In-plant vocational training report

9
th

May 9

th

July2013

NIRAJ KUMAR BAIRAGI

IIT KANPURPREFACE
Industrial training plays a vital role in the progress of future engineers. Not only does it provide insights about the industry concerned, it also bridges the gap between theory and practical knowledge. We were fortunate that we were provided with an opportunity of undergoing Industrial training at DCM Shriram Consolidated Ltd (DSCL), Kota, one of the leading fertilizer companies in India. The experience gained during this short period was fascinating to say the least. It was a tremendous feeling to observe the operation of different equipments and processes. It was overwhelming for us to notice how such a big plant is being monitored and operated with proper co-ordination to obtain desired results. This project is aimed at developing the process design of the ammonia preheater used in the Urea Plant. Presently four shell and tube heat exchangers are being used for this purpose and we were asked to design a single shell and tube heat exchanger which can be used in place of the four heat exchangers. Kerns Method was used for the design purpose. During our training we realized that in order to be a successful process engineer one needs to possess a sound theoretical base along with the acumen for effective practical application of the theory. Thus, we hope that this industrial training serves as a stepping-stone for us and helps to be successful in future.

CERTIFICATE
This is to certify that NIRAJ KUMAR BAIRAGI, student of INDIAN INSTITUTE OF TECHNOLOGY, KANPUR has done his Summer Training at Urea Plant and Project Report entitled Summer Training Report is a record of candidates own work carried out by him under my supervision and guidance during the period 9 May to 9
th th

June, 2013 at Shriram fertilizers and Chemicals, Kota.

Mr. Hari Om Mishra Head of Department (Urea Plant)

ACKNOWLEDGEMENT
We would like to express our deep sense of gratitude to Mrs. Neha Agrawal, HR Manager for granting us permission to undergo training at DSCL, Kota over a period of 6 weeks and for making it happen and providing us with necessary inputs as and when needed. It is my profound privilege to express my sincere gratitude and heartfelt indebtness to my advisor Mr. K. M. Tandon, Manager, Fertilizer R&D and Mr. Hari Om Mishra, HOD Urea Plant, who inculcated in me the inspiration and enthusiasm to undertake this training that will always remain with me. The topic of training was selected based upon the latest developments and applications of the technology in the industry. I would also like to express my gratitude towards my mentor Mr. J.S. Choudhary, who has helped me in better understanding of the manufacturing process of urea theoretically and practically. He also made the visit to the urea plant worth by explaining functions of every equipment in detail. I feel immense pleasure in expressing my thanks towards Mr. Dinesh Prasad Bhatt, who has helped me in my project for developing the process design of Ammonia preheater. He was kind enough to guide me throughout the project and cleared all my doubts related to the project. Last but not the least, I would like to express my gratitude towards the technical and support staff at DSCL. They were very helpful and always encouraged us to get an insight in to the work. The help and support of my friends and colleagues during the tenure of the training was enormous and is acknowledged from the core of my heart. I express my gratitude to my institute, Indian Institute of Technology Roorkee for giving me an opportunity to grow and develop my thoughts for my future life. The teaching staff has been the path providers and the non-teaching staff the supporters.

BRIJESH KUMAR PAL IIT ROORKEE

TABLE OF CONTENTS
INTRODUCTION...................................................................................................................................
6

UREA PLANT AT SFC (DSCL KOTA).................................................................................................

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14 23 24 26

PROCESS DESCRIPTION................................................................................................................. NEEM COATED UREA...................................................................................................................... CRITICAL PARAMETERS OF PRODUCT QUALITY........................................................................ MAJOR ENGINEERING PROBLEMS................................................................................................

POLLUTION CONTROL AND INDUSTRIAL SAFETY TYPES OF POLLUTION IN FERTILIZER INDUSTRIES.......................................................................................................................................

27 30 30

PROJECT............................................................................................................................................. PROCESS DESIGN OF AMMONIA PREHEATER............................................................................

INTRODUCTION
DSCL: AN OVERVIEW
DCM SHRIRAM CONSOLIDATED LIMITED KOTA Shriram Fertilizers & Chemicals(SFC) is a large and great facility established in the Shriram Nagar, Kota by DSCL. SFC is managed by Mr. K.K. Kaul and his very capable team. By having Training Centre in its facility, SFC provides a great opportunity for training to more than 200 students every year.

DSCL comprises the following list of processing plants in it : Urea Plant Ammonia Plant PVC Plant Cement Plant Thermal Power Plant Carbide Plant Fenesta

1. Chloro- Vinyl business: Chlor- Alkali: This comprises of Caustic Soda(Lye and flakes), Chlorine and associate chemicals including Hydrochloric acid, Stable Bleaching powder, Compressed Hydrogen and Sodium Hypochlorite. The Company has two manufacturing facilities located at Kota (Rajasthan) and Bharuch (Gujarat) with full coal based captive power. The Companys total Chlor- Alkali capacity is 765 TPD. ii. Plastics Business : This is highly integrated, covering manufacture of PVC resins, Calcium Carbide and PVC Compounds PVC Resin is fully integrated with captive production of acetylene, chlorine and coal based power, located at Kota. which PVC compounds of the Company is the largest manufacturer the organized sector is backed by an innovative Polymer Application Developmentin Centre (iPAC) at Gurgaon, India. ~ 143 MW of Generating capacity is used to supply power to the above said businesses orPower sell power in the market depending upon the economic effectiveness. i.

2. Agri- Business: i. Urea: The Company has the dual feed naptha/ LNG based urea plant with a capacity of 3.79 lakh T.P.A., Located at its integrated manufacturing facility at Kota. It is currently operating on 100% LNG. ii. Agri- Inputs: This business provides complete basket of agriinputs to farmers community by offering a range of fertilizers, micro- nutrients, hybrid seeds, pesticides ets. Through its wide distribution network. iii. Bioseed (Hybrid Seeds): The Companys Bioseed business is present across the value chain i.e. research, production, processing, extension activities and marketing with established significant presence in India, Philippines and Vietnam. Further Company has initiated its operations in Thailand, China and Indonesia. iv. Sugar: The Companys sugar business cpmprises of 4 facilities with a combined capacity of 33,000 TCD in Central U.P. abd Cogen power capacity of 94.5MW. 3. Hariyali Kisaan Bazaar: These are Rural Business Centres which are a one stop solution to the multiple needs of the rural communities. The outlets provide full range of agri-inputs backed by customized agronomy services as well as other necessities and consumer goods. 4. Cement Business: The Cement business, located at Kota of 0.4 Million tonne capacity is based on waste generated from the Calcium carbide production process. 5. Fenesta: Fenesta building system manufactures UPVC windows(UnPlasticized PVC) and door systems under the brand Fenesta. It offers complete solutions starting from desgign , fabrications to installation at the customers site. 6. Other Businesses: Textiles: The Company has a smaal textile operation in the form of 14, 544 spindles spinning unit at Tonk in Rajasthan.

UREA PLANT AT SFC (DSCL KOTA)

Urea plant of SFC (DSCL, Kota) was commissioned in February 1969 with an installed capacity of 700 MTPD. The plant is based on Stamicarbons Total Recycle Process technology. The construction of the plant was done by Chiyoda Chemicals Engineering and construction Co. now known as Chiyoda Corporation. The plant was expanded in August 1974 to 1000 MTPD by installing of balancing equipment and an additional 120 TPD ammonia synthesis loop in the ammonia plant by making minor modifications in the Urea Plant. In a continuous endeavor towards energy conservation and de- bottlenecking, the plant has achieved utilization of 120% and can operate at the peak level of 1250-1300 MTPD. As a whole Urea Plant is totally dependent on the following plants: DM Plant Power Plant Plant Ammonia Other supporting services: Fertilizer Workshop Urea Bagging Plant P.C.L. Laboratory Urea Sale Department The Stamicarbon Process for the production of Urea using Ammonia and Carbondioxide as raw material is realized as total recycle process in total recycling of NH3(l) and CO2(g) and carbamate solutions. DSCLs Fertilizer Plant has an approved capacity of 379,000 TPA of Urea at its integrated manufacturing complexes at Kota Rajasthan. The Company is the lowest cost producer of Urea in the Pre-92 Naphtha based group and markets its products under the Shriram Urea brand. Shriram Urea is a trusted name and enjoys high brand equity amongst the farmers. The Company has an extensive distribution network over the entire Northern and Central India. In 2006-2007, the Fertilizer Plant was modified to be capable of having natural gas as its feed stocks besides naphtha. The Company had entered into a long term gas supply agreement to procure Natural Gas from KG Basin, meeting its full requirement. With the availability of Reliance KG D6 gas, plant has been operating on full gas since May09. 8

The use of Natural Gas (instead of naphtha) has major posi ves which include reduc on in Feedstock casts and consequently subsidy accruals by Rs.320 Crores, higher energy savings which boosted our earning and reduction in working capital which resulted in lower borrowings. The earning from the Fertilizer Business was up by 73% at Rs. $$.6 crores due to better efficiencies achieved by switch to gas from Naptha, Notification of revised NPS III schemes received and gain on account of additional production done in Fy 2009. The Company also was able to produce 4000 tonnes over the base production inspite of undertaking a maintaining turnaround of 25 days the year. In line with government policy on the fortified fertilizers , 22,014 MT of Uera was also converted to Neem Coated Urea. Efforts are continuously being made towads further improving energy Efficiency and reduction/ Containment of fixed expenses. The plants have been modified to use natural gas in 2006 and have been running fully on gas since May09 with the availability if KG D6 gas. In order to avail benefit of government policy on fortified fertilizer, 22014 MT of Urea was converted into Neem Coated Urea. Further, Studies are being made to coat urea with Zinc and Boron.In addition to abive, efforts are made to produce additional quantities of urea over reassessed capacity to avail benefit of government policy.

Urea: An Overview
Urea (identified 1773), the first organic compound prepared by inorganic synthesis (1828 Wohler) NH3 + HCNO CO(NH2)2 Commercial production started in 1992- Germany , 1931- USA and 1935- UK. Urea has been considered as slow release fertilizer since it must undergo two transportation Hydrolysis: CO(NH2)2 + H2O 2NH3 + CO2 Nitrification: NH3 Nitrite of Nitrate (Microbes, moist and warm soil)

India is the second largest producer and consumer of urea in the world. Urea is the most preferred fertilizer and constitutes about 72% of entire fertilizer consumption in the country. Low farm gate price (fixed by government) and high nitrogen content makes it a preferred choice of farmers. The demand and consumption of urea have been growing and the gap in demand / supply is being met by imports. During 2009-10 the total urea production in the country was 21.2 million MT and India had to import more than 5 million MT of urea to meet its demand. More than 90% of world production of urea is destined for use as a nitrogenrelease fertilizer. Urea has the highest nitrogen content of all solid nitrogenouds fertilizers in common use(46.7%). Therefore, it has the lowest transportation costs per unit of nitrogen nutrient . urea is highly soluble in water and is, therefore, also very suitable for use in fertilizer solutions( in combination with ammonium nitrate:UAN), e.g., in foliar feed fertilizers. For fertilizer use, granules are preferred over prills because of their narrower particles size distribution which is an advantage for mechanical application. The most common impurity of synthetic urea is biuret, which impairs plant growth. Urea is usually spread at rates between 40 and 300 kg/ha but rates vary. Smaller applications incur lower losses due to leaching. During summer , urea is often spread just before , or during rain to minimize losses from volatilization(process wherein nitrogen is lost to the atmosphere as ammonia gas). Urea is not compatible with other fertilizers. Because of high nitrogen concentration in urea, it is very important ti achieve an even apread. The application equipment must be correctly calibrated and properly used, drilling must not occur on contact with or close to sed, due to the risk of germination damage. Urea dissolves in water for application as spray or through irrigation systems. In Grain and cotton crops, urea is often applied at the time of the last cultivation before planting. In high rainfall area and on sandy soils (where nitrogen can be lost through leaching) andwhere good in- season rainfall is expected , urea can be side or top- dressed during the growing season. Top-dressing is popular on pasture and forage crops. In cultivating sugarcane, urea is side- dressed after planting and applied to each ratoon crop. India is the second largest producer of Urea in the world and also the second largest consumer of Urea as well. Urea is the most widely used fertilizer in India and Constitutes about 72% of entire Fertilizer consumption. High Nitrogenous

content as well as low farm gate price (which is fixed my government) makes it an attractive nutrient for the farmers vis-a-vis other nutrients.

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Ureas commercial use includes:

As a component of fertilizer and animal feed, providing a relatively cheap source of fixed nitrogen to promote growth. As a raw material for the manufacturing of plastics specifically, ureaformaldhyde resin. As a raw material for the manufacturing of various glues (ureaformaldehyde or urea-melamine- formaldehyde). The latter is waterproof and is used for marine plywood. As an alternative rock salt in the de icing of roadways and runways. It does not promote metal corrosion to the extent that salt does. As an additive ingredient in cigarettes, designed to enhance flavor. Sometimes used as browning agent in factory- produces pretzels. As an ingredient in some hair conditioners, facial cleansers, bath oils and lotions. It is also used as a reactant in some ready- to- use cold compresses for first-aid use, due to endothermic reaction it creates when mixed wuth water. Active ingredients for diesel engine exhaust treatment AdBlue. Used along the salts, as a cloud seeding agent to expedite the condensation of water in clouds, producing precioitation. The ability of urea to form clathrates (also called host- guest complexes, inclusion compounds and adducts) was used in the past to separate paraffin. As a flame- proofing agent. Main application grades of Urea are: Fertilizer Grade Cattle Feed Grade Technical Grade

Chemistry of urea synthesis

When CO2 and NH3 are brought together under the synthesis conditions of 200 atm the following reaction occur: 2NH3 (liquid) + CO2 (gas) NH4COONH4 +38.06 Kcal/mol NH4COONH4 NH2CONH2 + H2O (Urea) The first reaction is strongly exothermic, the secong is endothermic. The first reaction is spontaneous and complete , provide the heat liberated thereby is discharged , while the second is -522 Kcal/ mol

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slowly involving equilibrium reaction, due to which only par of the carbamate is converted into urea. When both the raw materials are presented in stoichiometric ratio, the equilibrium is about 46% conversion. At higher N/C ration in the original synthesis moisture, the equilibrium reaction 2 shift to right by Le Chateliers principle.

PROPERTIES OF UREA
Compound Molecular Formula Molar Mass(g/mol) Appearance Density(g/m3) Melting Point Specific Gravity Ur e a CH4N2O 60.06 White solid without any odour 1. 3 2 132.7C 1.335 1 0 8 g /100ml (20C) 1 6 7 g /100ml (40C) 2 5 1 g /100ml (60C) 4 0 0 g /100ml (80C) 7 3 3 g /100ml (100C) pKBH+ =0.18 4 6. 6 0. 3 2

Solubility in Water

Basicity(pKb) Nitrogen % Content Specific heat @ 20C (Cal/gC)

Heat of Sol. In water (endothermic)(Cal/gC) Critical relative humidity 20C 30C

5 7. 8 8 1 % 7 3 %

SPECIAL QUALITIES OF SHRIRAM UREA

Dust Content: Dust content in Shriram Urea with new bucket has reduced to 0.2% to 0.4% with old bucket. Therefore there is very less change of cake formation now.

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Brightness: Shriram urea is brighter as compared to few brands available in the market as there is not possibility of oil content in the process it is always milky white.

Moisture Content: Shriram Urea is produced with a process which results a least amount of moisture and biuret content. A study Conducted by analyzing different brands of Urea from retailers outlet shows that the moisture content in Shriram urea is 0.27% which is less than other brands average 0.67%.

Biuret: Shriram Urea Contains about 0.45% biuret. SFC urea Contains biuret less as compared to other brands.

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PROCESS DESCRIPTION
Urea plant at DSCL operated on the Stamicarbon Total recycle basis. Urea is commercially manufactured using ammonia and carbon dioxide as raw materials coming from the Ammonia Plant. At the end of process description a section on recovery of some important compounds like ammonia and water is provided which consists of a figure which explains how exactly ammonia is recovered from the different section of the plant followed by a brief explanation of Hydrolyser Stripper Unit. The plant includes the following sections: NH3 and CO2 Compression Synthesis Section 1
st nd

Stage Recirculation

2 Stage Recirculation Crystallization, Drying and Remelting Prilling and Solid Handling Hydrolyser Stripper Unit

Raw Materials: The basic raw materials used in production of urea are ammonia and carbondioxide which are supplied by the Ammonia Plant. 1. Ammonia a. Purity = 99.0 % by wt. (min) b. Oil = 10 ppm (max) c. Moisture = 1.0 % by wt. (max) 2. Carbon-dioxide a. Purity = 96.0 98.5 % (Dry Basis) NOTE: Anti-corrosion air mixed with CO2, in a proportion so that O2 content in the supplied gas is kept between 0.4 0.7 % and CO2 purity is at least 96 % by volume. Utilities: Steam Panel I/C regularly monitors the pressure , temperature and flow of 14K & 4K steam supplied by Power & Ammonia Plant every hour at Control Room.

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Cooling Water The conformance of cooling water quality is monitored by Ammonia Plant on daily basis and records are kept. Its temperature, pressure and flow are monitored by Urea Panel I/C hourly. The supply characteristics of utilities for maintaining essential process control I/C are as follows:UTILITY 14K Steam 4K Steam Cooling Water TEMPERATURE ( ) 193-198 155 - 160 20 - 38 PRESSURE (kg/cm2) 11.8 14.0 3.5 4.5 2.5 3.3 FLOW 3.0 9.5 3.0 8.0 5.5 9.5 (MT/hr) (RX 8) (RX 2.5) (RX 1200)

NH3 AND CO2 COMPRESSION:

For synthesis reaction of Urea to happen, we need a finite amount of 2 temperature (190 ) and pressure (200 kg/cm ). For attaining this pressure, following procedures are followed: From a pressure of 1.43 abs pressure & 40 temperature, CO 2 is sent for compression at Ammonia Plant end only using 3 reciprocating 2 compressors to be compressed to about 200 kg/cm after the mixing of CO2 with anti-corrosion air (not being inert more than 4% by volume and 3 less than 15 mg/NM sulphur). About 0.5% of O2 is introduced to CO2 before compression as its presence helps stainless steel to resist the corrosiveness of Carbamate; and NH3 is pressurized at Urea Plant using ammonia feed pumps. Liquid ammonia at 23 atm gauge pressure & temperature of 40 maximum goes for filtration in Ammonia Filter Tank and then (with 10 ppm as maximum oil content left) to Ammonia Buffer Tank. Ammonia Reflux Pumps are then used to transfer the ammonia to the high-pressure Ammonia Feed Pumps(to prevent vapor lock in the pump, ammonia inlet temperature to the pump must be about 10 below the saturation temperature at the existing inlet pressure). Pressure of the discharged ammonia from Ammonia Feed Pumps is about 2 210 kg/cm . Flow of the pressurized ammonia is regulated by the control valve FRC 504-1/2/3/4 provided in the discharge to suction bypass of each pump. Pressurized ammonia now heads up to Ammonia Pre-Heaters 23-501 A/B/C/D which are shell & tube heat exchangers. After gain of sufficient heat to maintain desired reactor temperature (required ammonia temperature 85 ), ammonia is transported to mixer 24-501. During the start up of the Plant, the whole of heater has to be supplied with middle pressure steam so as to evaporate the ammonia and to heat the vapor to about 150 in order to prevent cooling down of reactors preheated with 14

K steam. For shutdown purpose line from HP flush water pump 31-513 is installed in order to flush the inlet of the NH3, CO2 and Carbamate line of mixer24501 and the outlet line of reactors 24-502 B. 15

SYNTHESIS:
The feed components (pressurized NH 3 and compressed CO2) are pured in the orifice mixer 24-501 to mixed thoroughly which also have concentrated Carbamate (H2N-CO2-NH4) solution (43% NH3, 31% CO2, 21% H2O & 5% Urea(H2N-CO-NH2) all by weight) coming from the recirculation section. In mixer, about 90% of the CO2 feed is spontaneously converted into Carbamate. The heat evolved during this reaction is being absorbed by the feed components themselves.

The system NH3-CO2-H2O shows at a certain pressure a certain temperature. Total pressure inside the mixer is maintained by the use of let down valve PRC2 502 at 200 kg/cm which in turn results in the temperature of about 172-178 . At constant pressure this temperature is supposed to change only with the change in the NH3/CO2 or H2O/CO2 ratio in the reactor feed.

An increase in NH3/CO2 ratio lowers while increases in H2O/CO2 ratio results in higher mixture temperature. Under design conditions NH3/CO2 ratio is 4 and H2O/CO2 ratio is equivalent to around 0.64, the optimum temperature in the reactor remains at around 190 . The overall heat of reaction inside the reactor is not sufficient enough to reach this required optimum temperature. Therefore, some extra heat as sensible heat has been put in the ammonia feed so as to control the optimum temperature. Inside the reactor the conversion of about 64% of total CO2 feed into urea has been observed; mentioned figure is being called the CO2 conversion per pass.

RECIRCULATION:
Effluent from the two reactors consisting about 32% urea, 13% CO2, 37% NH 3, 18% H2O (by weight) and some of the unconverted Carbamate enters the first re-circulation section. This part of the plant practically separates all the Carbamate, the excess of ammonia and part of water from the remaining urea solution. This separation takes place in two stages, the first stage operating at around 20 kg/cm and the second at 3 kg/cm . First Stage: The reactor effluent is throttled through the letdown valve to about 20 atm g pressures. The temperature of solution reduces due to evaporation of large amount of excess ammonia and part of the available Carbamate dissociating into ammonia and carbon dioxide. These vapour escape from the top of first
2 2

stage rectifying to MPCC (Middle Pressure Carbamate Condenser). The

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temperature here drops to about 132 as heat required for the gas formation in here is being extracted as sensible heat from the incoming synthesis solution. The remaining solution is distributed over the stainless steel IMTP (Intallox Metal Type Packing) rings of first stage rectifying column. Rising vapours in the coulumn are cooled by this solution reducing the water vapour content in the gas stream considerably. The solution temperature increases meanwhile to about 134 . The liquid from the first stage rectifying column is then fed to the first stage heaters and thus heated to about 160 . The heat input causes an additional vaporization of ammonia, carbon dioxide and water from the solution, the gas phase is separated from the liquid phase in first stage separator. The outgoing solution is transported to the secondary recirculation system containing 58% urea, 4% CO2, 10% NH3, 28% H 2O by weight. The gas phase out of first stage separator is returned to the bottom of first stage rectifying column in which as mentioned before, the water content of the gas stream is reduced. The vapours leaving the first stage rectifying column are introduced into the bottom of the MPCC, through submerged gas distributers, into a Carbamate solution. In this condenser nearly all the water vapours will be absorbed and about 90% of the gaseous CO2 is converted into the Carbamate. The non-absorbed gases will rise through the condenser, leave at the top and are together with Carbamate solution, introduced into level tank. During the formation of Carbamate from gaseous component ammonia and carbon dioxide and during the condensation of the entering water vapor heat is evolved in the condenser. This heat is removed by the conditioned cooling water flowing through the hairpin tubes of the condenser and circulated through water cooler by conditioned water pump. The temperature of conditioned cooling water is controlled by a three way valve in the bypass line of the water cooler. The pressure in the cconditioned cooling water system is maintained by a head vessel on top of the prilling tower. In the bottom of the MPCC a weaker Carbamate solution from washing column is introduced by means of intermediate Carbamate pump. Together with gaseous CO2, condensed water vapour and ammonia, a concentrated Carbamate solution is produced having a temperature of about 100 the boiling of the solution at the existing pressure and approximate composition by weight of 43% NH 3, 40% CO2, 12% H2O, and 5% urea. The solidification temperature of this is about 78 In the level tank the gas phase is separated from the liquid phase. The concentrated Carbamate solution is recycled to the orifice mixer by centrifugal Carbamate pump or first stage Carbamate pumps. The level in level tank is controlled by a control valve LRC-1501 or by regulating the speed of Carbamate pumps. The non-condensed NH3 and CO2 gases leave the top of level tank and are piped to the washing column. The NH 3/CO2 in the gas is approximately 80.In the bottom of washing column this gas is distributed through submersed through submersed gas distributor in the Carbamate

solution.

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In the washing column the remaining water vapour will be absorbed and about 95% of the gaseous CO2 is converted into the Carbamate. The non-absorbed gases will rise through the column. In the top part of the column which is filled with raschig ring, a spray desk is fitted, onto which ammonical water is fed from the scrubber. Thus gaseous CO2 and water vapour are completely removed from the rising gases, so that a pure NH 3 gas, with a temperature of about 50 leaves the washing column. During the formation of Carbamate from the gaseous components NH3 & CO2 and during the condensation of the entering water vapour heat is evolved in the bottom of the washing column. The temperature is controlled by means of ammonia reflux. This ammonia reflux, being vaporized absorbs the heat of reaction. In the bottom of washing column a weak Carbamate solution from stage nd Carbamate condenser is introduced by means of 2 stage Carbamate pump. Together with the gaseous CO2, condensed water vapour and NH 3, a concentrated Carbamate solution is produced. The solidification temperature of this solution is about 70 . The concentration can be adjusted by means of the amount of water fed to washing column via ammonia scrubber. The concentrated Carbamate solution is recycled to MPCC by intermediate Carbamate pump. A control valve LRC-503 controls the level in the washing column, which is in the discharge of their pumps. The ammonia gas from washing column is condensed in ammonia condensers A 1, A2 and B. Normal cooling water is used. The pressure of 20 atm g is sufficient for optimum condensation purpose. The liquefied ammonia is flowing into ammonia buffer tank. The non-condensed vapours from the ammonia condenser are fed to the scrubber, which have small amount of ammonia vapour. Here ammonia is dissolved in the process water and heat is taken out by cooling water. The solution from the ammonia scrubber level tank is fed to the washing column and vapour with inert will escape to the atmosphere. Nearly all of inert will escape in the first recirculation through PRC-503. These non-condensable inert will carry gaseous ammonia out of the system, the quantity being dependent on the inlet cooling water temperature and the plant load. This ammonia is absorbed in water at 20 atm g pressure by passing the gas stream through ammonia scrubber. The pressure of the first stage recirculation is automatically control by the control valve PRC-503 in the off gas line from scrubber level tank through which the inert are vented to the atmosphere. Second Stage: The solution leaving the bottom of the first stage re-circulation separator passes through level control valve LIC-502 which gives the pressure drop from 20 atm to 30 atm g. Because of pressure drop, ammonia and CO2 will gasify during the expansion. The heat required for this gas formation is extracted as sensible heat from the solution and causes a temperature drop to about 116 . The remaining

solution is distributed over the stainless steel rings of the second stage rectifying column. Rising vapour in column are cooled by this solution reducing the water vapour content in the gas stream considerably. The solution temperature increases meanwhile to about 125 . 18

In the second stage re-circulation heater almost whole of CO2 and NH 3 still being present in the solution are removed by heating to about 150 . The gas phase is separated from the liquid phase in second stage re-circulation separator. The solution of about 70% urea, 0.3% CO2, 1% NH 3, 28.5% H2O, 0.4% biuret (by weight) flows to flash drum. The gas phase from the separator is returned to the bottom of second stage rectifying column in which, as described before the water content of the gas is reduced. The major proportions of the ammonia and CO2 in the vapours leaving second stage rectifying column are condensed in two (in series) second stage Carbamate condensers namely old and additional. The heat of reaction evolved during the condensation of water vapour, ammonia absorption and Carbamate formation is absorbed in cooling water flowing through the tubes. The solution and the non-condensed gases leave at the top of old Carbamate condenser and are separated in old level tanki 22-506. The liquid phase is transported by means of second stage Carbamate pump to washing cooling column. The gas phase is introduced in the bottom of the second stage additional Carbamate condenser, which is also of submersed type. Here the remaining gases condensed in a weak Carbamate solution. A water connection is made to bottom of the additional Carbamate condenser in order to be able to adopt the concentration of the solution to the optimum condition. The solution over flows to the second stage additional Carbamate condenser level tank from where it is transported to second stage old carbamate condenser through second stage booster pump. The pressure of the second stage re-circulation is controlled by FRC-505 in the off gas line from additional Carbamate level tank, through which the inert are going to the vent stack. Crystallization, Drying and Remelting: The solution from second stage re-circulation separator is throttle in valve LIC504 and enters flash drum, which is operating under the vacuum. Due to this pressure drop a considerable amount of water vapour and some ammonia will escape from the solution, decreasing the solution temperature. By means of air valve PRC-1501 in the vapour line to ejector to urea flash drum condenser, the pressure in the flash drum is controlled in such a way that the outgoing liquid is at about 90 . The resulting concentration of urea in the solution being fed into urea buffer tank is about 70-75%. Urea solution pumps are installed to transport the urea solution via urea solution filter to the crystallization section. The concentration of UBT and Mother Liquor Tank(MLT) solution are checked by measuring crystallization temperature point and comparing it with concentration vs crystallization point chart. The incoming urea solution, part of which is going to the centrifuges for rinsing, is mixed in MLT with the liquor effluent from the centrifuges. MLT is provided with a stirrer which is not in use, in order to dissolve the crystals strain from

sieve bends and centrifuges. From MLT the urea solution is pumped to the evaporator. This flow is controlled, as per process requirement in the evaporator;

19

the solution is concentrated under a pressure of 300-mm Hg abs. Pressure is controlled through PRC-507 C/V. The concentrated solution of about 115 is mixed in the MLT with sieve bends solution from partial separation and the crystal strain from the centrifuges. The liquor from the MLT is pumped to crystallizers in which a crystal suspension is in circulation. In crystallizers, evaporation of the solvent take place under a pressure of 95 mm Hg abs and super saturation occurs in the surface region. In the down coming stream the super saturation will release on the circulating crystals until saturation of the liquid is obtained. The crystallizers are provided with the level indicator controller, which regulate the fflow to the crystallizers. The crystal suspension is extracted from the bottom and pumped by slurry pumps to sieve bends with a fixed capacity of 3 about 90 m /h. Each by means of the sieve bends crystal slurry concentration is increased to about 45% by weight. From the sieve bend the slurry is introduced into No.1 divider box which transfer it to the centrifuges. The mother liquor separated from the slurry by means of sieve bends flows into MLT. From this tank the biuret concentration in the mother liquor relates to a maximum concentration that depending on the crystallization temperature to be sure on the urea is crystallizing. In order not to exceed this maximum biuret concentration as much biuret in the form of mother liquor as corresponds with the fresh biret input must be continuously purged. The biuret concentration in the system is about 8-9%. The centrifuges are designed such that the crystals may be washed with a part of the frest urea feed, in order to lower the final biuret content. The vapours leaving the crystallisers and the evaporation section are condensed. The required absolute pressure in the condenser is maintained by the means of an evacuating system. The pressure is kept constant by pressure controllers, which admits air before the ejectors. The washed urea crystals separated off in the centrifuges fall in to screw feeding system for the pneumatic drying system. The crystals still contain maximum 1.5% of water and are dried in the pneumatic drying system to final moisture content of 0.3%. For pneumatic conveying of the crystals air is taken in via a filter and a blower for drying purposes this air is heated in a steam heater to a temperature of about 120 . This temperature is automatically controlled. The heated air takes up the wet crystals and in transporting them through a pneumatic drying tube,

the air takes up the moisture so that a final moisture content of the crystals of 0.3% is reached. 20

To add additional heat to the system, the pneumatic tube is provided with steam jackets, on which a constant steam pressure is maintained. The separation of crystals from the air is carried out in cyclone. The temperature is about 80 . The product separated in the cyclones goes to the melting equipment i.e. remelter. The product is fed in to remelter where it is suspended in to a circulating stream of molten urea. The slurry is pumped from remelter to remelter heater where the suspended urea crystals are melted. The temperature in the remelter is kept around at 138 . The melt is returned to the remelter, out of which it over flows to a second heater. This heater is installed to melt the crystals still present in the remelter over flow. Out of this heater the solution flows via a filter to the rotating bucket. The entire melting equipment is designed in such a way that the retention time is as short as possible in order to diminish biuret formation during remelting as much as possible. The inlet and outlet of the remelter are tangential; these two minimize the hold up in this vessel. By choosing a high circulating velocity in the remelter circuit, high heat transfer rates can be obtained and the dimensions of the heater can be as small as it is possible. Prilling and Solid Handling: The concentrated urea melt from the remelter system is fed to urea melt distributor which is designed for net production of 1000 MTPD urea. The bucket is provided with a high level alarm in order to warn the operator when there is a danger of bucket over flow which might occur when the holes are getting clogged. Therefore two buckets are provided. The prill bucket distributes the urea melt in fine droplets over the tower diameter. During their fall the urea solidifies. The heat of solidification is carried off by air sucked in through openings at bottom of the tower. The urea prill accumulating on the bottom of the tower are scrapped in to a slit by sccrapper. Conveyer loading chute transports the product into prill cooler where prills temperature is brought down and under size material is removed & discharged to dust dissolving tank. The product is transported via the product conveyor to the storage. In dust dissolving tank, provided with a stream cooil and a mixer, the over size and the dust are dissolved in to the urea solution coming from UBT. The resulting solution flows to urea storage tank.

HYDROLYSER SECTION
Feed to System: Desorption feed water from DWT is pumped through desorption feed pump to the LP absorber. The temperature of desorption feed water varies between 40-

50 and flows between 30-35 m /h. 21

Desorption feed water from desorption feed pumps is sprayed at the top column where it absorbs NH3 vapor coming from reflux condenser level tank. CO2 is fed at the bottom which helps in fixing NH 3. Heat exchangers are operating as feed effluent exchangers. First Desorber: Desorption water after absorbing NH3 and CO2 in LP absorber and exchanging heat in desorber heat exchanger is introduced in first desorber for stripping out ammonia and CO2 in it. Hydrolyser Stripper Column: This is the main part of system where urea is hydrolyzed into ammonia and carbon dioxide, heat of reaction is given by 36K steam. Vapors from hydrolyser 2 are sent to first desorber pressure is maintained 18.5 kg/cm . Second Desorber: The outlet of hydrolyser column after hydrolyser heat exchangers is fed to No. 2 desorber here remaining ammonia and carbon dioxide are stripped by 4K steam vapors from No. 2 desorber is sent to No. 1 desorber where it is used as stripping agent for ammonia and CO2. Stripped solution is taken to desorption heat exchanger where it is cooled. Reflux Condenser: Vapors from desorber outlet at 112 are condensed here up to 54 , the condensed vapor and liquid mixture are sent to reflux condenser level tank at 54

22

NEEM COATED UREA

The unit consists of three main parts: Concentrate Preparation Unit Emulsion Preparation Unit Spraying Unit

Concentrate Preparation Unit

In this unit 50 litres of neem oil and 2-5 litres of emulsifiers are added together and mixed thoroughly with the help of fan jet nozzles. The neem oil and the emulsifier mixture prepared are taken into emulsion preparation tank via two ejector nozzles.

Emulsion Preparation Unit

The concentrate produced in concentrate preparation tank is transferred to emulsion preparation tank and 150 litres of warm water is added to it. The solution is stirred by circulating through specially designed ejector nozzles, mixing nozzles and acoustic nozzles. Emulsion prepared in emulsion preparation tank is transferred to emulsion buffer tank.

Spraying Unit
This unit consists of calibrated spray nozzle to spray neem oil water emulsion drawn from storage tank, on to the curtain of urea prills at conveyor no.2. Oil emulsion at the rate of 120-150 litres/hr is sprayed for a prilling load of 40-50 Mt/h to get minimum of 300-500 PPM neem oil coated urea prills.

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CRITICAL PARAMETERS OF PRODUCT QUALITY

Colour: Product should be milky white in colour. If colour is not OK, following things were checked: O2% in CO2 should not be less than 0.5 % and air in the first stage should be about 12m /hr. In case product contains oil, check urea solution, Filter Cloth might have torn out. Wash sieve bend for the proper filtration Bulk density: It is to be maintained between 700- 760 Kg/m . It is to be maintained with bucket speed. At higher speed bulk density will be more and vice versa. Sieve analysis: Prill size of more than 2.8 mm is to be maintained at less than 4%. Prill size of less than 1.0 mm is to be maintained at less than 4%. Prill size of less than 0.3 mm is to be maintained at less than 0.3% Prill size is to be monitored with bucket speed and confirmation with analysis by PCL. At higher bucket speed, prill size below 1mm will be more. At lower bucket speed, prill size above 2.8 mm will be more. Maintain the optimum bucket speed. Clean the bucket cone if desired prill size is not obtained.
3 3

Moisture: It is to be maintained 0.30% by weight. If it is high, check: Moisture content of crystals from centrifuges which should not exceed 1.5% by weight. Check and wash the sieve bends for proper filtration. Adjust load on centrifuge and pusher strokes accordingly. Confirm from PCL analysis. Free ammonia: It is to be maintained less than 0.02%.If it is increases, following things has to be checked: Free ammonia in UBT, which should be less than 0.20%. Vacuum in Flash drum Condenser, which is to be maintained at less than 2 0.5% Kg/cm absolute.

24

Biuret: It is to be maintained below 0.65 and maximum limit is 1% as per SCF standard. If it is increases, following things has to be checked: Remelter heater temperature which should be between 137-139C. Ensure that indication is correct and instrument is calibrated. Biuret and rinsing flow to individual centrifuges. Increase rinsing flow to the particular centrifuge which contains high biuret.

25

MAJOR ENGINEERING PROBLEMS

Corrosion:
An important problem is the highly corrosive nature of the urea and the Carbamate solution, as well as their vapours involved in the process. In the stamicarbon process corrosion is restricted to a negligible amount by utilizing its grade through current stainless steel and non-expensive patented oxygen is injected to maintain an oxidizing atmosphere. If for any reason the oxygen supply is cut-off, the unit should be shut down immediately.

Biuret:
A problem faced by every urea maker is the formation of biuret during the production process. Biuret in fertilizer grade is considered harmful because of its damaging effects on several kinds of vegetation. A biuret content of 1% is considered as a safe limit.

Formation and Control:

During the formation of urea, biuret is formed as H2N-CO2-NH4 H2N-CO-NH-CO-NH2 + NH3 - heat

This is a slow and endothermic reaction and show that if one mole of ammonia is epelled out from two mole of urea, biuret is formed. The Biuret is favoured by following conditions: High urea concentration. Low Ammonia concentration/ low vapour pressure. High temperature. Longer residence/ retention time at temperature. Since the biuret is toxic/ harmful to plants/burns down green leaves. Its content in fertilizer grade urea has to keep as low as possible. This means that the conditions are to be avoided particularly in places where there is sufficient time for biuret formation. Permissible maximum biuret content in fertilizer grade urea is 1.5% wt.

26

POLLUTION CONTROL AND INDUSTRIAL SAFETY TYPES OF POLLUTION IN FERTILIZER INDUSTRIES

I. ATMOSPHERE POLLUTION BY UREA DUST FROM PRILLING TOWER Pollution Control board standard (PCBS) for urea dust content at out of dut 3 3 collector is 50 mg/m (max.) and 69 mg/m (max.) NH3 and Urea. EFFLUENT (PROCESS CONDENSATION FROM THE SYSTEM) PCBS = NH3 Content 5ppm (max) UREA content 5ppm (max)
FREE AMMONIA FROM AMMONIA SCRUBBER PCBS = 332 Kg/h Exhaust gas (max) WASTE WATER PCBS = 100mg.1 ammonical nitrogen (max)

II.

III. IV.

Pollution Control
Fertilizer plant deal with hazardous and toxic materials which are extremely poisonous and can ever cause death. SFC has been aware of it and has taken actions which are beyond economic consideration. As A result SFC has been awarded the state pollution control award. In the fertilizer plant, environment consideration have been adopted right from the intial designing of plant besides of plant healthy operation practices. Hazardous chemicals and effluent stream are recycled as far as possible and the discharge leaving plant equals if not better, the normal laid down by the control board standards.

Safety Features
Safety of workers and equipment in the plant is of prime importance in any industry extensive, Safety measures are taken in the plant due to hazardous and toxic materials like naphtha and ammonia and also other highly inflammable and explosive gases like synthesis gas, H2 gas etc. Besides handling of slow material the fertilizer plant operates at high pressure and temperature. The ammonia plant is designed so as to shutdown automatically in case of any

emergency. All hazardous material, chemical goes into specific drums and vessels. They do not leak into the atmosphere. 27

Safety measures have to be full proof interlocks and trip devices have been provided to product the plant and machinery from damage in case of any disoperation due to any error by both the operating staff or malfunctioning of instruments. In addition to this firefighting arrangements in the form of fixed installations and a mobile fire brigade are available to fight and minimize the damage in case of fire. SFC has a separate safety department which caters all the plants and is responsible for all safety measures. Their main functions are: Permit system observance Hot jot permit work General Vessel/confined space entry permit Work at high permit Excavation work permit General safety observation guarding monitoring Machine belt safety monitoring Conveyor control Hot job proof material/fitting Explosion Alarms No smoking First aid fire extinguisher Toxic hazard management Good Engineering practice monitoring The main hazard in urea plant is: Ammonia gas: of the raw materials in the plant is ammonia. Ammonia forms an One inflammable mixture in also air in the range of 16-25% concentration and it can lead to a cold burn also. We have Ammonia feed pumps. In case of heavy ammonia leakage it can form an inflammable mixture. This mixture can catch fire in presence of ignition source. However as ammonia is highly dispersible gas in air, it gets diluted and can create only a rare chance of forming explosive mixture. Normally we used ammonia PPEs for isolating the Ammonia leakages in the plant.
Personal Protective Equipments(PPEs) used in Plant:

Helmets, goggles, hand aprons, BA sets, ammonia canister mask and online sets. Self-contained breathing apparatus, Ammonia canister Masks and onBA line BA set are gloves, 28

available in the prominent locations. It is necessary to use PPEs in case of Ammonia leakage for isolating the leak point. Training work force awareness in addition. Emergency response plans for each plant and a total complex have been etched and strict monitoring and adhesive is expected in each plant.

29

PROJECT
GIVEN:

PROCESS DESIGN OF AMONIA SCRUBBING COLUMN

Gases coming from ammonia condenser at 155.25kgmol/hr containing 82.13% of ammonia . Allowable concentration of ammonia in exit gas mixture is 1.05% . Absorbing agent :- Liquid coming from Desorprion water tank Flow rate = 182.33 kgmol/hr Ammonia = 5% Carbon dioxide = 0.7% Urea = 0.3% Water = 94% Cooling water :Flow rate = 100om3/hr Inlet temp = 35 C DESIGN: As we now that absorption of ammonia is exothermic process which release much heat when we absorbed so if we design a normal absorption tower then we cannt control this much heat and temperature will rise and if temp will rise then absorption of ammonia is cann;t be possible . To control this much heat I have designed a vertical tower which containing tubes for cooling . So basically its like a shell and tube heat exchanger. So Amount of heat to be removed = 1322.8664 *103 Kcal/hr Now to find heat transfer area and heat transfer coefficient I used iterative method . Assume U = 500 Kcal / hr m2 oC (existing systems) R= (T1-T2)/(t2-t1) = 0 S = (t2 t1)/(T1-t1)= 0.45 LMTD for system = 13.23 oC Tube = 25.2 mm (1 in) Iteration 1) Heat transfer area(A) = Q/UT = 200.12 m2 Tube area (at) = 0.79168 m2 No. of tubes = 252.778 Shell dia = 25 in Shell side heat transfer coefficient :Area of shell(as) = 0.138 ft2 Flow rate(w) = 7275.25 lb/hr Mass Velocity (Gs) = 52681.058 lb/hr ft2 Reynolds No. (Res) = 3317.8 (Kern Table 29) ( Kern Eq. 7.3 )

Now So

JH = 30 and (c*/K)1/3 = 4.17 760.89 Kcal / hr m2 oC Tube side heat transfer coefficient :at = 0.594 at = 0.293 ft2 Flow rate (w) = 220462.25 lb/hr Gt = 752944.8 lb/hr ft2 Velocity of fluid (V) = 3.377 D = 0.0722 Ret = 34699.5 hi = 799.8 Kcal / hr m2 oC hio = 695.8 Kcal / hr m2 oC Overall heat transfer coefficient :Uc = 363.45 Kcal / hr m2 oC Ud = 173.9 Kcal / hr m2 oC Iteration 2) Uc = 197.54 Kcal / hr m2 oC Ud = 124.04 Kcal / hr m2 oC Iteration 3) Uc = 193.43 Kcal / hr m2 oC Ud = 122.40 Kcal / hr m2 oC So Finally Final Heat Transfer Area = 125.94 m2 Length of tube = 4m No of tube = 390 Shell Outer Diameter = 29 in Tube Diameter = 1 in Baffle spacing = 21.5 in

(Kern figure 28 )

ho =

(Kern Eq. 6.15(b) )

(Kern Table 10 )

(Kern Table 10) (Kern Figure 25) (Kern eq 6.5 ) (Kern 6.38) (Kern 6.13)

31