氯化苯工艺设计

1、精选优质文档-倾情为你奉上 学号： 常州工程职业技术学院毕业设计（论文）题 目： 60000t/a氯化苯工艺设计 学 生： 学院（系）： 常州工程学院 专 业 班 级： 精细化工0530 校内指导教师： 专业技术职务： 校外指导老师： 专业技术职务： 年产60000吨氯苯工艺设计摘 要：本设计是关于年产60000吨氯苯生产工艺，设计主要参照南京化工厂氯苯生产的有关生产工程，对整个工艺进行了相关的物料衡算、热量衡算和设备计算。并确定了工艺路线及反应设备类型。同时对氯化器、粗馏塔、精馏塔和换热器进行了较为详细的计算，绘制了带控制点的工艺流程图，平面车间布置图、主要设备装置图和物料流程图。这次设计对

2、以后的工艺生产和设计提供一些依据和参考。关键词：苯 氯苯 二氯苯 三氯苯 盐酸the project of 60000t chlorobenzen each yearAbstract: This plan is about the project of 60000t chlorobenzen each year. Based on the experimental date obtain in the chemical engineer and process laboratory of Jiangsu petrol chemical university. We have made mate

3、rial balance and energy balance calculate. And decide the process route and reaction equipment. Meanwhile, we have made detailed calculated about fractionating rectifying tower and heat exchanger. In the same time, we have draw the process flow diagram, lane arrangement diagrom, vertical view lay-ou

4、t drawing and main equipment drawing. This design offered some advises for later process producing and engineering design.Key word: benzene chlorobenzenes dichlorobenzene trichlorobenzene hydrochloric acid目 录 1 总论··············

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124、83;·················351 总论1.1 设计依据氯苯是重要的有机化工产品，是染料、医药、有机合成的中间体，用于制造苯酚，硝基氯苯，苯胺以及杀虫剂DDT，还用于制取溶剂和橡胶助剂、油漆、快干墨水及干洗剂等，用途十分广泛，已有近九十年的发展历史了。在医药、染料、农药、工程塑料等领域是重要的中间体，是用途较广的有机溶剂，合成高分子材料添加剂的重要原料，是有机氯中间体中规模最大、应用领域最广泛的产品之一，也是氯碱企

125、业进行氯平衡的重要产品之一。随着氯化苯系列产品的开发及应用范围的不断扩大，氯化苯系列产品在化工生产中起着越来越重要的作用。氯化苯对干整个氯碱生产，尤其是平衡氯气，起着举足轻重的作用。过去，由于跑、冒、滴、漏现象严重，生产环境恶劣污染严重，原材料消耗居高不下一直成为制约生产发展和效益提高的难点。几年来，通过引入清洁生产的思想，使氯化苯的整个生产面貌一改往日被动局面，促进了形势的好转。通过清洁生产实践，改变落后的生产工艺和设备，注重生产过程中物料的循环利用，使污染物排放总量大幅度下降，环境质量得到改善，而且取得了较好的经济效益，同时也为环保工作提供了一种全新的方法：从被动的末端治理转向主动的源头控

126、制。为了满足市场的需求，对氯苯的生产不断地加以改进并扩大生产能力，产品质量得到了提高，在节能降耗上取得了一定成效。1.2 设计地区的自然条件1.2.1 地形、地貌本项目位于常州市新北区及规划区，地形平坦，市区南北水网地带较低。市区地势平坦，大部分标高在68米之间，最高洪水位6.38米。本区地震烈度为6度区。以下是氯苯生产厂址选择的原则a、 厂址宜选在原料、燃料供应和产品销售便利的地区，并在贮运、机修、公用工程和生活设施等方面具有良好协作条件的地区。b、 厂址宜选在靠近水量充足或水质良好的水源地段。c、 厂址要有便利的交通条件，要优先考虑水运。d、 选厂址应注意节约用地，不占或少占耕地。e、 选

127、厂址应注意选择地的自然环境条件，并对工厂投产后对于环境可能造成的影响做出预评价，工厂的生产和居民区的建设地点应同时选定。f、 厂址应避免设于低于水平面或在采用措施后不能确保不被水淹的地段。g、 厂址应避免布置在下列地区：地震断层地区和基本烈度9度以上的地震区厚度较大的级重湿性黄土地区易受洪水、泥石流、滑坡等危害的地区有开采价值的矿藏地区对机场、电台等使用有影响的地区国家规定历史文物、生物保护区和风景游览地区。具体地址：常州市新北区1.2.2 气象气候根据常州市气象站19521998年气象资料统计，本地区气象要素如下：（1）气温历年最高气温: 39.4(1978.7.10)历年最低气温: -15

128、.5(1955.1.27)多年平均气温：15.4多年平均最高气温：19.9多年平均最低气温：11.9多年最热月(7月)平均气温: 28.1多年最冷月(1月)平均气温: 2.7（2）降水多年平均降水量: 1074.0mm最大年降水量: 1815.6mm (1991年)最小年降水量: 535.7mm (1978年)月最大降水量: 505.4mm (1991年7月)日最大降水量: 196.2mm (1994年8月19日)多年降雨天数: 126天降水次数：日降水量5mm （52.2天）日降水量10mm （32.1天）日降水量25mm （11.2天）日降水量50mm （3.0天）最大积雪深度: 22cm

129、 (1984年1月19日)最大冻土深度: 12cm (1982年1月19日)（3）风况全年主导风向及频率: ESE 向 14%夏季主导风向及频率: ESE 向 19%冬季主导风向及频率: NNE 向 9%多年平均风速: 2.9m/s实测最大风速: 20.3m/s大风日数(风力7级):平均6天/年, 年最多19天。（4）雾况多年平均雾天数: 29.9天历年最多雾天数: 56.0天(1980年)历年最少雾天数: 17.0天(1967年)（5）雷暴多年平均雷暴天数: 33.5天历年最多雷暴天数: 59.0天(1963年)（6）相对湿度多年平均相对湿度：77%七月份平均相对湿度：82%一月份平均相对湿

130、度：74%1. 3 生产方法，流程特点，技术的 先进性和经济合理性（1）本设计采用的是连续法：氯化在苯的沸腾温度下进行，氯化器装有催化剂（铁屑或无水氯化铁）反应热由苯和少量氯苯气化带出。经过干燥的苯经转子流量计计量后加入氯化器底部，与经过计量的干燥氯气顺流进氯化反应器反应。反应副产的盐酸气及部分苯和氯苯蒸汽经石墨冷凝器冷凝，再经吸收塔用粗氯苯喷淋吸收。当吸收液含苯量到3236%时，混入酸性氯化液去中和，而气体吸收成31%的副产盐酸。氯化器流出的酸性氯化液经水洗后，用液碱中和除去残余的酸及三氯化铁，再经盐干燥器，预热至一定温度后加入粗馏塔，从塔顶取出苯，塔釜的粗氯苯连续加入精馏塔，从塔顶得到氯苯

131、，塔釜残液间断放出，回收其中的二氯苯。（2）特点：该方法简单，反应原料价格低廉，环保1.4 车间的组成根据工艺特点，分为一个车间。车间组成由生产部分、辅助生产部分和行政-生活部分组成。生产部分包括生产区、控制室、储罐区等。辅助生产部分包括动力室（真空泵和压缩机室）、配电室、化验室、实验室、机修室、通风空调室，原料、辅料和成品仓库等。行政部分包括办公室、会议室、工人休息室。生活部分有更衣室、浴室、厕所和女工保健室等。1.5 生产制度生产量： 60000吨/年 生产方式： 连续生产年操作日： 300天/年 日生产时间： 24小时生产班数： 四班三运转工作制1.6 公用工程水电气，辅助工程需要量，标

132、明介质，温度，压力，流量等。1.7 经济分析主要结论静态分析：从国民经济角度投资回收期从企业经济角度投资回收期动态分析：从国民经济角度投资回收期从企业经济角度投资回收期2 文献评述2.1 简史叙述1905年首先报道用苯直接氯化制得氯苯。1909年由英国的United Alkali公司开始工业化生产。1915年Hooker电化公司的第一个8200 t/a 装置在美国投入运行。同年Dow化学公司在美国也开始工业化生产氯苯。因此可以说在主要有机化工产品中氯苯是第一个大规模生产的产品。1920年 Dow化学公司开发了两个大量使用氯苯的工艺。一是氯苯在溶解铜催化剂存在下用氢氧化铵水解生成苯胺，另一个是用

133、氢氧化钠溶液在高温高压下水解氯苯制苯酚。在之后30年中，这一直是制备苯酚及苯胺的主要生产方法。另外，氯苯经硝化制得硝基氯苯和经磺化后制得氯苯磺酸等均是较重要的有机化工中间体。到40年代末期，用异丙苯法生产苯酚实现工业化。由硝基苯加氢法制苯的工艺也于1954年建成大规模生产装置，所以氯苯生产量从70年代以来呈下降趋势，到80年代基本稳定在一定水平上。2. 1. 1 产品物理化学性质及质量指标（1）纯品的物理性质 氯苯，别名一氯化苯，英文名Chlorobenzene，monochlorobenzen结构式 分子式 C6H5Cl 分子量 112.5 主要物理化学常数 比重：d420 1.1064 闪

134、点：（闭环法） 28 沸点：（常压） 131.7熔点： -45.34凝固点： -45.58共沸点：氯苯与水共沸混合物沸点 90.2/常压，其中：一氯苯 71.6%、水28.4% 毒性： 本品为无色透明液体，气味有点像苯。对皮肤和上呼吸道有刺激作用。抑制中枢神经，具有麻醉作用。对肝脏、肾脏及造血系统有不良影响。慢性中毒引起头痛、头晕、精神不振、消化不良等症状。工作场所最高容许浓度为350mg/m3。推荐通风设计浓度50ppm，嗅觉阀浓度0.21ppm，最大排放浓度为150 mg/m3。（2）纯品化学性质苯环上氯原子很不活泼，在特定条件下转换为羟基、氨基及甲氧基等，如： 苯环上的氯基的邻对位氢原子

135、置换为硝基-NO2或氯基。如：（3）产品的质量指标（GB240480） 表1 质量指标指标名称一级品二级品外观在20时为无色或微黄透明液体（其色度不得深于40度）酸度对刚果红不变蓝相对密度d4201.10621.10761.10571.1082氯苯含量%99.5099.00苯含量%0.150.30多氯苯%/0.70 2.2 工业生产方法的选择及论证2. 2. 1 国内外生产概况目前世界上氯苯的主要生产国家和地区有美国、西欧、中国、日本和俄罗斯。90年代初世界总生产能力为500 kt/a 左右，其中美国170 kt/a 、西欧125 kt/a 、中国120 kt/a 、俄罗斯40 kt/a 、日

136、本28 kt/a。中国氯苯生产主要有10家左右工厂，其中锦西化工厂规模最大，1989年全国消费量为78kt左右，主要用于生产有机化工原料、中间体及农药。2. 2. 2 评述各种生产方案工艺上主要有苯液相氯化法和苯气相氯化法。气相法反应温度为400500，成本比液相法高，故已被淘汰。苯液相氯化法以脱水后的干苯和电解氯为原料，在路易斯型催化剂（如FeCl3、MnCl2或SnCl4）存在下，经催化而得，其反应如下：苯液相氯化有间歇式和连续式两种生产方式。间歇法：把干燥的苯装入氯化反应器中，再加入相当于苯量1%的铁屑作为催化剂。氯气的加入速度以能维持反应温度在4060为宜，温度过高有利于多氯苯的生成。

137、氯气鼓泡通入苯中至料液的相对密度达到1.280（15）。反应放出的氯化氢用苯或氯苯洗除有机雾滴，再用水吸收得到盐酸。氯化物料用10%的NaOH中和，并经干燥、蒸馏，得到下列馏分（以100%氯化料计）：苯和水（3%），苯和氯苯（10%），此二馏分返回系统；氯苯（75%）；作为产品：氯苯和二氯苯（10%）高沸物（2%），此二馏分用于分离邻、对二氯苯。氯化产品的组成决定于氯化温度，氯化速率，氯化深度和采用的催化剂。一般氯化产品组成为氯苯80%、对二氯苯15%、邻二氯苯和多氯苯5%。 表2 反应液组成与相对密度的关系反应液各种氯化苯含量%（重量）相对密度苯一氯苯对二氯苯邻二氯苯三氯苯1.0373163

138、421.07523235911.51.11685622141.24013040263连续法：氯化在苯的沸腾温度下进行，氯化器装有催化剂（铁屑或无水氯化铁）反应热由苯和少量氯苯气化带出。经过干燥的苯经转子流量计计量后加入氯化器底部，与经过计量的干燥氯气顺流进氯化反应器反应。反应副产的盐酸气及部分苯和氯苯蒸汽经石墨冷凝器冷凝，再经吸收塔用粗氯苯喷淋吸收。当吸收液含苯量到3236%时，混入酸性氯化液去中和，而气体吸收成31%的副产盐酸。氯化器流出的酸性氯化液经水洗后，用液碱中和除去残余的酸及三氯化铁，再经盐干燥器，预热至一定温度后加入粗馏塔，从塔顶取出苯，塔釜的粗氯苯连续加入精馏塔，从塔顶得到氯苯，

139、塔釜残液间断放出，回收其中的二氯苯。此外还有气相氧氯化法制取氯苯，其反应如下： C6H6 + HCl +1/2O2 C6H5Cl +H2O工艺过程为：将苯蒸气、空气、氯化氢气体混合物加热升温至210，通入氯化反应器，在迪肯型催化剂（CuCl2、FeCl3负载在三氯化铝上）存在下进行氯化。反应温度300，苯单程转化率为10%15%，氯化氢转化率为98%，生成物含多氯苯6%。此过程是拉西法苯酚生产的一部分，因此，该法主要用于生产苯酚。由于拉西法苯酚被淘汰，此法已不发展。因为间歇法生产力小，连续法成本较低，积存的可燃物较小，生成的二氯苯较少，所以本设计选用液相连续法作为生产方法。2.3 产品的发展前

140、景我国从1950年开始生产氯化苯，多年来一直供不应求，需从国外进口相当数量的硝基氯苯来满足国内市场的需求，由于市场需求迫切，90年代初国内各地纷纷建设或扩建氯化苯装置，目前生产厂家近20家，总生产能力达31万t/a左右。我国氯化苯的快速发展实际上是与下游产品硝基氯苯的不断扩建和新建有关系，目前国内氯化苯消费量的80%用于合成硝基氯苯，所有硝基氯苯生产企业都要配套建设氯化苯装置，可以说硝基氯苯市场及变化与氯化苯休戚相关。3 工艺叙述部分3.1 设计的生产方法及生产流程的选择氯化苯分子式 C6H5Cl无色透明液体，具有不愉快的苦杏仁味 。目前国内生产氯化苯主要采用苯氯化法,即用纯苯和干燥

141、氯气在氯化塔内进行反应,生成的氯化液经过水洗、中和、干燥后,送入粗、精馏塔蒸馏得到成品氯化苯。苯环上的卤代反应较困难，常用FeX3、Fe、AlX3等催化剂催化（X为卤素）。反应过程中，卤素分子在苯和催化剂的共同作用下异裂，以氯为例，反应需要加入催化剂FeX3。生产工艺流程见下图：主要生产工序有苯干燥、氯化、水洗中和、粗馏、精馏、尾气吸收及多氯化物回收。其工艺路线为干燥苯与氯气在氯化铁催化下连续氯化，得到氯化液经水洗中和、粗馏、精馏，除去其中的氯化氢、苯、多氯苯而制成氯化苯成品。氯化反应放出的尾气经冷却喷淋除苯后，用水吸收制成副产盐酸。精馏残液经多氯化物工序回收苯、氯化苯，返回生产用，回收的二氯

142、苯作为副产品出售，剩余的残渣包装出售。从事氯苯生产或使用氯苯的企业，以及在运输等过程中，由于操作和管理失误，均可构成氯苯的污染。该物质对环境有严重危害，应特别注意对地表水、土壤、大气和饮用水的污染。下面就工艺改进和设备完善两个方面作简要介绍。（1） 改进生产工艺干燥器加片碱在氯苯生产中物料带酸，严重腐蚀设备，而且影响安全生产，在实践中发现，片碱既是良好的干燥剂，又是理想的中和剂，加入少量片碱避免了物料带酸。拆除二段冷凝器氯化二段冷凝器经常造成盐酸气中的苯在其中凝结，影响安全生产。权衡利弊，故将二段冷凝器拆除。氯化液下料管增加冷却器氯化液下料温度在80左右，接近苯的沸点，在氯化液下料管和缓冲罐之间增加一台石墨块孔式换热器，把温度控制在40以下，使氯化液下料流畅。改进氯化器氯化器在生产运行中，氯化液出料流量不均，针对这一情况，做了一定改进。（2） 完善生产设备与扩大生产能力氯化器下部增加测温点氯化器下部出现局部过热现象，甚至造成铁环熔化粘结，发生黑料着火事故。为此可在氯化器下部增加1个测温点，以及时发现事故苗头并采取措施。安装静态混合器在水洗中和过程中，混合愈充分，除酸的效果愈好。可在泵的出口处安装管式静态混合器，