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<! Hindustan Petroleum Corporation Limited

Standing Operating Procedure for Vis-breaker Batch Reactor-II

Report No:

April’13

HPCL Corporate R&D Centre Bangalore Prepared by:								Reviewed by:

Rahul Pandey

Standing Operating Procedure for Vis-breaking Batch Reactor Back ground: Vis-breaking is a thermal cracking process, used for upgrading refinery residues viz VDU residues to gas, LPG, naphtha, middle distillates and visbroken tar. Vis-breaking comes from two words “viscosity” and “breaking”. The economic advantage of vis-breaker is linked to the ‘viscosity breaking effect’ which allows a reduction of cutter stock required to meet the fuel oil specification. The operating variables of vis-breaker are temperature, pressure and residence time. These variables can be interchanged within certain limits to achieve certain residue conversion. Thermal cracking severity can be increased either by increasing the temperature or residence time in order to get more conversion. In general, severity of the vis-breaker is limited by coke laydown and tar stability. From the literature studies, it was envisaged that VB tar stability can be increased by using catalysts or additives. In this context HPCL R & D has started research in the field of Vis-breaking process to optimize the operating parameters like temperature, pressure, residence time and catalyst dosages. To understand the impact of the operating parameters as mentioned above HPCL R&D has procured 1L batch reactor from M/s Amar Equipment for carrying out experiments in the field of vis-breaker with Vacuum Tower Bottoms as feed.

. HPGRD have the following analytical equipments which will be used for quality analysis of vis-breaking feed and product a)	HTSIMDIS- b)	Stabinger Viscometer- c)	S-value analyzer for product stability- d)	Sulfur analyzer- Process Description: Vis-breaker batch reactor-II consists of the following sections 1)	Reactor 2)	Reactor auxiliary cooling system 3)	Heating section 4)	Stirrer with external motor 5)	Condenser 6)	Knock Out (KO) Pot 7)	Pressure regulator 8)	Water Displacement Apparatus 9)	Auto cooling system 10)	Local control panel 11)	Data logger and controller 1)	Reactor: Reactor is a vessel made of SS-316 metallurgy with the following design specifications a)	Volume = 1 lt. b)	Design Pressure = 100 bar c)	Design Temperature = 500ºc It has a flush bottom valve at the bottom for collecting the product at the end of the experiment. Reactor is provided with a lid which has provision for the following a)	Stirrer blades which can be connected to external motor b)	Pressure gauge c)	Pressure sensor d)	Rupture pressure disc e)	Thermo-well for inserting temperature sensor f)	Gas injecting header g)	Reactor vent assembled to condenser inlet line h)	Reactor auto-cooling coil with inlet and outlet nozzles

2)	Reactor auxiliary cooling system This has been provided for circulating the cooling water to jacket coolers provided for the auxiliary systems viz. pressure gauge, pressure sensor, Magnetic driven stirrer, gas injecting header and reactor vent take-off. 3)	Heating section Heating section consists of a furnace chamber in which the reactor assembly can be fixed. The design temperature of the furnace is 500oC. Stirrer with external motor The stirrer in the reactor is driven by the external motor which is controlled from LCP or through SCADA software. The frequency of the stirrer is between 100-1450 RPM. 4)	Condenser Condenser is aligned in an inclined position for cooling the reactor outlet gases and condensed liquid will be refluxed back into the reactor. Uncondensed gases will be passed out of the condenser towards the knock out pot. 5)	Knock Out (KO)Pot 250 ml KO pot is connected to the outlet of the condenser. Liquid traces in the uncondensed gases are collected in the KO pot without allowing liquid carry over into the pressure regulator. 6)	Pressure regulator The KO pot outlet gases pass through 7 micron filter before it enters into pressure regulator. A 7 micron filter is provided on KO pot outlet to prevent solid particles going towards the pressure regulator. 7)	Water Displacement Apparatus The outlet of pressure regulator is provided with quick release coupling which is connected to inlet of water displacement apparatus. The water displacement apparatus is a 2L vessel with a threaded lid which is useful for measuring the amount of gases exiting from the pressure regulator. 8)	Auto cooling system Auto cooling system consists of water sump and a pump which can be operated either manually or automatically. Pump supplies water to cool the reactor and returns the hot water to the sump. 9)	Local control panel Local control panel is provided with the following a)	In the front end it consists of Main switch, temperature control, pressure control, alarm acknowledge, RPM control knob, heater switch, auto-cooling control switch and RPM control switch. b)	At the back end it consists of three power sockets for furnace, stirrer motor, auto-cooling pump, data logger port, pressure sensor port and temperature sensor port 10)	Data logger and controller Data logger is a AMAR DAS 3.0 software which logs the reactor temperature, pressure and stirrer RPM. The software is capable of controlling the batch reactor at required set temperature and RPM (as per experimental protocol). This has the facility to show the graphical trends of operating parameters as per the user requirement. Standard Operating Procedure: 1.	The experimental protocol has to be filled in the log book with these details: a)	Date of experimentation b)	Experiment number c)	Feed sample details d)	Set temperature, pressure and RPM e)	Residence time f)	Weight of the empty reactor + stand g)	Weight of the feed sample taken in reactor h)	Weight of the container for WDA water i)	Weight of the catalyst added as per protocol j)	Run Start Time at desired temperature k)	Run End time at desired temperature l)	Weight of empty sample can m)	Weight of the sample can with the product n)	Weight of reactor +stand+ product traces o)	Total weight of product p)	% recovery of product q)	pH of the sour water and tap water as per protocol r)	Signature of the experimenter 2.	Clean the reactor with kerosene and rinse with an aromatic liquid eg. Toluene by wearing necessary PPE (Chemical resistant gloves). 3.	Weigh the reactor along with the stand(Wt. of Reactor + stand=A) 4.	 Heat the feed sample above its pour point i.e. 100°C and ensure that it should not exceed 150°C to avoid cracking of the feed. 5.	Take approximately 500gm of feed sample in the reactor and fix it in the furnace chamber (Wt. of Reactor + Stand + Feed=B) 6.	Add catalyst/additive to the feed sample as per the protocol.(Wt. of catalyst=C) 7.	Fix the head of the reactor and tighten the clamps. 8.	Ensure water level in auto-cooling sump. Connect the auto cooling inlet and outlet quick release couplings for the reactor. 9.	Insert the temperature sensor in place and connect the pressure sensor. Connect the inlet of the condenser and tighten it properly. 10.	Connect the gas injection line to the reactor. 11.	Switch on the control panel to check the pressure inside the reactor through pressure sensor. 12.	Before injecting nitrogen gas into reactor, purge the injecting hose through vent provided and close the vent. 13.	Inject N2 into the system to check the setting of pressure regulator. Set the pressure regulator at required pressure as per the experimental protocol by corresponding opening or closing of the valve. Close the supply of N2 gas from the cylinder/ N2 header. 14.	Ensure the setting of pressure regulator by again passing the N2 into the system after stabilization. 15.	Release the pressure in the gas injecting line through vent and disconnect the N2 injection line. 16.	Release the pressure from knock out pot drain line to safe location. 17.	Fill the Weight Displacement Apparatus (WDA) with water to the brim. Close the lid of WDA. 18.	Connect the outlet of pressure regulator to WDA. 19.	Weigh the container used for WDA displaced water. 20.	The outlet of the WDA has to be kept in a dry container to collect the displaced sour water during experimentation. 21.	Take the control of the unit to SCADA software. Ensure the feedback data from the Local Control Panel (LCP) is appropriate. 22.	In the SCADA monitoring page Batch Number, Log rate and Batch Comments has to be entered by the user. 23.	Set the temperature and RPM to the required value as per the experimental protocol either from computer or in the local control panel. (Ensure the set temperature/ RPM in computer and local control panel is same)

24.	Click the Start Batch icon. 25.	Run the experiment till required residence time as per the experimental protocol is reached at desired temperature. 26.	Cool the system automatically/ manually by turning-on the water system either by setting the SV of temperature at very low temperature (eg. 60 ºc) or by switching the auto cooling system through manual switch. 27.	When the reactor temperature reaches below 100 ºc, click the Stop Batch icon. 28.	Store the Run data and Graphical report in a specified folder ‘VBU Batch Reactor- II Data’. 29.	Reduce the pressure of the system to 1.5-2 bar by depressurizing the system from KO pot drain line. 30.	Weigh the empty sample container(Wt. of empty container= D) 31. Collect the entire product from the reactor into a container using flush bottom valve. 32.	Weigh the product collected in container(Wt. of container + product=E). 33.	Remove the reactor for accounting the left over product traces in the reactor.(Wt. of reactor + stand + product traces= F) 34. Calculate the material balance by using the equation below {{(E-D) + (F-A)}/ (B-A)} x100 35.	Ensure the material balance is above 92%. 36.	50gm of the product has to be taken in a vial and handover to the lab for SIMDIST, Kinematic Viscosity, Product stability and Sulfur. 37.	Find pH of the sour water from the WDA and pH of tap water as per protocol. Note: 1.	Always handle the hot reactor with heat resistant gloves. 2.	Use necessary PPE during the experimentation as per the standard guidelines. 3.	For accessing the data a)	Click Analysis Report and select Batch Report. b)	Under Select equipment click VB batch reactor II. c)	For Select batch type VB # (respective number). -- EDIT BELOW THIS LINE -->