Rubber Lining Application Manual Section 11: Curing

Revision Date: September 1, 2009 Page: 11 - 1

CURING
The five basic methods used for curing tank lining are autoclave, internal (pressure) steam, exhaust or atmospheric steam, chemical cure, and hot water cure. The specific method used will depend on the nature and size of the vessel to be lined. Note that recommendations contained in this manual are suggested guidelines only. Actual cure times will be dependant on factors such as rubber thickness, vessel size and wall thickness, heat loss, ambient conditions and elevation. Your Polycorp representative should be consulted concerning major changes in cure. All cures should have proper temperature recording charts and these should be properly identified with job number and date. If there are any questions regarding conformance of cure to published time and temperature recommendations, please contact your Polycorp representative.

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1. AUTOCLAVE CURE This refers to vulcanization where the rubber-lined vessel is placed inside a pressure vessel and subjected to controlled steam under pressure. An autoclave cure provides the best and most uniform cure and should be used whenever possible. Metal parts should be placed in the autoclave so that the best possible drainage of condensate from the rubber will be obtained. To obtain the most accurate and uniform cure, it is desirable to have the autoclave fully equipped with thermocouples and instrument controls on air pressure and steam. The incidence of improper cure is more likely to occur when using a manually operated method. Sufficient boiler capacity should be available to raise the temperature from ambient to cure in a relatively short period of time. At termination of cure, it is recommended the rubber-lined vessel be cooled down by using water and/or air. Proper cool down of autoclaves will prevent post curing and preclude the possibility of cracking hard rubbers. The following cool-down procedures are suggested as recommended methods: a) Cool down soft natural and synthetic rubbers one hour with air and water. b) Cool down Triflex and hard rubber with air and water until autoclave temperature reaches 200F. Continue a gradual cooling down of the autoclave with air and then with air and water. This cool down procedure can be modified, but a step-wise procedure will prevent cracking of the hard rubber. During cool down it is important to maintain an air and water pressure equal to or greater than the steam pressure. All autoclaves should be equipped with temperature and pressure recorders. The recording charts should be properly identified and dated. An autoclave is shown in sketch 1401 with details of operation on following pages. Precautions must be taken against stratification of steam and air particularly in large vulcanizers. During start-up the bottom exit valve must be cracked open to allow a complete sweep of steam and cold air through the autoclave to avoid a cold bottom and subsequent undercured rubber.

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Sketch 1401 TYPICAL AUTOCLAVE POLYCORP PROTECTIVE LININGS

AUTOCLAVE OPERATION (BASED ON THE POLYCORP DESIGN ABOVE) 1. 2. 3. 4. 5. 6. 7. 8. 9. Close drain valve. Close blow off line. Close air line valve. Close cooling water valve. Open trap line valve. Set temperature desired on automatic control. Open vent line valve. Open steam valve. Automatic control valve on vent should close when autoclave reaches desired temperature. 10. Proceed with specified cure. 11. At end of cure, open-air line valve, close steam valve, open cooling water valve and close vent line valve.

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12. Maintain an air and water pressure equal to or greater than the curing pressure. The cooling water pressure must exceed the holding air pressure used for cooling. This is necessary so water will enter the autoclave. 13. Cool down soft rubber one hour with air and water. 14. Cool down Triflex and hard rubber lined tanks with air and water until autoclave temperature reaches 200F; then with air for one hour; then with air and water for one hour. This gradual cool down procedure precludes the possibility of cracking the hard rubber lining. 15. Turn off air. 16. Turn off water. 17. Open blow off valve. 18. Open drain valve. 19. When pressure is reduced to zero, open autoclave.

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2. INTERNAL OR PRESSURE STEAM CURE Internal steam pressure cures are used on vessels that are designed for pressure and are too large to be placed in an autoclave. The vessel should be positioned during cure so that complete condensate drainage is obtained. To accomplish this, tanks with a sump should be cured with a well pipe connected to a trap (see sketch 1402). Tanks without a sump can be cured with a steam trap and temperature recorder connected to a bottom outlet (see sketch 1403). All nipples should be bled with a 1/4 petcock. Bottom outlets should be left open long enough to be sure that all air is evacuated before building up pressure. Sufficient boiler capacity should be available to raise the temperature from ambient to curing in a relatively short period of time. Long uninsulated pipe runs from the steam source should be avoided. Low pressure steam plus uninsulated lines promote excessive condensate. A thermometer and pressure gauge should be placed in a blind flange near the bottom of the tank and when the thermometer registers the temperature corresponding to the gauge pressure, the air has been fully evacuated. Prior to introducing steam into the vessel all outlets should be blanked off. Flanges should be lined with one of the special constructions shown in sketches 1404, 1405, or 1406. This flange procedure will allow the vessel to be bolted up under pressure without undue distortion of rubber on face of flange. Contact your Polycorp representative for further information. Cool down internal steam cures by introducing air until cold. Some natural rubber compounds tend to develop tacky surfaces when air is introduced too quickly into the vessel. If this occurs, the curing pressure should be allowed to drop 5 to 10 psi before air is introduced. The air pressure must be maintained at five pounds higher than the curing pressure. All cures should have proper temperature and pressure recording charts and these should be properly identified with job number and date. Outside temperature has a significant influence on the time required to cure a vessel. In cold winter temperatures, it is imperative that the vessel be insulated to effectively carry out the cure. A cold winter factor cannot be offset by internal steam temperature. Steel thickness is also a factor. Heavy thick steel needs additional time to compensate for the heat sink and warm-up period. This is where external temperature gauges are quite valuable in monitoring the time/temperature so one can judge and insure themselves that a positive cure is being obtained.

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Sketch 1402 Internal Steam Cure Tank with Sump

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Sketch 1403 Internal Steam Cure Tank with Bottom Outlet (No Sump)

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Sketch 1404 Internal Steam Cure Flange Detail for Outlets

(Recommended for Vacuum Equipment)

Sketch 1405 Internal Steam Cure Flange Detail for Outlets

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Sketch 1406 Internal Steam Cure Flange Detail for Outlets (NOT Recommended for Vacuum Equipment)

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3. EXHAUST OR ATMOSPHERIC STEAM CURE Exhaust or atmospheric steam is normally used for field vessels that have open tops and/or bottoms, vessels that do not withstand pressure or vessels that are too large to fit in an autoclave. In the case of open top tanks, the opening must be covered with fabric or combinations of fabric and plastic. The covering must be made tight so the steam will be contained. Steam should be introduced into tank by means of a steam line through an outlet or the opening in the top of tank. It is absolutely essential that provisions be made to drain all condensate from the vessel during cure. The bottom outlet on a closed top tank may be left open for drainage, but other outlets should be closed with blind flanges drawn up to within 1/32 of rubber on flange. During the first stages of cure, steam should be introduced for approximately 1 hour. This time may vary according to the size of tank or size of steam line. The time should be long enough to expand any trapped air so that it may be found and repaired, and short enough so that the surface of the stock will not be cured to the stage where a needle patch repair cannot be made. After this initial warm up period, the steam could be turned off and the lining inspected while hot. At this stage, any visible trapped air blisters can be punctured with a hypodermic needle to remove the air. After air has been removed, the needle puncture should be repaired with a needle patch of the uncured rubber. Needle patches should be firmly stitched down to close the needle hole in the underlying stock. On completion of the needle patch repair, the steam should be again turned on in sufficient force to bring the temperature higher than 200F. The volume of steam should be enough so that some live steam can be seen blowing out the bottom outlet. The steam should not impinge directly on the rubber lining. Tanks that have an enclosed top with bottom outlet should start timing the cure when hot steam at 200F minimum is coming out the bottom outlet and the temperature of the rubber surface has reached the desired cure temperature (as measured in the coldest spot in the vessel). The length of cure is counted from the time the temperature reaches the requirements until the end of cure when the steam is turned off. Thermometers through outlets and internally located thermocouples at various points in the tank should be used to monitor the temperature. When temperature varies at different spots in the vessel, the coldest spot should govern how much the overall cure should be increased. No cool down period is required for this type of cure. If steam at atmospheric pressure cannot be obtained, the cure will have to be adjusted.

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EXHAUST STEAM CURING PRECAUTIONS: Specifications and information on the technical data sheets is written based on consistent lab conditions. Frequently the cure times are extended for the lining to receive the optimum cure. The following are all considerations in determining the correct cure cycle. Warm up vessel at a rate of 10-15 degrees/hour. The time it takes to warm up the unit does not count toward the cure time. Curing is a function of time and temperature. Lower temperatures will lengthen the cure time. Tank insulation, temperature of the surrounding air, elevation and wind velocity over the tank can shorten or lengthen the cure. Thickness and surface area (structure) of the metal will act as a heat sink and increase the length of the cure. The metal structure must reach a constant temperature before the cure time is started. Cold spots can develop as a result of trapped air, condensate accumulation or ineffective steam circulation. Thermocouples must be strategically placed to monitor the coldest spots in the tank. Temperature readings must also be taken on the metal opposite the rubber lining to ensure the metal temperature is high enough to cause the rubber/cement interface to cure. The amount of steam must be properly estimated for curing. To ensure proper cure of flange faces, steam must escape around openings. If the steam is stagnant, cold spots form. Petcocks may be installed on extended piping and shall be used to insure steam flows through those areas and across the flange faces. The steam supply must not only be adequate but must be directed in such a way to ensure it is flowing over all rubber lining surfaces, especially the bottom. All condensation must be removed. Drains should be provided at the bottom of the vessel and elsewhere to ensure condensate will run off and not collect in any pockets. An open top tank or one sitting on a concrete pad can result in situations where the tank walls are cured but the floor is not. The steam must be directed towards the bottom of the tank and flow around all surfaces. The entire cure and cool down must be monitored, especially if it is possible to pull a vacuum and collapse the vessel. Vacuum breakers may be necessary depending on the construction of the vessel.

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TYPICAL EXHAUST STEAM PIPING SETUP

Note:

For large tanks or during cold weather, larger size piping to furnish more steam may be required (insulation may also be necessary) to maintain appropriate inside curing temperature that is in accordance with Polycorps recommendation.

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SAMPLE CURVES FOR ATMOSPHERIC CURING

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KEY CALCULATIONS FOR STEAM REQUIREMENTS FOR ATMOSPHERIC CURES a) Pounds of Steam per hour: Example - during 2-hour warm-up period and based on an enclosed vessel with 3/8 plate on bottom and 1/4" on sides and top; Pounds per hour of steam = 0.05V + 0.15A + 0.005W Where: V = Volume in cubic feet A = Area in square feet W = Weight of rubber and steel in pounds

b) Boiler Horsepower Required = Pounds of steam per hour 30 c) Steam Flow Table: Table shows steam flow in pounds per minute through 1,000 feet of pipe Steam Pressure Pipe Size 50# 75# 100#
1 2 2-1/2 3 3-1/2 4 4.27 25.8 40.7 71.5 89.0 144.0 6.32 36.7 57.7 101.0 146.5 204.0 8.15 52.5 74.5 130.0 185.0 263.0

To the use the table, determine steam requirement in pounds per minute for 1,000 feet of pipe. For example, if 2,0000 pound per hour are required (2000/60 = 33.3 lb./minute), a 2 pipe at 75 pounds of steam pressure is required. To adjust for varying lengths of pipe, multiply flow rate from the table by the appropriate factor below:
Length of Pipe (feet)
100 200 300 400 500 600 700 800 900

Factor
3.16 2.24 1.83 1.58 1.41 1.29 1.20 1.12 1.05

Example: If steam source is 100 away, a 2 pipe is used and gauge pressure is 50# then steam delivery/minute = 3.16 x 25.8 = 81.53 pounds.

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4. CHEMICAL CURING There are cases where using heat to cure the rubber is not possible. Steam may not be available, or the equipment to produce the steam is inadequate. Chemical curing rubber is an acceptable solution for these situations. It is typically used in field repair situations. Chemical activators are used to cure these specialized compounds. They are almost always used by coating the activator on the rubber lining sheet and then adding another coat on the lining after the first has dried. In some cases you may want to coat the rubber sheet prior to lay-up. Specific instructions are contained on the respective Technical Data Sheets in this manual. Activator should not be applied to the side of the rubber being applied to the substrate as this may interfere with bonding. The chemical activator will only result in a rapid cure of the lining surface. Full cure of these types of linings may take weeks. The time required is dependent upon the type of activator and temperature. Steam, heat lamps or other heat sources may be used to accelerate the curing process. Chemical cure linings may also be restricted to thinner gauges as the activator my not penetrate the full thickness of heavier gauge materials. Care must be taken to ensure no dynamic forces (chemical or physical) will be applied to the lining until it has cured throughout.

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5. HOT WATER CURING On field lined tanks, one way to obtain some pressure during cure is to use water for hydrostatic pressure. In preparation for water cure, the outlets and/or manways must be prepared using chemical cured or pre-cured rubber. Alternatively, the outlet may be exhaust cured so the manway covers and blind flange plates can be tightened to hold the water. Cured rubber gaskets are also required. The other area requiring preparation is to extend a stand pipe column (pipe) for ten feet above the vessel structure with a hose to exhaust air and/or steam vapors during the curing process. The tank structure must be designed so that it is able to withstand the hydrostatic pressure of the water and curing temperatures up to 210F. Also, the tanks need to have sufficient foundation to support the water filled vessel, either a sand base for non-installed, or the proper tank setting itself. On open top tanks, the preparation procedures are the same, except the tank is lined all the way to the top and the water is filled to the top. Prior to filling the tank with water, steam sparger piping should be installed near the bottom of the vessel. The steam itself shall be directed not to impinge on the rubber surface and it is recommended that the steam be introduced in an angled, downward direction. Steam should be introduced to the filling tank as soon as the lowest sprayer nozzles are immersed. Once the temperature has reached 180F, the cure can be considered as starting. It is best for the water temperature to be 180F 205F. No water source is acceptable that may contain oil. Thermocouples should be used to monitor the temperature within the vessel from top to bottom. Also, metal temperature probes may be utilized on the outside for temperature information if the tank is not insulated. After the cure is completed, it is recommended that the water be allowed to cool down to approximately 110F before draining the vessel. This reduces the likelihood of trapped air expansion blisters. If the water temperature is slow to come down, it is permissible to add cold water.

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PROPERTIES OF SATURATED STEAM AT SEA LEVEL

GAUGE PRESSURE (in psi) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 58 60 62 64 66 68 70 ABSOLUTE PRESSURE (psia) 14.7 15.7 16.7 17.7 18.7 19.7 20.7 21.7 22.7 23.7 24.7 25.7 26.7 27.7 28.7 29.7 30.7 31.7 32.7 33.7 34.7 36.7 38.7 40.7 42.7 44.7 46.7 48.7 50.7 52.7 54.7 56.7 58.7 60.7 62.7 64.7 66.7 68.7 70.7 72.7 74.7 76.7 78.7 80.7 82.7 84.7 TEMPERATURE F 212.0 215.4 218.5 221.5 224.5 227.4 230.0 232.4 234.8 237.1 239.4 241.6 243.7 245.8 247.9 249.8 251.7 253.6 255.4 257.2 258.8 262.3 265.3 268.3 271.4 274.0 276.7 279.4 281.9 284.4 286.7 289.0 291.3 293.5 295.6 297.7 299.7 310.7 303.6 305.5 307.4 309.2 310.9 312.7 314.3 316.0 SENSIBLE HEAT (Btu/lb) 180.2 183.6 168.8 189.8 192.7 195.5 198.1 200.6 203.1 205.5 207.9 210.1 212.3 214.4 216.4 218.4 220.3 222.2 224.0 225.8 227.5 230.9 234.2 237.3 240.2 243.0 245.9 248.5 251.1 253.7 256.1 258.5 260.8 263.0 265.2 267.4 269.4 271.5 273.5 275.3 277.1 279.0 280.9 282.8 284.5 286.2 LATENT HEAT (Btu/lb) 970.6 968.4 966.4 964.5 962.6 960.8 959.2 957.6 956.0 954.5 952.9 951.5 950.1 948.6 947.3 946.0 944.8 943.5 942.4 941.2 940.1 937.8 935.8 933.5 931.6 929.7 927.6 925.8 924.0 922.1 920.4 918.6 917.0 915.4 913.8 912.2 910.7 909.2 907.8 906.5 905.3 904.0 902.6 901.2 900.0 898.8 TOTAL HEAT (Btu/lb) 1150.8 1152.0 1153.2 1154.3 1155.3 1156.3 1157.3 1158.2 1159.1 1160.0 1160.8 1161.6 1162.3 1163.0 1163.7 1164.4 1165.1 1165.7 1166.4 1167.0 1167.6 1168.7 1170.0 1170.8 1171.8 1172.7 1173.5 1174.3 1175.1 1175.8 1176.5 1177.1 1177.8 1178.4 1179.0 1179.6 1180.1 1180.7 1181.3 1181.8 1182.4 1183.0 1183.5 1184.0 1184.5 1185.0 SPECIFIC VOLUME STEAM (cu ft/lb) 26.80 25.20 23.80 22.50 21.40 20.40 19.40 18.60 17.90 17.20 16.50 15.90 15.30 14.80 14.30 13.90 13.40 13.00 12.70 12.30 12.00 11.40 10.80 10.30 9.87 9.46 9.08 8.73 8.40 8.11 7.83 7.57 7.33 7.10 6.89 6.68 6.50 6.32 6.16 6.00 5.84 5.70 5.56 5.43 5.31 5.19