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Operating Manual Old Unit PVC Reactors Page .36 t III. OPERATING PROCEDURES (CONTINUED) C. Polymerization General Information The polymerization phase of the reactor batch cycle is the phase in which the liquid VCM is converted into solid PVC. This portion of the reactor cycle is mainly accomplished by instrumentation which is controls the-transfer of heat from the reaction. The lead operator is responsible for monitoring the reactor temperature and pressure and-taking corrective action as needed such as venting the reactor if the temperature deviates from the setpoint or if the pressure on the reactor starts rising due to inerts blanketing the condenser. The lead operator must also coordinate the activities of the "A" operator who must sample'the reactor if it needs to be sampled or kill the reaction when it has progressed to the point that product quality is satisfactory. Figure 8 (in the Appendix) shows the pressure, temperature, and cooling water curves for a normal polymerization. tL cLit i <4/ 1. Steam continues to be added to the reactor jacket to expedite heating of the reactor contents to run temperature. The lead operator will monitor the reactor temperature and pressure during heat-up and shut off the steam to the jacket when the temperature in--felte reactor is within 2-3 of the setpoint. CTV^-' DTH 000110243 r Operating Manual Old Unit PVC Reactors Page 2 III. OPERATING PROCEDURES (CONTINUED) C. Polymerisation (Continued) Procedure (Continued) 2. The lead operator will record the heat-up time on the batch sheet when the reactor reaches the setpoint. The heat-up time is the time from when the reactor charge was completed until the time that the temperature setpoint is reached. Heat up time should be close to one hour on the small reactors (D-300 through D-600) and about 30 minutes on D-700. If the heat-up times vary more than 15 minutes from this standard, the Shift Supervisor should be notified and the particle size should be watched. Heat-up times more than 15 minutes shorter than the standard may indicate that the reactor charge temper ature was too high or that the reaction is progressing too fast. Either condition may alter particle size significantly. Heat-up times more than 15 minutes longer than the standard may also cause the particle size to be undesirable. Long heat-ups may be caused by no steam on the reactor jacket, cooling water leaking through the automatic cooling water valve, or by the cooling water valve opening before the temperature reaches setpoint. No flow or not enough steam flow to the reactor jacket can be yerified by the "A" operator by checking the steam valves and lines. If the "A" operator cannot correct the problem, the/csiupervisor should be notified and maintenance may be necessary. DTH 000110244 Operating Manual Old Unit PVC Reactors Page 3 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Procedure (Continued) The latter two conditions can be temporarily corrected by lock ing out the cooling water valve manually or valving off the automatic valve with a manual valve. If the reactor cooling water is manually valved off or locked out, a potentially dangerous situation is created because as the realtor reaches the tempera ture setpoint the cooling water for heat transfer control is not in automatic. The lead operator must monitor the reactor temperature very closely to make sure the controller is put back in automatic as soon as the setpoint temperature is attained. A main tenance work order should be made out and this situa tion corrected as soon as possible,if it occurs. Slow reactor heat-up may also be caused by weak or not enough initiator. This can be determined by checking and comparing initiator loadings or subse quent batches. 3. The lead operator will continue to monitor the reaction temper .UL Tfw /''Jn pm ature and pressure as the polymerization continues. A It is K /.a** usually necessary to vent the inerts from the condenser to the recovery system shortly after run temperature is reached. *Jr f5 ft hd- (Cvt 000110245 dth sbth Operating Manual Old Unit PVC Reactors Page 4 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Procedure (Continued) Inerts blanketing the condenser becomes evident by the cooling water flow rising and the reactor temperature overshooting the setpoint causing the reactor pressure to rise. The inerts should be vented, as a general rule, if the temperature over shoots the setpoint by 2F and if the cooling water flow is rising quickly and^within one or two roots of the normal maxi mum cooling water flow. If the reactor and/or weather conditions prevail that make inert-venting a certainty, it is usually best to go ahead and vent the reactor as soon as the temperature setpoint is reached.This prevents excessive inerts buildup in the condenser --------and helps feeep-froa. excessive venting later during the polymer ization. The reactor may require venting several times during polymer ization. Several short vents are preferable and will do more good than long vents. During a long vent, the VCM tends to channel through the condenser and will be vented out of the reactor much faster than inerts will. If the vent is stopped and the inerts are allowed to "regroup" to the top of the con denser, they can then be more easily vented out of the reactor. The procedure for venting a reactor is given in this section 1 beginning on page^XX. DTH 000110246 Operating Manual Old Unit PVC Reactors Page 5 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Procedure (Continued) 4. If any abnormalities in pressure, temperature^ or reactor motor amperage are detected by the lead operator, the "A" operator may be instructed to sample the reactor and examine the resin to make sure it is not going coarse. The reactor sampling /pa. procedure is given in this section beginning on pag&.jtXr Some of the conditions which may warrant reactor sampling in clude: a. The first batches after changing batch size. b. The batches following a coarse batch or a batch that had a very high 60 mesh particle size result. c. Test run batches. d. Batches with abnormal charge temperatures or heat-up times. e. Batches that had abnormalities during charging. f. Batches that show abnormal changes in agitator motor amper age (either high or low) during polymerization. g. Batches that have sudden changes in reactor temperature or pressure, especially in the last few hours of polymeriza tion. Pressure cycling toward the end of a batch often y/ signals a batchyabout to go coarse. DTH 000110247 Operating Manual Old Unit PVC Reactors Page 6 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Procedure (Continued) The Shift Supervisor should be notified if any of these condi tions develop and the reactor should be sampled immediately. If a batch is suspected to be going coarse, methocel should be added to the reactor to keep the particle size from worsen ing. Tests have shown that addition of extra methocel after two hours at run temperature will not cause a batch to have finer particle size but it will prevent a batch from getting I --coarser. If it becomes necessary to sample a reactor, the batch should first be sampled one hour after the reactor reaches heat-up (the .run temperature) and then it should be re sampled every 30 minutes to every hour (according to the jjupervisor*s instructions) until the batch is killed. 5. As the normal polymerization reaches about 75% conversion of VCM to PVC, the reactor pressure begins to decrease. The lead operator will instruct the "A" operator to kill the reactor when it is 3-5 pounds before reaching the pressure drop speci fied on the reactor panel. By the time the reactor is killed, it will have reached the specified pressure drop. Reactor normal kill procedures are given in this section, beginning on page ixT ; 7/ 7 dth 000110248 Operating Manual Old Unit PVC Reactors Page 7 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Procedure (Continued) Other specified conditions that may require killing the reactor include if a reactor temperature run away (rise above setpoint) or maximum run time is reached. These guidelines are specified on the control room panel. Abnormal conditions during polymerization may also require early or emergency killing of a reactor. These will be dis cussed under troubleshooting in this section of the manual. beginning on page-XX*. 6. The reactor "A" operator will notify the lead operator when he completes killing the reactor. The lead operator will record the batch sheet the time when the reaction was killed and the pressure of the reactor when kill is completed. The reactor is then ready for recovery. Reactor Venting Procedure i 1. Check the reactor conditions as given under the polymerization ! -7 procedure, step 3 on page^XX to make sure the reactor needs to be vented. DTH 000110249 Operating Manual Old Unit PVC Reactors Page 8 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Venting Procedure (Continued) 2. Turn on the large reactor recovery system if it is not running. At least one seal water pump, both recirculation knockout tank pumps, and one compressor must be running while venting a reac tor. If the recovery system is already running, shut off what ever is feeding the recovery system (for example, if another reactor is recovering, close the condenser and recovery valves on that reactor). NOTE: It is not recommended to vent inerts while another reactor is in the vacuum-hold period of recovery. This may cause the batch that is recovering to have high residuals. However, inerts must be vented if necessary to prevent overpressuring of the reactor that needs venting. If it becomes necessary to vent a reactor while another reactor is recovering, make sure that both valves on the reactor that is recover ing are shut (condenser and recovery) and pull the recovery header back down to the vacuum that the re covering reactor has attained prior to re-opening the valves and finishing the recovery. A recovering re actor should also be held at vacuum five minutes longer than the usual holding time if the inerts had o ----------------- --to be vented during the vacuum-held period of the re- covery DTH 000110250 Operating Manual Old Unit PVC Reactors Page 9 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Venting Procedure (Continued) 3. Put the recovery pressure controller in manual and close the automatic valve. This prevents slugging the recovery system when high pressure is vented into it, and also reduces foaming during the vent. 4. Put the reactor to be vented in the emergency mode. This de activates the Modicon interlock controls and any of the reyv%<? v --actor valves .to be opened. 5. Open the reactor condenser and recovery valves. 6. Put the recovery pressure controller in automatic. This will let the valve slowly open and feed the inerts into the re covery system until the controller setpoint pressure is reached. 7. When the recovery pressure controller has been put in automatic and the reactor condenser and recovery valves open (it usually takes several seconds for the condenser valve to open), close the valves. I- * `/ h*.ariL DTH 000110251 Operating Manual Old Unit PVC Reactors Page 10 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Venting Procedure (Continued) 8. Monitor the reactor conditions and if temperature control on -the reactor is not yet restored after about a minute, repeat the procedure starting at step 3. NOTE: Several short vents are more effective than one long vent. If the reactor is allowed to vent too long, VCM in the reactor will channel through the condenser and out of the reactor and inerts will not be re moved. Closing the valves and allowing the inerts to gather back into the top of the condenser and then re-venting will dispose of the inerts more effi ciently. Long vents also may cause fine particle size because of the amount of VCM removed from the reactor. 9. When the temperature control on the reactor has been restored as indicated by the cooling water flow, temperature, or pressure dropping and returning to normal, turn off the reactor emer gency mode switch and the reactor should return to the poly pi Ar< fA-f'- 7 merization mode. Recheck all reactor activated valves to make sure they are closed. 10. Turn off the recovery system compressor(s) and pumps after it has pulled the pressure out of the recovery header, or go back to recover operationsvbefore venting. I A jJ i ` ' 2 DTH 000110252 Operating Manual Old Unit PVC Reactors Page 10a III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Sampling Procedure It may become necessary to sample the reactor during polymerization 5 as instructed in Polymerization Procedure No. 4, page *34X7, The re actor sampling cart must be used to sample the reactor unless the Shift Supervisor gives specific approval not to use it. The sam pling cart allows reactor samples to be taken from the reactor and the residual VCM in the sample is recovered by the recovery system, minimizing operator exposure. The cart has a sampling bomb (small vessel) and relief bomb (larger vessel) on it with a rupture disc between the two bombs rated at 300 psig. The following steps ? should be taken to sample the reactor* DTH 000110253 Operating Manual Old Unit PVC Reactors Page 10b III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Sampling Procedure (Continued) 1. Check to make sure the sampling bomb is totally drained, then close the drain valve. 2. Add % pint of AMS to the sampling bomb, using the kill bucket. The relief bomb will already contain h pint of AMS. The AMS in the relief bomb should be changed out on a weekly basis. 3. Close all valves on both bombs except the valves to the pressure gauges. 4. Flush the reactor sample connection by opening the valve and flushing with the HPSW connected to the sample line. Then shut off the HPSW and let the line drain. 5. Attached/ the sample hose to the reactor sample connection using Afl carir the Weco fitting. Use the wrench chained to the piatfown to tighten the fitting. 6. Open the 1" valve in the reactor sample line and the 1" valve on the sample hose. 7. Open the sample bomb hose valve. DTH 000110254 Operating Manual Old Unit PVC Manual Page 10c III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Sampling Procedure (Continued) 8. Open/reactor sampling ram valve using the local switch. When the pressure in the bobm reaches 120 psig, close the ram valve, the valve in the line^and the hose valve at the Weco fitting. Do not close the sample hose valve at the sample bomb. Block ing in the hose with the reactor contents may over-pressure and rupture the hose. 9. Check the pressure on the HPSW header. If the pressure is above 200 psig, open the HPSW line to the reactor and then the Hanuvalve, and flush the sample line for about 30 seconds, then r, close the sampling ^am valve using the local switch. Do not flush the sampling line formore than one minute. 10. Close the HPSW valve. Open the valve in the line and the hose valve at the Weco fitting. Slightly open the HPSWVgavle> and flush the hose into thebomb. Flush for about 10 seconds, then close the HPSW valve in the line and thehose valve at the Weco fitting. 11. Disconnect the sample hose at the Weco fitting using the wrench to loosen the fitting. DTH 000110255 Operating Manual Old Unit PVC Reactors Page lOd III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Sampling Procedure (Continued) Cart > 12. Move the sampling gystnai to the emission recovery system hook up station. In the new module, this is located at the west end of the reactor structure near reactors 742 and 743 near ground level. In the old module, this is located west of T-701 near ground level. 13. Connect the sample hose to the emission recovery hook-up sta tion with the Weco fitting. Open the sample hose valve and the emission recovery line valves and pull a vacuum on the sample bomb. 14. When the sample bomb is pulled down to at least 10 inches of mercury vacuum, close the bomb hose valve first, then the .emission recovery valve nearest the bomb and finally the second emission recovery line valve. 15. Disconnect the hose connection at the Weco fitting and break the vacuum on the sample bomb by opening|AMS funnel valve. ;~U,r t~~ 9 7^ ` 16. Move .`sampling .apparatus toAdrain location near .^emission/re covery hook-up station. The drain is located at the northeast corner of D-742 reactor structure in the new module and directly west of T-701 at ground level in the old module. DTH 000110256 Operating Manual Old Unit PVC Reactors Page lOe III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Sampling Procedure (Continued) 17. - Open the bomb drain valve slightly and let liquid AMS drain C\. off, then fully open the valve. Obtain a resin sample intone gallon sample bucket. The bucket should be filled at least 2/3 full. 18. Connect a water hose to the sample ttgbjn water hose connection and rinse the bomb through the drain valve. 19. Close the bomb drain valve, open the sample hose valves and flush the sample hose. 20. Shut off water to the sample bomb and disconnect the water hose. Open the drain valve and allow the bomb to drain com pletely. 21. The sample bomb is now ready for reuse. To obtain a reactor sample without using the sample cart, the "A" operator must perform the folowing steps: 1. Clear the area downwind of the sample point. 2. Connect and put on a fresh air mask. 3. Flush HPSW through the sample line to flush it out. A. Flush HPSW into the reactor per procedure step number 9 r (above), except do not close the ^am valve. DTH 000110257 Operating Manual Old Unit PVC Reactors Page lOf III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Sampling Procedure (Continued) 5. Shut off the HPSW, open the sample valve and let the reactor contents be blown to the ground until enough resin is blown out for a sample. 6. Shut the sample valve and flush the sample line again per step number 9 (above). 7. Close the HPSW flush. NOTE: The Shift Supervisor must give approval to sample a reactor without the reactor sampling cart. rPhe~~roao"> YAe rs*.<-tor sample should be closely examined by the "A" f operator. If resin particles that are stringy and stuck together or gritty resin particles which are ----------- ' harder and larger than most are observed, contact the lead operator and Shift Supervisor immediately. The batch may need to be killed and methocel added if these conditions exist and it is going coarse. Coarse batch procedures are given in Section R of , this manual. DTH 000110258 Operating Manual Old Unit PVC Reactor Page lOg III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Methocel Addition Procedure It may become necessary to add methocel to the reactor during polymerization for a variety of reasons. These may include if the batch is going coarse or if other batches running at the same time come up coarse or with high 60 mesh particle size results. The following procedure will be followed to add methocel to a charged reactor that is in the polymerization mode: 1. Check to make sure that no other reactor is charging. r ij&hculd- only be added to one reactor at a time. Methocel 2. Reset the methocel charge counter on the control panel to zero, by pushing the button below the counter readout. 3. Start the methocel charge pump and open the pump discharge valve. c&c '`C.y 4. Put the reactor in the emergency mode. 5. Open the colloid valve on the reactor. NOTE: Steps 3-5 will momentarily deadhead the methocel charge pump but will eliminate the risk of getting VCM and the ^reactor contents back through the methocel charge line and tank. The colloid charge valve on the reactor must be opened last when putting methocel into the reactor and closed first when the desired amount has been put into the reactor. DTH 000110259 Operating Manual Old Unit PVC Reactors Page lOh III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Methocel Addition Procedure (Continued) 6. When the specified amount of methocel has been added to the reactor, close the colloid charge valve. It may take two people (one to watch the meter and one to open and close the colloid charge valve) to perform this operation if a small amount of methocel is added to one of the reactors that are not close to the charge panel and methocel counter readout. GrtBU&tNc/ 7. Take the reactor out of the 'jEmeygenty') mode. 8. Shut off the methocel pump and discharge valve. 9. Record on the batch sheet how much additional methocel was added to the reactor. This should be recorded in the top right hand corner under the actual methocel charge section of the sheet. DTH 000110260 Operating Manual Old Unit PVC Reactors Page 11 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Normal Kill Procedure - NOTE: The chemicals used to kill the reactor are irritating to smell and should not be allowed to come in contact with the skin. Disposable plastic gloves must be worn while killing a reactor. If any of the kill solution splashes on a person, the affected area of skin should immediately be flushed. Medical attention should be sought if there is any burning sensation or reddening of the skin. 1. When told to kill a reactor, the "A" operator will put on dis posable plastic gloves to prepare for handling the kill solu tion. ^ 2. P.our the specified amount of Naugard, AMS, and antifoam into the marked 5 gallon bucket and transport it to the catalyst bomb (which is also referred to as the kill bomb). The amounts of raw materials to be used are posted in the control room panel and should be checked by the "A" operator at the first of the shift, and any changes noted. The specified-amounts may i total more than 5 gallons, so the operator will have to divide the amounts accordingly to make sure the correct amount of each ingredient is put into the kill bomb. DTH 000110261 Operating Manual Old Unit PVC Reactors Page 12 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Normal Kill Procedure (Continued) It is recommended that the Naugard and AMS be mixed together in the bucket because AMS will thin out the very viscous Naugard making the solution easier to pour. For best results j*k) the AMS should be put in the bucket first and Naugard poured the -ssb bucket and mixed with the AMS. are The 5 gallon buckets used for killing one marked at one gallon intervals to facilitate adding the proper amount of each raw material. Resin quality will be affected if the proper amounts are not added by every operator every time. The kill solution bucket must not be used for calcium stearate addition because the calcium stearate will coat the sides of the bucket and cover the marks. Notify the Shift Supervisor (and Operations Supervisor) if a marked bucket is not available and one will be supplied as soon as possible. ii - 3. Check the positions of the following valves: a. The valve at the base of the bomb funnel (it should be open). b. The valve which separates the bomb from the pressure, gauge (it should be open and the gauge should be showing no pressure). DTH 000110262 Operating Manual Old Unit PVC Reactors Page 13 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Normal Kill Procedure (Continued) NOTE; It is the operator's responsibility to change out any defective pressure gauges. Gauges on catalyst bombs should be changed out immediately if they have malfunctioned. c. The bomb drain valve (it should be open). d. The valve which supplies high pressure service water to the bomb (it should be closed). e. The bomb vent drain valve. 4. Close the bomb 'drain valve. NOTE: AMS is highly reactive in the presence of the catalysts used in the plant. Make sure that the bomb is drained and that no initiator remains in it prior to putting the kill solution in the bomb. 5. Pour the bucket of kill solution into the.bomb. Make sure that all the materials are added (Naugard, AMS, and antifoara) in the proper amounts. NOTE; Be careful not to splash the kill solution. If any kill solution gets on your skin, flush-immediately with water.. DTH 000110263 Operating Manual Old Unit PVC Reactors Page 14 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Normal Kill Procedure (Continued) 6. Close the bomb funnel valve. 7. Close the bomb vent valve. 8. Slowly open the valve which supplies high pressure service ^5* water to the cataflyst bomb. 9. Be sure that the valve which separates the bomb from the pressure gauge is open and allow the pressure in the bomb to increase to at least 200 psig and wait for the HPSW water meter to stop counting. NOTE; Extreme caution must be exercised by the "A" operator to be sure that the reactor contents are not allowed to get back into the kill bomb. To guard against this situation, the operator must know "that there is is adequate water supply and pressure on the bomb ber fore killing the reactor. The reactor catalyst ,Ram valve must" never be opened unless the bomb is fully pressurized and the" inlet HPSW valve is .open, r- 10. Open the catalyst injection ,Ram valve-fot'\reactor, which sepa rates the reactor from the catalyst bomb system. This is done with a local hand- switch _at the catalyst bomb." The catalyst bomb pressure should drop to about 150 psig. DTH 000110264 Operating Manual Old Unit PVC Reactors Page 15 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Normal Kill Procedure (Continued) 11. Allow 50 gallons (5 rounds) of water to pass through the high pressure service meter. NOTE: When the HPSW pressure on the bomb reaches 150 psig, a pressure switch activates a timer which gives the lead operator an alarm in the control room after 5 minutes. If the HPSW is cut off within 5 minutes, the alarm is de-activated. This is to give warning if the HPSW is left going into the reactor and is designed to prevent hydraulically filling the reactor when charging or killing -a reactor.^ The reactor "A" operator must remain at the kill bomb used while 'do jo killing a reactor. Failure to fulluw- tills "irrsHiuc*Js5if could result in the loss of a reactor contents to the atmosphere. 12. Close the catalyst Injection .Ram valve and then close.the high pressure service water supply valve (must be in the specified order). 13. Notify the lead operator that the reactor is killed. The lead will record the time and reactor pressure on the batch sheet. DTH 000110265 Operating Manual Old Unit PVC Reactors Page 16 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Reactor Normal Kill Procedure (Continued) 14. Open the bomb drain valve and then slowly and carefully open the bomb vent valve, then open the funnel valve. 15. Make sure the bomb is draining by checking the drain outlet. If the bomb did not drain, it may contain amounts of kill solution which may be hazardous. Check the drain by flushing it if it does not appear to be working. Troubleshooting As discussed in the operating procedures for this section, there are numerous abnormal situations which can arise. In almost every case the corrective measure will be the addition of some amount of AMS through the catalyst (kill) bomb or the Emergency AMS Addition System. The reactors are equipped with pressure relief mechanisms' which provide for reactor venting at excessive pressures. Safety discs on the small reactors are set at 185 psig (minimum) and safety discs on the D-700 1* . - are set at 205 psig (minimum). Although relief of excessive reactor pressure is necessary to avo'id equipment failure, control'should be re- stored as soon as possible afte^such' relief to avoid fire and per sonnel exposure hazards. DTH 000110266 Operating Manual Old Unit PVC Reactors Page 17 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) Coarse Batch - If a coarse batch is detected and found to be i/Don ij going coarse4 the batch should immediately be killed with five gallons of AMS and the usual amount of antifoam and Naugard. Fifty (50) gallons of methocel should also be added to the 10a reactor (see procedure on page "XX) and steps should be taken as given in the Coarse Batch Procedures section of this manual. Section R. The lead operator should record on the batch sheet why the batch was killed early (using the "Comments" section at the -H\. bottom of thirsr sheet), and that fifty gallons of methocel were added. 2. Long Reaction Time - This may be caused by low initiator levels, weak intiator, long heat-up times, or low reactor temperature setting. Maximum run times are given on the con trol panel for each product. If the run time gets within an hour of this maximum, the batch must be sampled by the "A" operator. If it reaches the maximum poly time,, the batch should be killed with the normal amount of kill-solution and recovered per normal procedures. DTH 000110267 Operating Manual Old Unti PVC Reactors Page 18 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) 3. Simultaneous Temperature and Pressure Drop - This is usually caused by the cooling water valves staying wide open. Even though the valve position and flow in the control room show that the valves and flow are normal, an instrument malfunction can occur, especially in freezing weather. The "A" operator should check the valves and throttle the manual cooling water valves if the automatic valves are staying wide open, until the problem is found and corrected. 4. Hydraulically Full Reactor - This occurs when too much of an ingredient is charged or an excessive continuous water source is allowed to enter the reactor during polymerization. A hy draulically full reactor has no place to relieve the closed-in pressure so the pressure will rise uncontrollably. The pres sure rise on a hydraulically full reactor may be so fast that it cannot be stopped. The following guidelines may be used to control a hydraulically full reactor if the pressure rise is caught in time. These are in order of priority such that if the first step does not control the pressure rise, the second one should be tried, etc. The Shift Supervisor should be noti fied as soon as this condition is noticed. DTH 000110268 Operating Manual Old Unit PVC Reactors Page 19 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) a. If the reactor pressure rises very rapidly with only a small rise or no rise in the reactor temperature, a hydraulically full reactor should be suspected. The lead operator should immediately vent the reactor to the recovery system by opening the reactor recovery and condenser valves (it is preferable to put the recovery pressure controller in manual and close the P valve first per the venting procedure, depending upon the rate of pressure rise in this situation, this part of the procedure -=P may be bypassed under these conditions only^. If the reactor is vented and the pressure drops immediately, this is a further indication that the reactor may be hydraulically full. b. The lead operator can put the emergency full cooling on the re actor and have the "A" operator shut off the lip seal and sprayhead flush flows. This will attempt to lower the reactor pressure and keep it * fr* om filling up more. - mfoatJ c. Equalize the reactor an evacuated reactor through the recovery line on tap or through the dump line on bottom, if an evacuated reactor is available. The receiving reactor must have been properly evacuated prior to-equalization. Equaliza tion through the recovery line should be used if necessary to prevent reactor overpressuring but may cause pluggage at low spots in the line due to resin carryover. DTH 000110269 Operating Manual Old Unit PVC Reactors Page 20 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) The recovery pressure control valve or knockout tank inlet (Jv'X'.cl valve should be oloed to prevent feeding the reactor through the recovery system. Equalization through the dump lines on bottom requires that the^ automatic slurry dump box w pinning-out the puuips'~and opening IIPSW into the suction^ line whiclr will overflow the dump~box and kegp-the va-lve closed. M hlanked-to-prevent leakage of-VCM to the atmos- d. Vent the full reactor into a recovered but not dumped reactor that is in the pressure drop or any stage of recovery (after shutting down the recovery system). e. Vent the full reactor into a reactor that is in polymeri zation mode that has lined out on temperature and pressure. 5. Temperature and Pressure Run-Away - Operational or mechanical conditions can exist such that loss of reactor temperature and pressure control can occur. . DTH 000110270 V \l Operating Manual Old Unit PVC Reactors Page 21 III. OPERATING PROCEDURS (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) jPuai a tv's.y' 5. Temperature and Pressure -Run-Away (Continued) When this loss of control occurs, some means of restoring con trol must be established. One such situation which can occur is a "Run -Away" or a "Heatji-^tick". As discussed in the polyCcAn hi f~ merization section, a certain amount of initiator is added to each batch. This amount of initiator varies from one season to another due to a variation in the cooling water temperature. (yJ The colder the cooling water the more initiator which can be used. The more initiator used the faster the reaction and ftuL shorter the polymerization time. The fPilant normally adjusts initiator amounts in half gallon increments. Sometimes half gallon increments are not accurate enough and an excess of initiator is charged for a given cooling water temperature. When this happens the reaction will proceed normally except at some point in polymerization the temperature (and possibly- the pressure) will b&gin to rise above the normal run condi tions, not responding to increases in cooling water flow. The following guidelines should be used to control a run-away reaction: a. The lead operator will try to vent the reactor using the . . j ncujA. V . venting procedure. If venting will not turn the JStaMMcaq*) y I ) the reactor will need to be "bumped". DTH 000110271 Operating Manual Old Unit PVC Reactors Page 22 III OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) Qu #|<UOa y 5. Temperature and Pressure Jhm-rAway (Continued) The lead operator will tell the "A" operator to "bump" the reactor. This means that a small amount of AMS, approximately one pint to one quart, is to be injected into the reactor through the catalyst bomb. The "A" operator will give bumping a reactor highest priority over any other task he is perform ing during normal operations. No Naugard or AMS is added to the reactor when it is bumped. The "A" operator will pour one pine to one quart of AMS into the kill bucket (just enough to entirely cover the bottom of the bucket) and will charge it into the reactor per the Reactor Normal Kill Procedure in this I . manual, beginning with step number 3 on page^XX. c. Bumping the reactor will normally restore control' of the reac tor. If the reactor temperature (and pressure) should continue to rise, the lead operator will have the "A" operator bump the is - reactor again. Unless word is given to kill the reaction, AMS should not be added'in more than one quart increments for run away reactions. This is because the AMS will carryover into tee fC;A the recovery system and the recovered --V6M and will affect par ticle size control of subsequent batches charged. DTH 000110272 Operating Manual Old Unit PVC Manual Page 23 III. OPERATING MANUAL (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) 5. Temperature and Pressure Ren-Awa/ (Continued) NOTE: The lead operator should closely monitor any reaction that has been bumped or killed early to make sure it does not "take-off" or begin to run-awa^ again. This will require further action steps by the lead or "A" operator. 6. Reactor Early Kill - If reactor run-away cannot be controlled or under various other abnormal conditions such as a plugged condenser, it may become necessary to completely kill a reactor that has been initiated (catalyst has been added). The Shift Supervisor must approve or give word to kill the reaction if the normal polymerization endpoints (pressure drop, maximum poly time, specified temperature run-away at the end of a batch) are not reached. The lead operator will tell the "A" operator to kill the reactor with 5 gallons of AMS and the Q '' normal amount of Nauga'rd and pentifoam. The lead operator must be careful to differentiate between "kill the reactor" (which implies normal kill procedures) and the early.kill situ ation where more AMS is added than normal kill procedures. The additional AMS is added to insure tha-t the .reaction is com pletely killed and because during the reaction there is more initiated monomer or catalyst in the reactor than at the end of the reaction. - DTH 000110273 Operating Manual Old Unit PVC Manual Page 24 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) 6. Reactor Early Kill (Continued) -- Reactions that are killed early will almost always have eoa- cl<95iralo\p a side.rab.Le quality characteristic's**! R gallon slurry sample should be taken when the batch is dumpedj^and sent to the lab for analysis. The lead operator will note on the batch sheet that the batch was killed early with 5 gallons of AMS and the batch should be dumped separate (to isolated blend tanks) if at all possible. It will then be blended into the large blend tanks according to the quality results on the slurry sample. 7. Emergency AMS Kill - If the temperature or pressure reaches the given ^emergency AMS kill parameters given on the control room panel, the batch must be immediately killed with the Emergency AMS Kill System. The system and procedure is described sepa rately below. Agitator Kicks Off or Power Failure - If the reactor agitator kicks off during polymerization, a low amperage alarm will sound. The lead operator should immediately try to restart the agitator with the agitator on/off switch on the'reactor panel ' t'f y . as the low amperage alarm is acknowledged and noty the Shift Supervisor. If the agitator does not re-start, the lead will have the "A" operator to check the reactor agitator motor f breaker and se-eet it immediately. DTH 000110274 Operating Manual Old Unit PVC Reactors Page 24 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Troubleshooting (Continued) 8. Agitator Kicks Off or Power Failure (Continued) Most power failures are of short duration (seconds to a few minutes) and the reactor pressure does not have time to build to a dangerous level. The lead operator should re-start the agitator as soon as power is restored. Both of these situations may necessitate the use of the Emer gency AMS Kill System, per the Shift Supervisor's instructions. Emergency AMS Kill System Procedures are described separately in the following section of this manual. Power Failure Proce dures are described in Section S of the Operating Procedures in this manual. Emergency AMS Kill Procedure Mechanical failures may occur during reactor polymerization which may result in loss of reaction control. Most of the time the mechanical failures that lead to this situation take the form of an overall plant power failure or a reactor agitator motor failure. Any condition that causes a loss of reactor agitation during poly^ merization may necessitate the use of the emergency' AMS Kill - -- System. Loss of^reactor agitator very rapidly reduces heat tran'-y fer in the reactor^ which may cause the reactor temperature and pressure to rise uncontrollably. DTH 000110275 Operating Manual Old Unit PVC Manual Page 25 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Emergency AMS Kill Procedure (Continued) The Emergency AMS Kill System nozzles must be tested on every reac tor on a weekly basis, according to the notice on the control panel. Both the manual and automatic injection nozzles must be checked and inspected by the Shift Supervisor. This can be done while the reactor is rinsing. Further testing procedures should be set up on a regular basis for testing the operability of each AMS kill pot. These procedures are given in Section T of manual. 1. The Emergency Kill System should be activated under the follow ing circumstances, according to the Shift Supervisor's instruc tions. a. Extended loss of cooling water to a reactor in the polymer ization mode. b. Extended loss of agitation to a reactor in the polymeriza tion mode. When agitation is lost, it is important to kill the reaction as soon as possible. The reactor contents will continue to swirl for about four.minutes after the agitator is shut down, and AMS injection during this period is much more effective. c. Any circumstances considered by the. Supervisor to represent a significant chance of over-pressuring the reactor or affecting the safe operation of the plant. DTH 000110276 Operating Manual Old Unit PVC Reactors Page 26 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Emergency AMS Kill Procedure (Continued) 2. The emergency kill system must be activated if the reactor reaches the following parameters for 5385, which is run in the old module: 145 psig or 142F. These are posted on the control room panel. 3. Under all circumstances of poor reactor temperature or pressure control% the lead operator should make sure that full cooling water flow is on the condenser (the switch on the affected re actor panel for emergency cooling water should be opened). 4. Upon the Shift Supervisor's instructions, the lead operator should remotely inject AMS into the polymerizing reactor which requires killing^by placing the panel emergency AMS injection switch in "AUTO". This automatically opens the double block valves on the AMS injection line and allows a low level switch to automatically closiet the valves_ . 5. The lead operator will inform the "A"- operator which reactor is being killed, and the "A" operator will immediately proceed to the Emergency AMS kill pot being used. DTH 000110277 Operating Manual Old Unit PVC Reactors Page 27 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Emergency AMS Kill Procedure (Continued) 6. The "A" operator will field-check the AMS injection on the reactor to be killed. He will confirm that the injection pot level is at a low level on the level gauge and will notify the lead operator when the level stops dropping. Too high a level fa means not enough AMS was injected,\effectively po kill the reac tor. No level may mean that nitrogen has entered the reactor. NOTEr When using the Emergency AMS System, radio communica tions between the lead operator and the "A" operator are crucial. The "A" operator must inform the lead operator how the system is operating and what is be ing done in the field. The lead operator must keep the "A" operator informed of reactor status and any apparent need for additional AMS injection. 7. The lead operator will confirm AMS injection from the controlpanel low level indicating light and from the "A" operator via radio. Injection time should be about- 30 .seconds. The injec tion pot low pressure alarm will normally be tripped.during AMS injection (it comes on below 275 psig). If-the pressure and level alarms are not tripped, tha automatic AMS injection line may be plugged requiring manual injection. DTH 000110278 Operating Manual Old Unit PVC Reactors Page 28 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Emergency AMS Kill Procedure (Continued) 8. If the automatic injection system fails to work, the "A" opera tor will manually inject AMS into the reactor, using the following procedure: a. Open both manual double block injection valves. b. Wait for the injection pot low level indicator light to come on (should take about 30 seconds). Immediately close the double block valves when the light comes on. The valves should also be immediately closed if the line begins to vibrate from flowing nitrogen. 9. After the reactor has been killed, the "A" operator will check the pressures of the nitrogen cylinders used for AMS injection. Any cylinder with a pressure lower than 750 psig should be changed out to allow for a second AMS injection, if needed. 10. After checking the ip^ection pot and nitrogen cylinders, the "A" operator will proceed to the reactor top level to confirm that the automatic injection valves are closed. If the valves are open, he should manually block in the line and inform the the lead operator that nitrogen has entered the reactor.. It may be necessary to vent nitrogen to the recovery system to maintain reactor cooling. DTH 000110279 Operating Manual Old Unit PVC Reactors Page 29 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Emergency AMS Kill Procedure (Continued) 11. After AMS injection, the lead operator will closely monitor the reactor temperature and pressure. If additional killing is required, the Emergency AMS injection "MAN" switch can be used which will open the automatic valves for as long as the switch is depressed. Caution should be exercised to prevent nitrogen from entering the reactor and blanketing the conden ser, when using the manual switch. The lead operator will have the "A" operator check the AMS kill pot level to check for nitrogen entering the reactor. If excess nitrogen does enter the reactor, the condenser may need to be vented to the recovery system to keep the nitrogen from blanketing the con denser and impairing heat removal from the reactor. 12. If additional injection is required, the "A" operator should prepare the emergency injection header for use. This header- is supplied to allow any injection pot to be used for.any re actor. This is accomplished by connecting one hose from a full and pressurized pot to the header and connecting a second -------- hose ftom the header to the appropriate reactor. Injection ( then proceed either locally or from the board. Caution should be exercized when using this header since the injection pot low level switches will_not work correctly and nitrogen may enter the reactor. DTH 000110280 Operating Manual Old Unit PVC Rectors Page 30 III. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Emergency AMS Kill Procedure (Continued) 13. As soon as possible after injection, the "A" operator must refill the empty ^SM'pot and prepare for a second injection if needed. The following procedure must be used to refill the AMS pot: a. Close the block valve on the nitrogen supply line at the pot. b. Depressure the pot through the pressure gauge vent valve. c. Refill the pot with AMS from a 55-gallon drum using the air operated drum pump supplied with the system. An al ternate filling procedure is to manually pour AMS into the funnel on the side of the injection pot. d. Block in the pot and repressure it with nitrogen from the nitrogen bottles. 14. If AMS will not kill the reaction, the nitric oxide (NO) emergency kill systeimt must be used. The fo- llowing procedure should be used to kill a reactor with NO. a. The "A" operato'r will put on a Scott Air Pack and test the face seal before proceeding to the NO bottles. NOTE: Nitric oxide is a highly toxic orange-brown colored gas. A Scott Air Pack must-be worn while killing a reactor with the NO system. DTH 000110281 Operating Manual Old Unit PVC Reactors Page 31 III. OPERATING MANUAL C. Polymerization Emergency AMS Kill Procedure (Continued) b. Open the valve on the NO bottles for the reactor to be killed. There are six NO bottles for each reactor D-300 through D-600 and there are twelve NO bottles for D-700. c. Open the manual valve on the header that puts the NO into the lip seal flush line. d. Replace the No bottles that were used as soon as possible. 15. If reactor pressure should continue to rise after Emergency AMS killing and NO killing has been completed, the following steps are to be taken: a>.fc>, Equalize the reactor with any other empty or killed reac IT tor of the same type product. P** If the pressure still continues to rise, vent through the main condenser valve to the recovery system and the re covered VCM receiver. c. If this will not relieve the pressure buildup, then equalize the reactor with a reactor of different type resin. DTH 000110282 Operating Manual Old Unit PVC Reactors Page 32 i HI. OPERATING PROCEDURES (CONTINUED) C. Polymerization (Continued) Emergency AMS Kill Procedure (Continued) d. If steps a, b, and c above fail to relieve the reactor pressure, the relief valve vent system will allow the reactor to vent through the relief valves to control the pressure. NOTE: Step d is to be the last resort. Under the new EPA law, any venting must be reported and could result in a fine. e. If the reactor pressure should continue to rise even after all the relief valves have lifted, the reactor vent valve should also be opened to assist in relieving the pressure, and to try to prevent overpressuring and failure of the reactor vessel. ** DTH 000110283