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CMS Chlorination Unit Start-up Procedures: 1 气密性试验 1. Pneumatic test
CMS Chlorination Unit Start-up Procedures: 1 气密性试验 1. Pneumatic test
CMS Chlorination Unit Start-up Procedures: 1 气密性试验 1. Pneumatic test
1 气密性试验
1. Pneumatic test
(1) 装置首次开车,由于管道焊接、法兰连接较多,以及对施工质量的检验,需要
采用高于正常控制压力进行检查(0.75 MPa)。压力高,更能够检查发现漏点,
也可以保证装置在开车后正常运行时的安全。
(1) For the large amount of pipeline welding and flange connection, and to test the
construction quality, a relative higher pressure (0.75 MPa) test is needed. If the pressure
is higher, it is easier to check the leakage and ensure the safe operation.
(2) 装置运行后,停车检修,由于装置开车后对所有管道、法兰、阀门、仪表等性
能进行了检验,符合要求。因此,需要临时停车后检修的管道、阀门等只需要
进行~0.3 MPa 压力测试,认真检查更换管道焊缝、拆卸法兰等 地方,如果 0.3
MPa 时无泄漏(这样检查可以确保焊缝无质量问题,安装法兰面清理干净,如
果在正常运行压力下有泄漏, 也可以通过紧固螺栓进行处理)泄压置换。
(2) During a shutdown after commissioning, only around 0.3 MPa pressure test is needed
for the attended pipeline and valves, for other pipelines, flanges, valves, and instrument
have already been tested to be qualified. Check carefully the wielding joints and flange
connections. If there is no leakage at 0.3 MPa (which means the welding joints are sealed
and flange interface is clean. Even if there is a leakage at running pressure, it can be
attended by tightening the bolts), release the pressure and purge N 2.
2 检测系统内含氧量
(1) 待系统氮气试压压力稳定并检查检修过的管道焊缝、法兰无漏点时,系统氮气
置换,做氧含量分析(具体操作方法:通过在再循环塔塔底 T2202 和预热器
E2202 预留口处接临时软管,进行氮气置换,置换用爆破吹扫的方式进行,在
三级分离器 S2203 处取样做含氧分析,使其氧含量低于 0.5%)。
(1) When the N2 pressure is steady and there is no leakage of the attended wielding joints
and flanges, flush N2 and analyze O2 content as follows: add hose pipes to the bottom of
T2202 and E2202, N2 blast, take sample at S2203 and make sure the O2 content is below
0.5%.
(2) 临时停车由于系统未打开,空气无法进入系统,此时不需要做氧含量分析,或
装置打开的反应器后面的系统,可以通过提物料压力从前往后系统赶的方式来
保证反应器前不进入空气时,也可不做氧含量分析。
(2) For temporary shutdown, air cannot go inside the system, thus O 2 content analysis is
not necessary. If the maintenance is at the later process after reactor, air can be kept away
from the system by increasing the pressure with material flow, thus no O 2 content analysis
is required.
3 用物料提升系统压力
After the procedures above, release all the N2 in thermal section. Then open the gas bypass of
V2202, V2203, and V2204. Increase the system pressure with material slowly. Line up all the
thermal section and maintain the pressure at 0.5~0.6 MPa (G). If there is no leakage, open
the isolation valves of V2202, V2203, and V2204 and close gas bypass valve. Then start
Electrical Heater (Y2201) to heat Reactor (R2201).
4 反应器升温
4. Heating reactor
(1) Heating the Reactor (R2201) with Electrical Heater (Y2201). Before heater starts, open
the N2 inlet valve for the protection cover. Set the “Reactor Inside Temperature” (TI2210) at
400 ℃. Set the Upper Limit of Copper Temperature at 550 ℃. At first, set the Heating Rate at
30 ℃/h. when the Cooper Temperature reaches 100 ℃, set the Heating Rate at 60 ℃/h. All
the setup are done on the Electrical Heater Panel.
5 开车前物料循环的操作步奏
5.1 开车前物料循环步骤
(1) V2202 - T2202 Circulation: through P2201, transfer some of the material in V2202 to
S2205 (Recycle Dryer), transfer the other to T2202 through E2208 and keep the T2202 level
at 65~70%. Then transfer the material back to V2202 through E2209.
(2) V2202 - T2201 Circulation: transfer the material in V2202 to T2201 through P2201, and
keep the T2201 level at 60~75%. Transfer the material in T2201 to V2202 through pipeline
CP-2051. After start-up, close this pipeline. Drain T2201 to V2205A/B every two hour. After
steaming, the organic in V2205 will be condensed to V2202 through E2211.
(3) V2203-E2204 Circulation: after P2202, transfer the material to E2204 Shell and keep the
level of E2204 at 35~40%. Circulate the material in E2204 Shell with P2203.
(4) Recycle Column System Circulation: transfer the material in V2202 to T2202 through
P2201, and keep the T2202 level at 65~70%. Increase the temperature of T2202 bottom to
around 130~140 ℃ with reboiler. The top pressure should be within 0.85~0.95 MPa (G).
The gas at the top will be condensed to V2204 through E2207. Material will reflux to T2202
via P2204 and keep the top temperature below 90 ℃
5.2 液位及压力调整
★ 液位调整
经过上述物料混合循环后,以下贮槽液位调整入下:
V2202 30%以上
V2204 40%以上
★Level adjustment
6 正常开车及操作
开车前应保证液氯气化系统运行正常,氯气出口压力控制在 0.90~1.20MPa (G);
要求精馏系统已运转;必须保证氯化氢洗涤塔 T2404 及氯气尾气洗涤塔 T2405 系统工
作正常,运行合格,HCL 吸收系统也必须处于正常状态;氢氯化单元处于备开状态。
完成上述准备工作后,热氯化单元就可以开车了。
6. Start-up steps
Before start-up, make sure Liquid Cl2 Vaporizer System runs normally and keep the PIC
2201A at 0.90~1.20MPa (G); make sure the Rectification Unit is in operation; make sure
T2404, T2405 and HCl Absorption System run normally; and make sure Hydro Section is
ready. After all the above preparations, Chlorination Unit is ready to start.
(1)打开所有电伴热。
(3) Open the valve on liquid line from E2207 to V2204. Open XCV2209. Open XCV2208
(balance valve).
(5) Slowly open TV2224 (steam valve). When the pressure in T2202 increase to 0.9 MPa,
open HV2202, HV2203, PV2221. Line up XCV2210 to T2404 (emergency release) and vent
noncondensable gas into VG4 Header, then close the valve.
(6) Increase the bottom temperature of reactor (see TIC2224). Open FV2219, reflux the
material from V2204 to T2202 top, and keep TI2227 at below 90 ℃. Slowly open HIC2202
to control the top pressure (PICA2221) within 0.85~0.95MPa (G).
(7) When material is condensed to V2204 by E2207, adjust reflux flow to ensure T2202 level
(LT-2212) is stable at 60%~80%. Set LICA2212 Auto and keep the level at 60%~80%. If
the level is too high, adjust LV2212 to return the material to V2202.
(8)调节合适进料量、回流比、蒸汽量、建立平衡。
(8) Adjust the feed, reflux ratio and steam flow to establish balance.
(9) When TI2210 reaches 400 ℃, open HIC2203 to 40%~100%. Line up XCV2210 to
CH3Cl Feed Preheater (E2202AB). Slowly open PV2221 to 5%~10% to transfer the CMS
from Recycle Column to R2201 through E2202A/B. Then start refrigerator and make its
whole system running.
特别注意:
再循环塔处理的物料中会含有氯化氢及系统中微量的水份。当进料中水份偏高
(大于 1000ppm 以上)时,塔盘将被腐蚀,严重时会发生脱落。因此必须严格控制氯
化系统中水份低于 300ppm。
Note:
The material in Recycle Column contains HCl and trace moisture. When the moisture content
of feed is higher than 1000 ppm, the column tray will be eroded, and even fall off when it’s
serious. Therefore, moisture in Chlorination Unit must be kept under 300ppm.
注意:E2202A/B 为一开一备。
CMS from the Recycle Column enters reactor R2201 through E2202A/B. Open TV2206 10%
manually at first, then set it to auto. The set temperature is 80~90℃.
Note: For E2202A/B, run only one and the other is standby.
6.4 氯气进料 (V2206/R2201/T2202)
After confirming that the V2206 chlorine system has passed the 1.0MPa (G) pneumatic test,
notify all the people to leave the field and Cl 2 is going to feed. Carry out the following
operations:
(1) Open the valves on the inlet and outlet pipeline of the Cl 2 Surge Drum V2206. Set
PV2201 to manual and set the opening zero. Open the FV2203 upstream valve, and the
downstream valve is to be opened just before Cl 2 feeding. Set FV2203 to manual and set the
openness zero. When there is pressure in the pipe, slowly open PV2201(regulating valve).
When the pressure of Cl2 Surge Drum increases gradually, set PV2201 to auto.
(2)保证氯气输送管道电伴热的正常运行,防止管道内气氯降温液化。(开车前启用
缓冲罐及其后面的导淋阀,排放氯气管道内的氯气去 T2405 几分钟,防止有冷凝的液
氯进入混合器。)
(2) Ensure electric tracing on chlorine pipeline work normally to prevent gas Cl 2 from
liquidation. (Before start-up, line up the Surge Drum and drain valve. Discharge gas Cl2 to
T2405 for a few minutes to prevent liquid chlorine from entering the mixer. )
(3) When PIC2201 is stable at 0.90~1.20MPa (G), open XCV2201, open the upstream and
downstream valves of FV2203, and slowly open FV2203, feeding gas Cl 2 to R2201. Open
FV2203 slowly 0.5% ~ 1% at first. At this time, pay close attention to TI2210 (Reactor
bottom temperature), and normally the temperature should be an upward trend. Then
gradually open FV2203 1%, 2%, 3%... In the process of feeding gas Cl 2, the opening of
PV2221 must be increased slowly according to the reaction temperature at the same time.
(4)开始热氯化反应主要集中在反应器下部,控制好混合氯化物和氯气的加入比例和
节奏,控制好反应器的温度。
(4) In the beginning, the chlorination reaction was mainly at the bottom of the reactor. Have a
good control of the reactor temperature by controlling the ratio and rate of CMS and gas Cl 2
feeding.
6.5 热氯化系统压力的控制(S2203)
(1)反应稳定后,对氯化系统进行全面检查。各漏点是否泄漏,仪表、机泵是否正常,
膨胀节、弹簧、支吊架是否正常,现场数据是否与 DCS 显示一致,确认无误后逐步提
高整个反应系统的压力至正常操作压力。
(1) After the reaction is stable, check the chlorination system comprehensively. Check if there
is a leakage, if the instrument and pump run normally, if the expansion joint, spring and
support are normal, whether the field data is consistent with the DCS display. If everything is
normal, gradually increase the pressure of the whole reaction system to the normal operating
pressure.
(2)随着循环氯化物和氯气的加入,反应持续进行,反应系统的压力逐步升高,通过
三级分离器 S2203 上的调节阀 PV2218A、PV2218B 和 PV2219B 来控制反应系统压力。
(2) With circulating CMS and gas Cl 2 feeding, the reaction continues. The pressure of the
reaction system increases gradually. The pressure of the reaction system is controlled by the
regulating valves PV2218A, PV2218B and PV2219B on the Third Separator S2203.
(3) In the initial stage, manually turn on PV2218A, and turn off PV2218B, adjust the opening
of PV2219B so that the pressure of S2203 is controlled at around 0.6MPa (G), the pressure
(PI2210) of R2201 is around 0.63Mpa (G). With the increase of load, the pressure of S2203 is
also increasing, and is maintained at 0.62~0.65Mpa (G) by adjusting the opening of
PV2219B.
(4) When the reactor temperature is above 380℃ and the outlet temperature (TI2222) of
E2205-1 is below -15℃, the HCl concentration at the outlet of S2203 is above 90~95%wt,
notify the lab to analyze the concentration of HCl and the content of free Cl 2. If the result is
qualified, transfer HCl to Hydro Chlorination Unit, and be ready to start 100# Unit.
在 E2205 投入系统之前,首先保证冷冻机全负荷运行。
First of all, ensure the full load operation of the Refrigerator before the E2205 is put into
operation.
The R22 from the Refrigeration Unit enters the shell of E2205. Set CV2876 to “Auto”
and the value at around 30%.
(1) As the reaction proceeds, light components such as CH 3Cl and HCl are gradually
condensed to V2203. When the level of V2203 is more than 15%, start the pump P2202A/B,
keep circulating.
(2) Most of the materials in V2203 are CH 3Cl and HCl, and the others are organic and inert
gases. Therefore, the pump P2202 is prone to cavitation. So while maintaining a certain level
in V2203, the pressure of S2203 should not be lower than 0.6MPa (G). The pressure of the
reaction system is maintained above 0.6Mpa (G), which is beneficial to the normal operation
of P2202.
3) Set the TV2220 to manual and open the regulating valve,the materials is transferred from
V2203 to E2204 via P2202. Set LV2204 to automatic, the SV of LICA is 40% ~ 50%. The
gas from S2201 will change heat with the material in the tube and shell of E2204. CH 3Cl and
HCl will evaporate in the shell, and the pressure increases gradually. The PV2214 is set to
auto and the set pressure is controlled at 0.70~0.85MPa (G).
(4) The evaporated CH3Cl and HCl and other light components will be mixed with circulating
CMS from T2202 and fresh CH3Cl from E2201, and entered the reactor R2201 through
preheater E2202A/B to react. With the increase of circulating gas in E2204, adjust the outlet
flow at the top of Recycle Column to keep the total amount of CH 3Cl at the outlet of E2202
unchanged.
(1) The CH3Cl is stored in the V2104A/B and transferred to E2201 by P2107.
(2) Set FV2205 fully open. The opening of LV2201 is adjusted automatically according to
the level of E2201. The level of LICA2201 is set at 35% ~50%.
(3) Open XCV2202. The opening of steam regulating valve (PV2204) is automatically
adjusted according to the evaporation pressure in E2201 shell, and the evaporation pressure
is set at 0.9MPa (G).
(4)上述操作完成后,缓慢开启 FV2202,通入一氯甲烷后,一定注意观察反应器
R2201 的温度变化,及时增加氯气。
(4) After the above operation, slowly open FV2202. After feeding CH 3Cl, attention must be
paid to the temperature change of reactor R2201, and increase Cl 2 in time.
※特别注意:
E2201 的操作关键在液位和蒸发压力的控制。由于一氯甲烷属于液化烃,对应温度下
必须有 80%的气相空间,液位控制不好或满液就可能造成压力瞬时升高甚至爆炸。所
以在 E2201 投入运行前一定要检查及标定就地液位计,使其和集中液位计指示一致。
The key to the operation of E2201 lies in the control of level and evaporation pressure. CH 3Cl
is liquefied hydrocarbon, if the level is not well controlled or the level is full, it may cause
instantaneous pressure to rise or even explosion. Therefore, it is necessary to check and
calibrate the LG before E2201 is put into operation, and keep it consistent with DCS display.
6.9 再循环塔塔底到精馏系统
随着反应的进行和用氯量的升高,再循环塔塔底温度逐渐上升,当温度升高到~130℃
时,通知分析在 E2209 处,取样分析,当检测出无一氯甲烷时,将再循环塔塔底物料
倒至 V2301A。
With the reaction proceeds and chlorine flow increases, the temperature at Recycle Column
bottom increases gradually. When the temperature rises to about 130℃, notify the lab to take
a sample at E2209 and analysis. When CH 3Cl is nil, transfer the material at the bottom of
Recycle Column to V2301A.
※特别注意:
(2)P2201AB/P2202AB 机泵
(2) P2201AB/P2202AB
Because the mixed material contains light components such as HCl and CH 3Cl,
P2201AB/ P220AB is prone to cavitation during start-up, especially when the system pressure
is low. When cavitation occurs, open the valve on the outlet pipeline of the pump, discharge
the gas in the pipeline, and start the pump again.
至此热氯化单元的所有关键设备和仪表都已投入运行。保持反应器温度稳定,系统
压力平衡,贮槽液位平衡是操作的关键。
So far, all the key equipment and instruments in the Thermal Chlorination Unit have been
put into operation. The key to the operation is to keep the temperature of the reactor stable,
the pressure of the system balance and the level of the tank balance.
热氯化系统按照上述操作正常运行后,进入后续精馏系统。精馏系统控制好二三氯
精馏塔的灵敏板温度,并保持精馏塔的稳定运行,使二三氯塔顶的产品质量高于
99.95%时,进入共沸系统除游离酸和水分后,进入二三氯检测槽分析,使二三氯检测
槽的产品质量达到 99.95%,水分低于 100ppm,色度低于 10,游离酸未检出时,输送
至成品罐区,从而进行产品的包装和发放。
After the Thermal Chlorination System runs normally according to the above operation,
it enters the subsequent Distillation System. Control the sensitive plate temperature of the
MDC and CFM Distillation Column and maintains the stable operation, make product purity
at the top of the MDC and CFM tower higher than 99.95% respectively. After the acidity and
moisture are removed in the Azeotropic System, transfer the material to MDC and CFM
Check Tank and analyze. When the purity of the MDC and CFM reach 99.95% respectively,
moisture is less than 100 ppm, the color is less than 10, and acidity is nil, transfer them to
Storage Tank Area for packaging and distribution of products.