Parr Instrument 4560 User Manual
4560
Mini Bench Top Reactors
Operating Instruction Manual
396M
Mini Bench Top Reactors
Table of Contents
Preface
Scope — 3
Related Instructions — 3
Safety Information — 3
General Specifi cations — 3
Electrical Ratings— 3
Explanation of Symbols — 4
Environmental Conditions — 4
Provisions for Lifting and Carrying — 4
Intended Usage — 4
Cleaning & Maintenance — 4
User’s Responsibility — 5
Unpack Carefully — 5
Fixed Head or Removable Head Vessel Design — 6
Flat PTFE Gasket or Self Sealing O-ring Closure — 6
Installation
Pressure and Temperature Limits — 7
Assemble the Reactor — 8
Identify the Valves
Gas Inlet Valve — 9
Gas Release Valve — 9
Liquid Sampling Valve — 9
Other Vessel Head Fittings
Safety Rupture Disc — 10
Type J Thermocouple — 10
Pressure Gage — 10
Heaters — 10
How to Use the Vessel
Removable Vessels — 11
Fixed Head Vessels — 11
Air Motor — 13
Explosion Proof Operation — 14
Periodic Pressure Tests — 15
Accessories
Liners — 15
Spare Parts Kit — 15
General Maintenance Notes — 16
4560 Series Reaction Vessel Parts List
Standard Vessel Fittings — 17
High Temperature Vessel Fittings — 22
Overarm Parts List — 25
Figures
Fixed Head with O-ring — 6
Moveable Head with Flat Gasket — 6
Removable Head Vessel (Standard Temperature) — 19
Air Motor Option — 13
Vessel Closure and Standard Internal Parts — 17
4561 Gas Entrainment Assembly — 20
4563 Gas Entrainment Assembly — 20
Mini Head External Fittings & Parts List — 21
Vessel Closure and Standard Internal Parts — 22
Overarm Diagram — 25
Bomb Support Stand with Fixed Head and 1/8 hp
Stirrer Drive Motor — 26
Bomb Support Stand with Moveable Vessel and 1/4
hp Stirrer Drive Motor — 27
Customer Service
Questions concerning the installation or operation of this instrument
can be answered by the Parr Customer Service Department:
1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453
E-mail: parr@parrinst.com • http://www.parrinst.com
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Parr Instrument Company
Mini Bench Top Reactors
Preface
Scope
These instructions describe the installation, operation and maintenance of Parr Series 4560 Mini
Bench Top Reactors offered in sizes from 100 mL to
600 mL. They cover the basic steps to be followed
for installing these reactors and describe the function of all standard components. They cover the
basic steps to be followed when installing these
reactors and describe the function of all standard
components. They are intended to be used in conjunction with several related instruction sheets listed
on the previous page. This information describes
several components that are common to most Parr
pressure reaction equipment, and includes safety
precautions and other related information applicable
to all reaction laboratories. The users should study
all of these instructions carefully before starting to
use these vessels so that they will fully understand
the capabilities and limitations of the equipment.
Related Instructions
The following Parr publications are also included to
further your understanding of this instrument and
its component parts:
No. Description
201M Limited Warranty
230M Safety Precautions to be observed when
operating Pressure Reaction Equipment
231M Operating Instructions for Parr Safety
Rupture Discs
234M Operating and Maintenance Instructions
for Parr Magnetic Drives
323M Operating Instructions for Parr Pressure
Relief Valves
548M Operating Instructions for 4848 Reactor
Controllers
F0042 Health & Safety Assurance Certifi cation
Safety Information
To avoid electrical shock, always:
Use a properly grounded electrical outlet of correct
voltage and current handling capacity.
Disconnect from power supply before servicing. The
power supply cord of the equipment is the main
disconnect device.
To avoid personal injury:
Do not use in the presence of fl ammable or combustible materials; fi re or explosion may result. This
device contains components which may ignite such
materials. Refer servicing to qualifi ed personnel.
General Specifi cations
Electrical Ratings
Controller ratings are found in the Operating Instruc-
tions for the controller supplied with your reactor.
Before connecting a controller to an electrical outlet,
the user must be certain that the electrical outlet has
an earth ground connection and that the line, load
and other characteristics of the installation do not
exceed the following limits:
Voltage: Fluctuations in the line voltage should not
exceed 10% of the rated nominal voltage shown on
the data plate.
Frequency: Controllers can be operated from either
a 50 or 60 Hertz power supply without affecting their
operation or calibration.
Current: The total current drawn should not exceed
the rating shown on the data plate on the controller
by more than 10 percent.
Inductive Loads: Inductive loads must be limited to
750 watts (1 hp) at 115 volts, or to 1100 watts (1-1/2
hp) at 230 volts. Do not connect these controllers
to the primary (input) side of an auto-transformer
(Variac, Powerstat or the like). The heavy inductive
load on the primary side of such transformers will
destroy the relay. The secondary (output) side of an
auto-transformer can be carried through the relay if
this circuit is isolated from the controller. A separate, full-voltage connection must then be made to
operate the temperature controller and to actuate
the relay.
Thermocouple: Unless otherwise specifi ed, all
Series 4848 Controllers operate with a Type J (ironconstantan) thermocouple. The total resistance of
the thermocouple and the lead wires should not exceed 20 ohms. If the resistance of the thermocouple
circuit is higher, it will reduce the sensitivity of the
control system.
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Mini Bench Top Reactors
Explanation of Symbols
II On position, full power heater switch
I On position, half power heater switch
O Off Position
~ Alternating Current (AC)
This CAUTION symbol may be present on the Product Instrumentation
and literature. If present on the product, the user must consult the appropriate part of the accompanying product literature for more information.
This CAUTION symbol indicates that the surface may be hot.
Protective Earth (PE) terminal. Provided for connection of the Protective Earth (green or green/yellow) supply system conductor.
Environmental Conditions
This instrument is intended to be used indoors.
Caution!
Do not use in hazardous atmospheres.
Operating: 15 ºC to 40 ºC; maximum relative humid-
ity of 80% non-condensing. Installation Category II
(over voltage) in accordance with IEC 664.
Pollution degree 2 in accordance with IEC 664.
Altitude Limit: 2,000 meters.
Storage: -25 °C and 65 °C; 10% to 85% relative hu-
midity.
Provisions for Lifting and Carrying
Before moving ensure all cables are disconnected.
Use proper and safe lifting techniques when install-
ing or moving the 4560 Reactor and/or its compo-
nents.
Intended Usage
This system has been designed for use as a high
pressure reactor system. It has been designed, built,
and tested to strict physical and electrical standards.
However, it is the user’s responsibility to install and
operate it in conformance with local pressure and
electrical codes.
If this equipment is used in a manner beyond its intended usage, the protection provided by the equipment may be impaired.
Cleaning & Maintenance
Periodic cleaning may be performed on the exterior
surfaces of the controller with a lightly dampened
cloth containing mild soap solution. All power
should be disconnected and the power cord should
be unplugged when cleaning the instrument.
There are no user serviceable parts inside the product other than what is specifi cally called out and
discussed in this manual. Advanced troubleshooting
instructions beyond the scope of this manual can
be obtained by calling Parr Instrument Company
in order to determine which part(s) may need to be
replaced or serviced.
Ensure that any hot surfaces have had
adequate time to cool before cleaning
or maintaining the reactor and/or its
components.
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Parr Instrument Company
Mini Bench Top Reactors
User’s Responsibility
All Parr reactors and pressure vessels are designed
and manufactured with great care to assure safe
operation when used within their prescribed temperature and pressure limits.
But . . . the basic responsibility for safety when using this equipment rests entirely with the user; who
must:
1. Select a reactor or pressure vessel that has the
capability, pressure rating, corrosion resistance
and design features that are suitable for its
intended use. Parr engineers will be glad to discuss available equipment and material options
with prospective users, but the fi nal responsibility for selecting a reactor or pressure vessel
that will perform to the user’s satisfaction in any
particular reaction or test must rest with the user
– not with Parr.
In exercising the responsibility for the selection
of pressure equipment, the prospective user is
often faced with a choice between over-or underdesigned equipment. The hazards introduced
by under-designed pressure vessels are readily
apparent, but the penalties that must be paid for
over-designed apparatus are often overlooked.
Recognizing these criteria, Parr reactors and
pressure vessels are offered in several different
styles, each designed for convenient use in daily
operation within certain temperature and pressure limits, using gaskets, closures and other
elements carefully selected for safe operation
within the limits specifi ed for that design. But in
order to preserve the validity of these designs,
all temperature and pressure limits must be
observed, and no attempt should be made to
increase these limits by making alterations or by
substituting components which are not recommended by Parr Instrument Company.
2. Install and operate the equipment within a
suitable barricade, if required, with appropriate
safety accessories and in full compliance with
local safety codes and rules.
All standard Parr pressure vessels are provided
with either suitable relief device or a means to
attach one (typically in the form of a plugged
opening). When a pressure vessel is delivered
without a pressure venting device, it is the customer’s responsibility to provide pressure relief
in order to protect the operator and the equipment from destructive high pressures. If you
need more information or need help in selecting
a proper relief device, please contact Parr Instrument Company.
3. Establish training procedures to ensure that any
person handling the equipment knows how to
use it properly.
4. Maintain the equipment in good condition and
establish procedures for periodic testing to be
sure the vessel remains structurally sound.
Unpack Carefully
Unpack the equipment carefully and check all the
parts against the, packing list. If shipping damage
is discovered, report it immediately to the delivering carriers. The vessel, motor, heater, and temperature controller may be packed separately for
convenience in shipping, but these parts are easily
reassembled. Examine the components closely for
any loose parts or shipping damage and be sure to
check all layers of packing materials thoroughly so
as not to overlook any parts which might otherwise
be discarded.
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5
Mini Bench Top Reactors
Parr Series 4560 Mini Reactors are furnished with two structural options in addition to the size, pressure
range, stirrer motor, controller and similar options. These are:
Fixed Head or Removable Head
Vessel Design
In the fi xed head design, the head of the vessel
may remain fi xed in the reactor support stand. All
attachments to the head, gas and liquid feed and
discharge lines, cooling water, vapor take-off and
condenser, thermocouple, and any electrical leads
can remain permanently in place. The reactor is
opened by removing the cover clamp sections and
lowering the cylinder away from the head.
In the removable vessel design, the entire vessel
must be removed from the support stand for charging, product recovery, and cleaning.
There is no difference in the pressure or temperature limits or basic operating instructions based
upon the fi xed head or movable vessel options.
There are differences in the design of the stand
components which adapt the vessels to the support
system.
Flat PTFE Gasket or Self Sealing
O-ring Closure
The fl at gasket is held in a recess in the vessel head
and a machine pilot on the cylinder closes the recess to completely contain the gasket. The split ring
closure used with this gasket has six cap screws
which must be tightened to develop the loading on
the gasket.
The self sealing design features an O-ring retained
in a groove on the vessel head. This design is self
sealing and the split ring used with this sealing system does not require nor have the cap screws used
with the fl at gasket.
Maximum temperatures of a given system are dependant upon the material of construction and type
of seal. Other accessories may limit operating temperature. The fl at PTFE gasket can be used to operat-
ing temperatures as high as 350 °C. The fl at fl exible
graphite gasket can be used to operating temperatures as high as 500 °C. The maximum temperature
of the vessels equipped with O-ring seals depends
upon the material used for the O-ring. The most
common material is a fl uoroelastomer (FKM) which
has a 225 °C maximum operating temperature limit.
Fixed Head with O-ring
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Parr Instrument Company
Moveable Head with Flat Gasket
Mini Bench Top Reactors
Installation
Pressure and Temperature Limits
The working pressure and temperature at which any
reactor or pressure vessel can be used will depend
upon the design of the vessel and the materials
used in its construction. Since all materials lose
strength at elevated temperatures, any pressure
rating must be stated in terms of the temperature at
which it applies. The standard material of construction for Parr Instrument Company is Type 316 Stainless Steel.
Limits for vessels made of other materials and for
other operating temperatures can be obtained from
Parr Customer Service. No attempt should be made
to increase these limits by making alterations or by
substituting components that are not recommended
by the Parr Instrument Company. It must also be
understood that lower pressure and temperature
limits may be required for modifi ed reactors and for
vessels made of special alloys.
Limits for vessels will be determined by the physical characteristics of the vessel material and will be
prescribed on an individual basis.
The maximum working pressure and temperature
for any vessel is governed by the design of the
vessel and the strength of the material from which
it is constructed. There is also a close relationship
between working pressure and temperature since
the strength of any material will normally fall off
as the temperature is increased. Temperature and
pressure limits are also affected by the physical
properties and temperature limits of the gaskets and
seals used in the vessel, and by any valves, gages or
other fi ttings attached to the vessel. The safe operating pressure of any system can be no higher than
that of its lowest rated component.
Working temperatures up to 225 °C are permissible
in Mini Reactors equipped with fl uoroelastomer
(FKM) O-ring seals. The higher the operating temperature above 200 °C, the shorter the life of the Oring will be. Perfl uoroelastomer (FFKM) O-ring seals
have a broad chemical resistance and can be used
to temperatures up to 300 °C. Unfortunately they
are very expensive and will generally be reserved
for unique applications. Ethylene-propylene (EP)
O-rings can be used to 170 °C and are recommend-
ed for applications such as ethers, ammonia and
amines which will rapidly destroy fl uoroelastomer
O-rings.
Pressure Vessel and Temperature Limits
In the standard pressure and temperature setup, the
system must not exceed the following:
Vessel
Material
T316SS 3000 psig (200 bar)
T316SS 3000 psig (200 bar)
T316SS 3000 psig (200 bar)
Maximum
Pressure
Maximum
Temperature
350 °C PTFE
Flat Gasket
225 °C FKM
O-Ring
300 °C FFKM
O-Ring
In the high pressure/high temperature setup, the
system must not exceed the following:
Vessel
Material
T316SS (HT) 2000 psig (138 bar) 500 °C Flexible
Maximum
Pressure
Maximum
Temperature
Graphite Flat
Gasket
All Parr reactors show the maximum safe operating
pressure and temperature imprinted on the cylinder.
An accompanied restricted operating limit tag and/
or supplemental manual is given when a component of the system limits the operation below the
imprinted valves.
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Mini Bench Top Reactors
Assemble the Reactor
These reactors require at least 10 sq. ft. of workspace in a well-ventilated area with convenient
access to an electric outlet, running water, air and a
drain.
1. Set the stand in the workspace.
Bolt the stand to the bench top using the
holes in the base plate.
2. The support and heater are shipped fully assembled. The heater raises and lowers on its
support rod to permit the vessel or cylinder to
be removed. Lower the heater, open the hinged
retainer on the front of the support and slide the
vessel into its support. Fixed head vessels have
a square lip which fi ts into a matching groove in
the support plate. Removable vessels are supported by the split rings which rest on the support plate adapter. The stirrer drive connector
lifts by rotating and lifting the knob above the
belt guard. The universal joint contains a cross
pin that slips into the groove on top of the magnetic drive. There is a bracket at the back of the
area where the split ring rests. The thumb screw
on the drop band which encircles the split ring
closure should fi t into the slot on this bracket.
This will keep the vessel from rotating when
stirring viscous reactions. It may be necessary
to reposition the drop band if the gage does not
face forward when the thumb screw is in the
slot.
3. Set the Temperature Controller near the reactor,
leaving a space of at least six inches between
the controller and the base of the reactor so
that the controller will not be unduly affected by
radiant heat. Connect the reactor to the controller using information contained in its Instruction
Manual 548M or follow the steps below.
Parr Heating Only:
The Parr Heating output connector is to be used
only with Parr Instrument Company heater assemblies supplied with the appropriate heater
power cord.
Note: Do not make connections to a Variac,
Powerstat or the like to attempt to control the
heating output. The heavy inductive load on
the primary side of such devices can destroy
the internal sold state relay located in the 4848
controller.
Motor:
Secure the clamp on motor cord to the
controller with the provided screw next
to the motor socket for safety purposes.
The Motor output connector is to be used only with
Parr Instrument Company motor assemblies supplied with the appropriate motor power cord.
4. Connect the heater cord from the heater into
the heater socket on the rear panel of the Series
4848 Reactor Controller.
5. Plug the motor cord into the motor socket on the
rear of the controller.
Secure the clamp on the motor cord with
the provided screw next to the motor
socket for safety purposes.
6. Connect the thermocouple and extension wire
to both the thermocouple and to the controller
in the “Primary Temp Input” position on the rear
panel. Insert the thermocouple in the thermowell.
Labeled connections are provided on the rear
panel of the controller.
Parr Cooling Only:
The Parr Cooling output connector is to be used
only with Parr Instrument Company cooling solenoid valve assemblies supplied with the appropriate cooling power cord.
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Parr Instrument Company
7. Connect leads from accessory packages such as
tachometer, pressure transducer and high temp
cut-off to the designated positions on the back
panel of the 4848 Controller.
8. Connect cooling water to the magnetic drive.
See Instruction Manual No. 234M.
9. Connect tubing to the rupture disc outlet and run
to a safely vented area. See Instruction Manual
231M.
Mini Bench Top Reactors
10. Note the voltage and amperage requirement
stamped on the controller data plate, and then
plug the power cord into an appropriate outlet.
Power for these reactors should be drawn from
a grounded outlet capable of carrying up to the
full current rating of the reactor.
11. If an electric stirrer motor is supplied, turn the
speed control knob fully counterclockwise on
the Reactor Controller, turn on the motor switch
and slightly increase the speed for a short run
to check the stirrer drive system but do not turn
on the heater, put heater toggle switch in center
position (OFF). There must always be a vessel in
the heater when it is turned on, and the vessel
and heater sizes must match. If the heater is operated without proper size vessel in contact with
the heater, the heater may overheat and fail.
Identify the Valves
Gas Inlet Valve
The gas inlet valve is easily identifi ed when the
vessel is open by noting that it is connected to a dip
tube which extends to a point near the bottom of
the cylinder. With this arrangement, incoming gas is
always introduced below the surface of the liquid.
This valve includes a coupling with an “A” socket
connection for attachment of the pressure hose.
Gas Release Valve
The gas release valve is typically connected to a side
opening on the gage adapter. Gas released from
this valve will be drawn from the top of the reactor.
Liquid Sampling Valve
The liquid sampling valve is attached to the same
fi tting as the gas inlet valve and connected to the
same dip tube. This provides the operator with a
means for clearing the dip tube to be sure that any
sample taken during a run will be representative of
the charge. This can be done by opening the upper
gas inlet valve momentarily to allow the inlet gas to
force any liquid in the dip tube back into the reactor before withdrawing a sample from the sampling
valve.
Safety Rupture Disc
Gas Inlet Valve
Liquid Sampling Valve
Dip Tube
Stirring Shaft
Lower Guide
Bearing
Pressure Gage
Magnetic Drive
Thermocouple
Gas Release Valve
Vessel Water Cooling
Channel
Cooling Loop
Thermocouple / Thermowell
Adjustable
Impeller(s)
Removable Head Shown (Standard Temperature, T316)
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