华北科技学院毕业设计（论文）
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。
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年产一万吨甘氨酸生产工艺设计
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70~80℃，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 回收 甲醇 精馏 副产物 氯化氨 氨气 合成 醇析 离心 醇洗 产品 烘干 包装
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。 5、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。
华北科技学院毕业设计（论文）
（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 1 2 3 4 5 6 7 8 项目 合成釜体积 直径 筒体高度 夹套直径 夹套高度 传热面积 夹套厚度 夹套封头厚度 规格 3000L 1400mm 1600mm 1500mm 1100mm 7.12m2
4.88mm
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。
关键词：甘氨酸，生产工艺，收率，氯乙酸氨解
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年产一万吨甘氨酸生产工艺设计
ANNUAL OUTPUT OF 10，000 TONS OF GLYCINE WORKSHOP PROCESS DESIGN
Design general description
1.The design purpose and meaning
Glycine 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. Can’t 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 task
The 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. (4) Wuping Chen. Inorganic chemical engineering technology.2002, Beijing: Chemical
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华北科技学院毕业设计（论文）
Industry Press
4. The design process
Glycine 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, can’t 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 70~80, 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.
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