年产1万吨甘氨酸生产工艺设计说明书Word格式.docx

1、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

2、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。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

3、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。（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

4、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

5、，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ANNUAL OUTPUT OF 10，000 TONS OF GLYCINE WORKSHOP PROCESS DESIGNDesign general description1. The design purpose and meaningGlycine is the more simple

6、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

7、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

8、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 tow

9、er 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. Principl

10、e of chemical industry.2006, Beijing: Chemical Industry Press.（4） Wuping Chen. Inorganic chemical engineering technology.2002, Beijing:4. The design processGlycine production process a lot of, at present industrialization and has the prospects for industrialization production technology mainly in th

11、e 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

12、 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%, t

13、he 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 consu

14、mption 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

15、 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%. Un

16、der 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 chl

17、oride 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. The Fig.1 design processFig.1 Design flow block diagramProcess narrativeThe acid, hexamin

18、e 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 g

19、as 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 libra

20、ry 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 produ

21、ce three batches 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

22、 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

23、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:Table 1 N

24、umberProjectSpecificationsSynthesis reactor volumediameterCylinder heightJacket diameterJacket heightHeat transfer areaJacket thickness Jacketed head thicknessNote: The data listed in the table only some important data, other data are reflected in the text.7.Design conclusionThe design of the select

25、ed device meets the 10,000 tons of glycine synthesis requirements. Through research and analysis of the amino acid glycine solution preparation, retrieve relevant documents and data, process parameters to determine and optimize the process parameters can be obtained control; selected major reaction

26、apparatus its energy balance and design. Through the course of the reaction was material balance drawn purity of the final product was 98.5%, other impurities are in line with quality standards. Of the production process has been designed, and the layout and planning workshop, theoretically feasible

27、.KEY WORDS: glycine, production process, yield, chloroacetic acid ammonolysis process引言美国、法国、日本、中国等都是甘氨酸的生产与消耗的大国, 目前全球的生产总量约为250KT。在国外, 甘氨酸的使用范围较广泛,生产的技术工艺也较先进, 成品的含量或纯度也较高,而且在许多的食品和猪、鸡、牛、羊的饲料中及农药、除草剂等已得到广泛使用。甘氨酸化学合成主要有氯乙酸氨解法、施特雷克法（Strecker）、和海因法（Hydantion）三种。目前全国生产甘氨酸的厂家约有 50 家 左右,目前，制备甘氨酸主要有以下几种方

28、法 : （ 1 ） 以乌洛托品、氯乙酸 、液氨（ 或氨水 ）为原料，以水为介质的合成方法 ; （ 2） 与 （ 1） 类似但以醇为介质，以碳酸钱（或氨基甲酸钱 ）、氯乙酸和氨水为原料的合成方法 ; （ 3） 用氨基乙睛与酮类合成恶哇烷，再将其水解 ; （ 4） 乙内酞脉水解法等。目前国内主要采用氯乙酸氨解法制备甘氨酸，60年代以前，德国的Kraut用氯乙酸和氨水反应，在缓慢搅拌、室温下反应48小时以上，再经一系列复杂的后处理，才得到粗品，收率很低，成本高且再生能力很低。70年代后，法国人Henri Martin以乌洛托品、氯乙酸、氨水为原料在水相中合成，反应后，经醇析、过滤、精制、干燥制得。只

29、有70%左右的收率，生产周期长达40小时，纯度在90%左右1。后来用液氨代替氨水，收率达80%以上，此工艺成熟，目前国内生产厂家都在此方法前提下，不断的进行改进。自1969年实现工业化以来，国内许多专家对其进行了众多改进性研究，使甘氨酸收率由约70%提高至85%以上，产品甘氨酸含量从95%提高到98.5%。本设计所选用的工艺路线为国内较为成熟的氯乙酸氨解法，其中部分内容参考和引用了前人的技术成果，在此表示特别感谢。1 设计概论1.1甘氨酸的基本性质产品编号： FZS118 中文名称： 甘氨酸 中文别名： 甘氨酸;氨基乙酸,氨基醋酸 英文名称： Aminoacetic acid 英文别名： Gly ; Amino acetic acid; Aminoethanoic acid; Glycine 线性分子式： NH2CH2COOH等级： AR CAS号： 56-40-6 分子式： C2H5NO2 分子量： 75.07外观描述：白色结晶或结晶性粉末。味甜。溶于水，微溶于吡啶，不溶于乙醚。熔点:250（dec.） 密度：1.1607 沸点：233C物化性质：白色单斜晶系或六方晶系晶体，或白色结晶粉末。无臭，有特殊甜味，相对密度1.1607。熔点248（分解）。易溶于水，在水中