 | 约瑟夫·迈斯纳两合公司 | 用于芳香族化合物绝热硝化的方法及装置 |
CN110546130B (zh) * | 2017-02-03 | 2022-07-15 | 约瑟夫·迈斯纳两合公司 | 用于芳香族化合物绝热硝化的方法及装置 |
CN113694858A (zh) * | 2020-05-26 | 2021-11-26 | 唐山金坤化工有限公司 | 苯环硝化的连续硝化反应装置及方法 |
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JP2003160543A (ja) | 2003-06-03 |
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