【作者】 叶斌；

【导师】 陈新志；

【作者基本信息】 浙江大学 ， 化学工程， 2002， 硕士

【摘要】 本文采用管式反应器，以丙酮和氯气为原料合成一氯丙酮，考察了反应物料相态、反应管尺寸、反应物料配比等因素对反应结果的影响；研究了共沸精馏分离沸点及其相近的氯丙酮混合物；进行了100t/a一氯丙酮中试的研究和设计。中试产品经过数家制药企业使用，产品符合制药企业的质量要求。 丙酮与氯气反应制取一氯丙酮，是一个快速的连锁反应。采用管式反应器，可有效抑制二氯和多氯丙酮的生成，提高反应的选择性。丙酮气化后与氯气反应，较之液态丙酮与氯气反应，物料易于混合，可通过控制反应物配比和单程转化率来提高反应的选择性，抑制二氯及多氯产物的生成。气相停留时间直接影响反应转化率和选择性。本研究课题没有花费大量时间进行动力学测定，直接采用尺寸不等的反应管考察反应结果，确定优选的工艺条件。经过实验，选定Φ20*600mm的反应管进行氯化反应，物料配比为：丙酮/氯气=4：1-5：1(摩尔比)。 丙酮氯化制备一氯丙酮时，难免会有少量的1、1-二氯丙酮产生，由于二者沸点仅相差0.3℃，常规分离方法不能将两者分开。通过实验研究，确定采用水作共沸剂，恒沸蒸馏分离氯丙酮混合物。实验确定共沸剂水的加入量与氯丙酮混合液的比例为1：1(体积比)时，能达到良好的分离效果，可得到纯度99％以上的一氯丙酮。 反应过程的放大是过程放大的核心和关键。参照小试反应管参数和工艺参数，采用多根同尺寸反应管并联的列管式反应器作为中试反应器，有效减小了“放大效应”的影响。在综合考虑产品质量、生产成本、环境保护等因素的前提下，进行工艺流程设计，在生产一氯丙酮的同时，副产染料级氯丙酮和盐酸，既减少环境污染，又降低了生产成本。 该生产工艺流程简单，过程易于控制。中试装置经过正常运转和成本核算，证明该生产工艺技术可行，投资少，污染小，具有较好的经济效益和社会效益。更多还原

【Abstract】 This thesis focuses on developing a novel technology to produce Monochloroacetone in high degree of purity and less environmental pollution.Monochloroacetone is prepared by the reaction of acetone vapor with chlorine in a pipe reactor. The influence of several factors on the reaction, such as the states of acetone in the reaction, sizes of the pipe reactor, ratios of acetone to chlorine, has been investigated experimentally and theoretically. The reaction of acetone with chlorine gas is a rapid chain reaction. Using a pipe reactor can diminish formation of polychlorinated products. Comparing with liquid acetone ,acetone vapor is easier to mix with chlorine gas and this will befits to the results of the reaction. Selectivity of the reaction can be increased by controlling ratio of acetone to chlorine and conversion per pass of acetone. Residence time of reactants in the pipe reactor is a main factor to influence the conversion of acetone and selectivity of the reaction. We didn’t spend much more time on establishment of dynamics equation of the reaction, but carry out the reaction in a series of different sizes pipe reactors to get the best technological parameters. That is the size of reactor is 20·600mm and the ratio of acetone to chlorine is 4: 1-5: 1 (mole ratio).The mixture of Monochloroacetone and 1,1-dichloroacetone ,which have very similar boiling points, the difference of boiling points of theses two compounds is only 0.3℃, is separated by azeotropic distillation using water as azeotropic former. The purity of Monochloroacetone can be reached to 99% by azeotropic distillation in the ratio of water to the mixture of Monochloroacetone and 1,1-dichloroacetone 1:1(volume ration).The amplification of reactor is the core of scaling process. We designed a tubular reactor with one hundred tubes that have same sizes with the pipe reactor in laboratory research and operate under the sametechnological condition with laboratory experiments. This way minimize the "scaling effects" in scaling process. Based on the consideration of purity and cost of the products and environmental protection, the process is designed to produce Monochloroacetone as well as by products of choloroacetone for dyestuff manufacture and hydrochloric acid to reduce cost and avoid pollution.The pilot plant research in the scale of 100t/a Monochloroacetone and the design of the producing process have been done. And the products of Monochloroacetone of this pilot apparatus have been tested and used by several pharmaceutical factories. The quality of Monochloroacetone meets the quality requirement of pharmaceutical industry. And the apparatus has been running more than two years profitably.更多还原