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华北科技学院毕业设计(论文)I年产一万吨甘氨酸生产工艺设计设计总说明1、设计目的及意义甘氨酸是氨基酸系列中结构最为简单,人体非必需的一种氨基酸, 在分子中同时具有酸性和碱性官能团。根据甘氨酸制备工艺和产品的纯度可分为食品级、医药级、饲料级和工业级四种规格产品。甘氨酸的生产、运用及其功用价值, 已在全球越来越引起人们的关注。许多国家的食品、医药药物、化肥、农药、饲料等的生产,已离不开它的加盟, 或借助与利用它的一些特殊功效作用来改变产品的一些风味或质量。2、工艺设计任务本甘氨酸生产项目以乌托品,氨气为原料,合成甘氨酸的方法为氯乙酸氨解法,主要设备为氨化合成釜,精馏塔,采用间歇式生产方式生产,预计生产能力为每年 1 万吨。3、工艺设计依据(1)2016 届本科毕业设计任务书(2)朱炳辰主编.化学反应工程 ,2012. 北京:化学工业出版社(3)谭天恩.化工原理.2006,北京:化学工业出版社(4)陈五平.无机化工工艺学.2002,北京:化学工业出版社4、设计工艺说明甘氨酸生产工艺路线很多,目前工业化和具有工业化前景的生产工艺主要有氯乙酸氨解法,施特雷克法(cstercker法),氢氰法,及生物合成法等。本设计采用的方法为氯乙酸氨解法。该法根据原料不同,又可分两种工艺:(1)水相或醇相中以乌洛托品,氯乙酸、氨水(氨气或者液氨都可以)为原料合成;(2)水相中以碳酸铵或氨基甲酸胺、氯乙酸、氨水为原料合成。目前国内的生产方法以前者为主,收率在70%左右,后者收率较低(约42%),故很少用于工业化生产。由于水相合成甘氨酸中乌洛托品消耗较大,且乌洛托品价格较高,无法回年产一万吨甘氨酸生产工艺设计收,因此成本较高,而以醇溶液代替水溶液则会大大降低乌洛托品的消耗量,从而降低生产成本,因此,目前国内普遍采用醇相法合成甘氨酸。氯乙酸氨解制备甘氨酸过程中,氨解工序优化条件为:反应温度为 7080,催化剂用量为氯乙酸添加量的 15%左右为宜,氨水质量分数为 28%以上。在此条件下,甘氨酸转化率达到 99.0%以上,反应液中的甘氨酸产率为 98%,整个过程中甲醇的加入量也应该控制在一个合理的范围内,以达到产量的最大化。反应原理:氯乙酸和氨气在六次甲基四胺的催化作用下,反应生成氨基乙酸和副产物氯化铵。最后再通过精馏得到甘氨酸产品并滤去副产品。设计流程如图 1。氯乙酸乌洛托品溶解氨气 合成 醇析 离心醇洗烘干包装产品精馏回收甲醇副产物氯化氨图 1 设计流程方框图工艺流程叙述将氯乙酸、六次甲基四胺固体按工艺配比分别溶解成工艺指标要求含量的溶液,然后备入计量槽。首先向反应釜内投入六次甲基四胺水溶液,加热至一定温度后,开始滴加氯乙酸溶液,并通入氨气反应。反应过程中控制好反应温度和 pH 值,待加料结束后保温一段时间,通过甲醇醇析、真空抽滤、甲醇醇洗,分离出甘氨酸,并甩干、烘干、取样化验,包装合格后入库出厂。华北科技学院毕业设计(论文)III5、设计工艺特点(1)本设计采用目前国内普遍使用的氯乙酸氨解法。(2)除甲醇精馏是半间歇生产外,其他生产工序都是分批投料、间歇生产,生产周期为8小时,每天可生产3批。这样的生产过程,容易造成工艺指标控制不稳定,使产品质量、收率产生波动。因此,生产中各工序工艺指标的控制、操作过程关键因素的掌握,对产品质量的稳定,特别是产品收率的提高,有着十分重要的影响。(3)反应过程中,催化剂加入量、反应温度、pH值的调节以及反应时间长短等因素,对产品质量和收率有着决定性的影响。(4)影响醇析效果的主要因素有甲醇的加入量和醇析温度,因此为保证产品的收率,这两个条件必须控制好。6、设计计算结果数据本设计氨化合成釜各数据如下表 1:表 1 序号 项目 规格1 合成釜体积 3000L2 直径 1400mm3 筒体高度 1600mm4 夹套直径 1500mm5 夹套高度 1100mm6 传热面积 7.12m27 夹套厚度 4.88mm8 夹套封头厚度 6.01mm注:表中所列数据仅为部分重要数据,其他数据正文中都有体现。7、设计结论本设计所选设备满足年产 1 万吨甘氨酸合成的要求。通过对氯乙酸氨解法制备甘氨酸的研究分析,检索了相关文献和数据,对工艺参数进行了确定和优化,得出了可控制的工艺参数;选取了主要的反应设备对其进行了能量衡算和设计。通过对整个反应过程进行了物料衡算得出最后产品的纯度为 98.5%,其它杂质含量均符合质量标准。对生产工艺流程进行了设计,并对车间进行了布置和规划,理论上切实可行。年产一万吨甘氨酸生产工艺设计关键词:甘氨酸,生产工艺,收率,氯乙酸氨解华北科技学院毕业设计(论文)VANNUAL OUTPUT OF 10,000 TONS OF GLYCINE WORKSHOP PROCESS DESIGNDesign general description1.The design purpose and meaningGlycine is the more simple structure in the amino acid series, one of the non- essential amino acids in the human body. It has both acidic and basic functional groups in the molecule. According to the preparation process of glycine and the purity of the product can be divided into food grade, pharmaceutical grade, feed grade and industrial grade four kinds of products. The production, application and function value of glycine have attracted more and more attention in the world. In many countries, the production of food, medicine, fertilizer, pesticide, feed, etc. Cant be separated from its joining, or with some special effects to use it to change some of the flavor or quality of the product.2. Process design taskThe glycine production projects to Utopia and ammonia as raw materials, synthesis of glycine method for chloroacetic acid ammonolysis process, main equipment for ammonia synthesis reactor, distillation tower by batch production is expected production capacity of 1 million tons per year.3.Process design basis(1) The design plan descriptions of the undergraduate course graduation class of 2016.(2) Bingchen Zhu. Chemical reaction engineering, 2012 Beijing: Chemical Industry Press(3) Tianen Tan. Principle of chemical industry.2006, Beijing: Chemical Industry Press.年产一万吨甘氨酸生产工艺设计VI(4) Wuping Chen. Inorganic chemical engineering technology.2002, Beijing: Chemical Industry Press4. The design processGlycine production process a lot of, at present industrialization and has the prospects for industrialization production technology mainly in the chloroacetic acid ammonolysis process, Trey g (cstercker method), hydrogen cyanide, and biosynthesis method etc. This design adopts the method of ammonia chloride solution. The method according to the different raw materials, and can be divided into two processes: (1) alcohol or aqueous phase with methenamine, chloroacetic acid and ammonia (ammonia or liquid ammonia) synthesis as raw material; (2) in the aqueous solution with ammonium carbonate or carbamate amine, chloroacetic acid, ammonia as raw material synthesis. At present, the main production methods in China, the yield of about 70%, the latter yield is low (about 42%), it is rarely used in industrial production. At present, the main production methods in China, the yield of about 70%, the latter yield is low (about 42%), it is rarely used in industrial production. Because of urotropine in aqueous phase synthesis of glycine consumption is larger, and methenamine higher price, cant be recycled, so cost is higher, and with alcohol solution instead of water solution will greatly reduce the consumption of urotropine, thereby reducing the cost of production. Therefore, the current domestic popular with alcohol phase synthesis of glycine.In the process of preparing glycine by ammonium chloride, the optimum conditions for the process of ammonia hydrolysis were as follows: the reaction temperature was 7080, the amount of catalyst was about 15% of the amount of chloride and the ammonia water mass fraction was more than 28%. Under these conditions, glycine conversion rate reaches above 99.0%, glycine yield of reaction solution was 98%, methanol in the whole process of adding amount should also control in a reasonable range, in order to maximize yield reached.Reaction principle: the reaction of acetic acid and ammonium chloride was formed under the catalytic action of six methyl four amines by the reaction of acetic acid and ammonia. In the end, the glycine product is obtained by distillation and then filtered to the by-product.华北科技学院毕业设计(论文)VIIThe Fig.1 design processchloroacetic acidUrotropinsolutionnammonia synthesis Alcohol precipitationcentrifugalAlcohol washingdrypackingproductionDistillationMethanol recoveryBy-productAmmonia chlorideFig.1 Design flow block diagramProcess narrativeThe acid, hexamine solid ratio were dissolved according to process requirements into technical specification of the content of the solution, and then prepare the metering tank.First put into the reactor hexamethylenetetramine solution, heated to a certain temperature, it begins dropping acid solution, and ammonia gas reaction. During the reaction to control the reaction temperature and pH, until the end of the incubation period of the addition, by methanol alcohol precipitation, vacuum filtration, methanol, ethanol washing, separating glycine, and drying, drying, sampling tests, packaged into conformity library factory.5.Design and process characteristics(1) The current design uses ammonia acid solution commonly used in the country.(2) In addition to the methanol distillation is a semi-batch production, other production processes are fed-batch, batch production, the production cycle is 8 hours, to produce three 年产一万吨甘氨酸生产工艺设计VIIIbatches a day. Such a production process, likely to cause instability in the control process indicators, product quality, yield fluctuations. Therefore, the control of each step of the production process indicators, a key factor in the operation of control, product quality and stability, in particular to improve the yield of the product has a very important impact.(3)During the reaction, the catalyst is added to adjust the amount of the reaction temperature, pH value and duration of the reaction and other factors, yield and product quality has a decisive influence.(4) Analysis of the effect of the main factors affecting alcohol are added and the amount of alcohol precipitation temperature of methanol, so as to ensure product yield, two conditions must be controlled better.6.Design calculation result dataThe design ammoniated synthesis reactor each data in Table 1 below:Table1Number Project Specifications1 Synthesis reactor volume 3000L2 diameter 1400mm3 Cylinder height 1600mm4 Jacket diameter 1500mm5 Jacket height 1100mm6 Heat transfer area 7.12m27 Jacket thickness 4

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