Parr Instrument 4580 User Manual

No. 398M

Parr Instrument Company

Operating Instruction Manual for

4580

HP/HT Pressure Reactors

Related Instructions.........................2

Customer Service............................2

Preface..................................................3

Scope...............................................3

Safety Information............................3

General Specifications.....................3

Explanation of Symbols...................4

Environmental Conditions................4

Provisions for Lifting and

Carrying ...........................................4

Cleaning & Maintenance..................4

Intended Usage ...............................5

User’s Responsibility .......................5

Unpack Carefully .............................5

Fixed Head or Removable

Head Design.........................................6

Flat Flexible Graphite Gasket..........6

Installation............................................7

Pressure and Temperature

Limits................................................7

Assemble the Reactor.........................8

Heaters .................................................10

Identify the Valves...............................11

Gas Inlet Valves...............................11

Gas Release Valve..........................11

Liquid Sampling Valve.....................11

Other Vessel Head Fittings.................12

Safety Rupture Disc.........................12

Type J Thermocouple......................12

Pressure Gage.................................12

Gage and Valve Adapters................12

How to Use the Vessel........................13

Fixed Head Vessels.........................13

Removable Head Vessels ...............13

Gas Connections.............................14

Pressurizing the Vessel...................14

Do Not Overfill the Vessel................14

Releasing Pressure .........................15

Withdrawing Liquid Samples ...........15

Initial Operating Test........................15

Accessories .........................................16

Pneumatic Lift..................................16

Internal Cooling Loop.......................17

Liners...............................................17

Spare Parts Kit.................................17

Air Motor ..........................................17

Variable Speed Electric Motor.........18

Explosion Proof Operation.................19

Periodic Pressure Tests .....................20

General Maintenance Notes...............21

Parts Lists............................................22

Reaction Vessel Parts List...............22

4580 Head Assembly Front View....24

4580 Head Assembly Rotated View 25

Overarm Parts List...........................26

Related Instructions

The following Parr publications are also available to further your understanding of this instrument and its component parts:

No. Description

230M Safety Precautions to be observed

when operating Pressure Reaction Equipment

231M Operating Instructions for Parr Safety

Rupture Discs

285M Sealing Instructions for Flexible

Graphite Gaskets

548M Operating Instructions for Series 4848

Reactor Controllers

234M Operating and Maintenance

Instructions for Parr Magnetic Drives

323M Operating Instructions for Parr

Pressure Relief Valves 201M Limited Warranty F0042 Health & Safety Assurance Certification

Customer Service

Questions concerning the installation or operation of this instrument can be answered by the Parr Customer Service Department: Phone: 309-762-7716 800-872-7720 Fax: 309-762-9453 www.parrinst.com parr@parrinst.com

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PREFACE

Scope

These instructions describe the installation, operation and maintenance of Parr Series 4580 HP/HT Pressure Reactors offered in two sizes, 1.0 and 1.5 gallon. 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 which are common to most Parr pressure reaction equipment, and includes safety precautions and other related information applicable to all research 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.

Safety Information

To avoid electrical shock, always:

1. Use a properly grounded electrical outlet of

correct voltage and current handling

capability.

2. Ensure that the equipment is connected to

electrical service according to local

national electrical codes. Failure to

properly connect may create a fire or

shock hazard.

3. For continued protection against possible

hazard, replace fuses with same type and

rating of fuse.

4. Disconnect from the power supply before

maintenance or servicing.

To avoid personal injury:

1. Do not use in the presence of flammable

or combustible materials; fire or explosion

may result. This device contains

components which may ignite such

material.

2. Refer servicing to qualified personnel.

General Specifications

Electrical Ratings

Controller ratings are found in the Operating Instructions 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.

Thermocouple: Unless otherwise specified, all Parr Controllers operate with a Type J (iron-constantan) 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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PREFACE (Continued)

Explanation of Symbols

On position, full power heater switch On position, half power heater switch 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 apparatus is to be used indoors.

Operating: 15 °C to 35 °C; maximum relative humidity of 80% non-condensing. Installation Category II (overvoltage) 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 humidity.

Provisions for Lifting and Carrying

The Series 4580 HP/HT Pressure Reactor and its components are very heavy. Before moving ensure all cables are disconnected. Use proper and safe lifting techniques when installing or moving the 4580 and/or its components.

Caution

Do not use in hazardous atmospheres.

Cleaning & Maintenance

Periodic cleaning may be performed on the exterior surfaces of the instrument with a lightly dampened cloth containing mild soap solution. All power should be disconnected when cleaning the instrument.

There are no user serviceable parts inside the product other than what is specifically 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 be replaced or serviced.

Caution

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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PREFACE (Continued)

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.

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 final

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 under-designed 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 and other elements carefully selected for

limits, using gaskets, closures

safe operation within the limits specified 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.

3. Establish training procedures to ensure

4. Maintain the equipment in good condition

Unpack Carefully

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.

All standard Parr pressure vessels are provided with either a 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.

that any person handling the equipment knows how to use it properly.

and establish procedures for periodic testing to be sure the vessel remains structurally sound.

Unpack the equipment carefully and check

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FIXED HEAD OR REMOVABLE HEAD DESIGN

Parr Series 4580 High Pressure/High Temperature Reactors are furnished with t wo structural options in addition to the size, pressure range, stirrer motor, controller and similar options. These are:

Fixed Head with Flat Gasket

There is no difference in the pressure or temperature limits or basic operating instructions based upon the fixed head or movable vessel options. There are differences in the design of the stand components which adapt the vessels to the support system.

In the fixed head design, the head of the vessel may remain fixed 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 head vessel design, all connections to the head are removed to allow the vessel to be opened.

Flat Flexible Graphite Gasket

The flat 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 sixteen compression bolts which must be tightened to develop the loading on the gasket.

An alternate PTFE gasket may be used for operating temperatures up to 350 C. Metal gaskets can be furnished for special applications. The metal gaskets are not interchangeable with the flat gasket design, but require special grooves machined into the head and cylinder.

Parr recommends the flexible graphite gaskets for most applications.

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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 which are not recommended by the Parr Instrument Company. It must also be understood that lower pressure and temperature limits may be required for modified reactors and for vessels made of special alloys.

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 fittings attached to the vessel. Obviously, the safe operating pressure of any system can be no higher than that of its lowest rated component.

All Parr reactors show the maximum safe operating pressure and temperature imprinted on the cylinder.

The working pressure and temperature in these 1.0 and 1.5 gallon reactors must not exceed the following maximum limits:

Pressure and Temperature Limits Bomb Material

T316SS 3000 psig T316SS 3000 psig T316SS 3000 psig

Maximum Pressure

Maximum Temperature

500 C Flexible Graphite Gasket

350 C PTFE Gasket

500 C Metal Gasket

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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. This unit needs to be placed at least 10 inches away from walls or flammable materials.

1. Set the stand in the workspace.

2A. Removable Vessels.

First pivot the overarm assembly to the back of the support stand.

The pressure vessel has been shipped as a complete assembly; it may be easiest on the initial setup to place the entire pressure vessel assembly into the heater. Note: The complete assembly does not need to be removed from the heater during opening and closing operations. It is designed so that the cylinder can remain in the heater while the head and split rings are attached or removed.

Once the vessel assembly is in place rotate the magnetic stirrer by hand to make sure that it turns freely. Then move the overarm back into position above the vessel. The knob on the top of the overarm will raise the upper shaft with coupling for attachment to the adapter on the top of the magnetic stirrer. Push down and rotate the upper shaft to bring these components into alignment.

Occasionally the motor housing and overarm assembly may vibrate out of the standard position. If the upper shaft is not in alignment with the center of the top of the magnetic stirrer it will be necessary to loosen the bolt which attaches the motor housing to the support stand. Remove the motor housing panel; there is a single bolt that runs through the lower housing support and the top shelf of the floor stand. Once the bolt is

loosened, rotate the housing the required amount, connect the upper shaft to the magnetic stirrer and then tighten the motor housing bolt.

2B. Fixed Head Reactor.

Bolt the stand to the floor using the holes in the base plate.

Loosen the panel screw of the vessel

retainer mounted on the midplate of the support stand and open the retainer bracket.

The pressure vessel has been shipped as a complete assembly. It is necessary to loosen the split ring bolts and remove the split ring. Lift the head assembly out of the cylinder and slide it into the midplate of the stand. Close the retainer bracket. The cylinder should be placed in the cylinder lift bracket.

Rotate the magnetic stirrer by hand to make sure that it turns freely.

Connect an air line to the 1/4” quick disconnect fitting at the base of the support stand. This pneumatic lift package will raise or lower the cylinder. It may also be used for the heater. The lever on the side panel of the support frame controls the lift motion.

The pneumatic package includes a pressure regulator with gage located inside of the support stand housing. It can be accessed by removing the back panel of the support stand. The regulator has been preset to 50 psi. The regulator can be adjusted by lifting up on the cap. Rotate clockwise to increase pressure, counter-clockwise to decrease the amount of pressure sent to the pneumatic lift cylinder. Press the cap back down after setting the pressure.

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