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Casale300B type ammonia synthetic tower TA201-2/ TA201-2 – H

时间:2019-04-09 点击: 192 次

Casale300B型氨合成塔使用TA201-2/TA201-2-H型氨合成催化剂升温还原技术要求
Casale300B type ammonia synthetic tower TA201-2/ TA201-2 – H
The ammonia synthesis catalyst reduction technical requirements
催化剂的还原质量关系到催化剂的性能能否正常发挥,因此,事先应制订升温还原方案。本次的还原采用分层还原,由于就是第一床层选用预还原型的TA201-2-H型氨合成催化剂,它是采用氧化态的TA201-2型氨合成催化剂在制造厂专用设备中预先进行还原,然后有控制的进行表面钝化处理,使其在催化剂的表面生成一层氧化亚铁薄膜,当催化剂使用前,装入塔内进行还原时,由于预还原氨合成催化剂还原起始温度低(约200℃),其主还原期也比A110系列约低20~30℃,因此先对一层进行还原,在一层进入还原末期前,控制二层入口温度在还原主期温度之下(300~320℃),,才提高温度使二层进入还原主期,以下依次类推。由于均为径向段,因此,当第一层还原后,可利用氨合成反应热逐渐加大气量,提高空速,使还原进度加速进行。
Catalyst reduction quality decides the performance of the catalyst , therefore, it needs make a temperature-rising reduction plan in advance. With hierarchical reduction, the first layer with pre- reduction  reaction TA201-2 - H type ammonia synthesis catalyst, it is the oxidation state of TA201-2 type ammonia synthesis catalyst reduction in specialized equipment , then do the surface passivation treatment to generate a layer of ferrous oxide film in the surface of the catalyst, before using catalyst, when doing reduction reaction in tower, the pre reduction reaction ammonia synthesis catalyst is in low temperature (200 ℃), its temperature of main reduction period is  20 ~ 30 ℃ lower than A110 series , So it needs reduction  the first layer , before the end of the first layer reduction,make sure the temperature of inlet on the second layer is around 300 ~ 320 ℃, and then raise the temperature to make the second layer going through main reduction reaction period, the following analogy in turn. So after finishing the first layer reduction, it can gradually increase the air volume, improve the airspeed, accelerates the reduction reaction.
4.1 催化剂升温还原前的准备工作
4.1 Preparation before the reduction of catalyst
4.1.1 合成单元的气密试验工作已结束。
4.4.1 Synthetic unit of air test work is over.
4.1.2 各设备、调节阀、仪表元件等均处于良好状态。
4.1.2 All equipment, regulating valve, instrument components are all in good condition.
4.1.3 合成回路进行氮气置换合格,合成塔吹灰后。压缩机采用氮气进行系统循环,并清除过滤器中的催化剂灰。
4.1.3 Synthesis loop qualification nitrogen replacement, synthetic tower after blowing. Compressor with nitrogen cycle, and the catalyst ash removal filter.
4.1.4 排氨水的临时管道配置结束,稀氨水接收装置具备接收氨水的条件。
4.1.4 Row of temporary ammonia pipeline configuration is over, dilute ammonia receivers can receive ammonia.
4.1.5 化验室具备分析还原水汽浓度和气体成分等条件
4.1.5 Laboratory has the condition of analysis water vapor concentration and gas composition.
4.1.6 开工加热电炉具备投入运行的条件。
4.1.6 Starts heating furnace works well.
4.1.7  对所有连接处进行检查,确认无泄漏。
4.1.7 Inspection on all joints, confirm no leakage.
4.2 催化剂的升温还原
 4.2 Temperature rising reduction of the catalyst
4.2.1 升温阶段
4.2.1    Stage of temperature rising
4.2.1.1第一床层的热点温度从常温升至200℃,升温速率为30~40℃/h,合成回路的操作压力逐渐升至8Mpa左右。
4.2.1.1 The first layer hot spot temperature ,from room temperature to 200 ℃, the heating rate is 30 ~ 40 ℃ / h, the operation of the synthesis loop pressure gradually rose to about 8 mpa.
4.2.1.2 气量由压缩机,和合成塔前放空阀等控制,在满足升温速率的情况下,尽量提高空速。
4.2.1.2 Gas from the compressor, and synthetic tower before emptying valve control, such as in the case of satisfy the heating rate, try to improve the airspeed.
4.2.1.3 热负荷由开工加热电炉提供,应根据设计单位提出的对加热电炉安全气量的要求进行操作,在容许的条件下加大电炉功率,提高床层温度。
4.2.1.3 Heat load is provided by starts heating furnace and should be operated  according to the of gas in heating furnace safety requirements, under the allowed condition,  increase its electric power, and increase the layer temperature.
4.2.1.4 一层催化剂到达200℃,开始分析出口气体的水汽浓度,每小时进行一次。严格控制出口气体中水汽浓度小于1000ppm(V/V)。
4.2.1.4 when catalyst in the first layer reaches 200 ℃, starts to analyze the outlet gas water vapor concentration once an hour. Strictly control the outlet water vapor concentration is less than 1000 PPM (V/V).
4.2.2  还原初期
4.2.2 The early catalyst reduction reaction
从300~360℃为催化剂的还原初期。
The early catalyst reduction reaction means the temperature range is 300 ~ 360 ℃.
4.2.2.1 当催化剂床层温度达到300℃左右,催化剂便进入还原初期。此时催化剂开始出水。当达到340℃以上,出水已十分明显。应加大水汽浓度分析频率,建议每半个小时分析一次。并每两个小时测定一次进口气体中水汽含量。入塔气体水汽浓度越低越好,最大不得超过200ppm。
4.2.2.1 When catalyst layer temperature is up to 300 ℃, catalyst  is into the early reduction reaction. Water comes out from catalyst. When reaching above 340 ℃, there is much water. Should increase the water vapor concentration analysis frequency, it is suggested that once half an hour to analysis. And test water vapor content in inlet gas every two hours. The lower gas water vapor concentration,the better ,but no more than 200 PPM.
4.2.2.2  从300℃逐渐升至360℃,控制升温速率为10~15℃/h,合成回路压力维持8Mpa左右。
4.2.2.2 In the process from 300 ℃ to 360 ℃, controlling the heating rate as 10 ~ 15 ℃ / h, the synthesis loop pressure is around 8 mpa.
4.2.2.3  热点温度达到320℃左右后,已还原的催化剂将发生明显的氨合成反应,产生合成反应热。此时应注意床层的温度,防止温升过快。若发现温升过快,可加大循环气量。同时注意控制好塔出口的水汽浓度不得大于1000ppm。
4.2.2.3 After hot spot temperature reaches 320 ℃ , the catalyst which has done reduction reaction will happen ammonia synthesis reaction obviously, synthetic reaction heat is produced. At this time pay attention to the layer temperature, in case the temperature rising too fast. If found that temperature rising too fast, can increase the circulation of air. At also control the water vapor concentration in outlet is no more than 1000 PPM.
4.2.2.4 氨水浓度达25~30%时,投用氨冷凝器。
4.2.2.4 When ammonia concentration is up to 25 ~ 30% starts using ammonia condenser.
4.2.2.5 当分离器中有液位后,可通过排放阀排放低浓度的稀氨水排放到沟。并每小时对氨水浓度进行一次分析。氮水浓度达30%左右,停止排放,回收到贮罐。
4.2.2.5 When there is a liquid level in the separator, using discharge valve to let our low concentration of dilute aqua ammonia . And make a analysis for ammonia concentration per hour a time. Nitrogen concentration is about 30% water, stop discharging, recycling to the storage tank.
4.3  还原主期和末期
4.3 The middle and end catalyst reduction reaction
从360~440℃是TA201-2催化剂的还原主期。而440~470℃为还原末期。
Middle period: From 360 ~ 440 ℃ ; the end period is from 440 ~ 470 ℃
4.3.1 催化剂在360~440℃这段温区内,催化剂大量出水。因此应降低升温速率,视出口水汽浓度进行调节,一般为1~5℃,并加大循环气量,必要时可以稍为提高压力,但最好不要超过10Mpa。
4.3.1 When catalyst temperature is 360 ~ 440 ℃, catalyst comes out much water. Therefore should reduce the heating rate according to the water vapor concentration in outlet,usually its 1 ~ 5 ℃, and also increased circulation gas, can slightly improve the stress if necessary, but no more than 10 mpa.
4.3.2  当一段催化剂进入还原主期时,二层催化剂也会进入还原初期。因此,应严格控制二层的温度,尽量使其不超过320℃,以防止两层催化剂一起进入还原主期,出水过猛,使水汽浓度严重超标。
4.3.2 When the first layer catalyst is in middle reduction reaction period, the second catalyst will  enter the early reduction reaction . Therefore, we should strictly control the temperature of the second layer, try to make it less than 320 ℃, in order to prevent the two layers of catalyst enter both middle reduction that will lead to suddenly much water, water vapor concentration will exceed badly.
4.3.3  一段催化剂还原主期的水汽浓度可控制在1500ppm以下,每半个小时进行一次出口气体水汽浓度的分析。每二个小时进行一次进口气体水汽浓度的分析。
4.3.3 Catalyst in middle reduction period ,its water vapor concentration can be controlled below 1500ppm, do analysis for outlet gas water vapor concentration every half an hour. do analysis for inlet gas water vapor concentration every two hours.
4.3.4  为了保证催化剂的彻底还原,上层催化剂进口的温度可升至360~380℃,上层出口温度可控制在470±10℃。
4.3.4 In order to ensure the catalyst reduction reaction completely, upper imported catalyst could be up to 360 ~ 380 ℃, the temperature of the upper outlet temperature can be controlled in 470 ±10 ℃.
4.3.5  一层催化剂升至440℃后,可视出口水汽浓度的情况,把升温速率提高到10~15℃/h。
4.3.5 When the first layer temperature is up to 440 ℃,depending on the water vapor concentration of outlet, increase the heating rate to 10 ~ 15 ℃ / h.
4.3.6 一层催化剂进入还原末期时,可把二层催化剂的温度逐渐升至380℃,使二层催化剂进入还原主期,并以1~5℃/h的升温速率继续升至440℃,440℃后,以10~15℃/h的升温速率继续升至470±5℃。
4.3.6 When the first catalyst layer enter into the end reduction reaction period, you can increase the second layer catalyst temperature gradually to 380 ℃to let the second layer catalyst enter into the middle reduction reaction period, and increase the temperature to 440 ℃by 1 ~ 5 ℃ / h heating rate ,when reaches 440 ℃, continue increasing temperature to 470 + 5 ℃ by 10 ~ 15 ℃ / h heating rate .
4.3.7当二层催化剂进入还原末期后,把三层进口温度提高到360℃,使第三层催化剂进入还原主期,并以1~5℃/h的升温速率继续升至440℃,440℃后,以10~15℃/h的升温速率继续升至470±5℃。并保持4~6个小时,使全部催化剂得到较彻底还原,确保还原的质量。
4.3.7 When the second catalyst layer enter into the end reduction reaction period, increase the third layer inlet temperature to 360 ℃, to let it enter into the middle reduction reaction period, and increase the temperature to 440 ℃by 1 ~ 5 ℃ / h heating rate ,when reaches 440 ℃, continue increasing temperature to 470 + 5 ℃ by 10 ~ 15 ℃ / h heating rate . And keep it for 4~ 6hours, to make sure all catalyst reduction reaction completely. And keep in 4 ~ 6 hours, make all get relatively thorough reducing catalyst, to ensure the quality of reduction.
  1. 4.3.8连续三次分析出口的水汽浓度稳定时,把还原温度提高1~3℃后分析出口的水汽浓度没有升高,整个还原结束,调整工艺参数,把负荷调整到70~75%,进入轻负荷生产期,轻负荷生产期为24~48小时。
4. 4.3. 8 continuous three analysis of outlet water vapor concentration, if stable, increase the reduction reaction temperature 1 ~ 3 ℃ then analysis if outlet water vapor concentration didn’t increase, the whole reduction reaction comes to an end, adjust process parameters and the load adjusted to 70 ~ 75%, into the light load production period, light load production period for 24 to 48 hours.
4.3.9  整个升温还原过程,必须认真做好记录,及时绘出升温还原曲线,精心操作,加强检查。
4.3.9 The whole reduction reaction, must be recorded carefully, make curve chart in time, elaborate operation, strengthening inspection.
4.4 还原中几点注意事项
4.4 Attention
4.4.1 还原过程中,应适当提高氢气含量,要求循环气中氢气含量达78~80%。
4.4.1 In reduction reaction process, should increase hydrogen content and require hydrogen content in the recycle gas amount to 78 ~ 80%.
4.4.2 当一层催化剂合成氨反应较强,放出热量大时,应及时调节循环气量及适当关小开工加热电炉功率,当合成反应热已足够维持系统平衡的热量时,可以逐渐关小开工加热电炉。
4.4.2 When the first layer of catalyst for synthetic ammonia reaction is strong, gives off huge heat, should be timely adjust circulation volume appropriately and slow down starts heating furnace power, when the heat of synthesis reaction is enough to maintain system heat balance, you can start gradually turn down the heating furnace.
4.4.3 为了保证每层全部催化剂能够达到彻底还原,每层出口温度必须升至480℃左右,为了防止上层温度过高,因此可采用低压、大空速、高氢的条件进行作业,一方面制止上层的合成反应,减少反应热;另一方面使有更多的氢来促进下层的还原。
4.4.3 In order to ensure each layer catalyst reduction reaction completely, every layer outlet temperature must rise to around 480 ℃, in order to prevent the upper temperature is too high, so can use low pressure, big space velocity, high hydrogen conditions for operation, on one hand to prevent the upper synthetic reaction, reduce the heat; On the other hand make more hydrogen to promote the reduction of the lower layer.
4.4.4 在下层催化剂进入还原主期后,为了提高空速,可以适当提高压力,但要求不超过去10Mpa。
4.4.4 After lower layer catalyst enter to the middle reduction reaction period, in order to improve the space velocity, you can appropriately increased pressure, but required less than 10 Mpa.
4.4.4 在下层催化剂进入还原主期后,为了提高空速,可以适当提高压力,但要求不超过去10Mpa。
4.4.5 When the ammonia concentration is up to more than 95%, according to the factory condition, send the ammonia into ammonia storage tank.
4.4.6 升温还原时应严格遵守以下原则:提温不提压,或提压不提温,不可同时提温又提压。每次提温或提压时,应维持一段时间,观察温升情况和出口水汽浓度,当确定温升正常或水汽浓度未发生变化时,方可进入下一轮提温或提压的操作。
4.4.6 Following principles when temperature rising reduction : increase temperature without pressure or increase pressure without temperature, can’t increase both temperature and pressure at the same time. Every time when increase temperature or pressure, shall be maintained for a period of time, observe the temperature rise and outlet water vapor concentration, when can confirm the temperature or water vapor concentration did not change, you can enter the next round of the temperature or pressure operation.
4.4.7 所有分析数据应及时报到合成塔操作岗位,并认真做好记录。
4.4.7 All the analysis report data should be timely sent to synthetic tower operating post, and carefully recorded.
4.4.8 建立统一指挥,专人负责,一切服从统一指挥的决定。还原中遇到的问题应及时反映,组织讨论,由统一指挥下达更改措施。
 
4.4.8 Establish a unified command, special person arranged. Any problems, should be reflected in a time, group discussion, changed by the unified command issued measures.
4.4.9 还原过程中如需进行加减压,其速度不得太快,特别是降压时应小于0.2Mpa/min。
4.4.9 If you need to add or subtract pressure in the process of reduction reaction, the velocity should not be too fast, especially when decompression should be less than 0.2 Mpa/min.
4.4.10 停车
4.4.10 Shut down
当前面工序或合成系统内的设备发生故障时,需要停车,应先查出造成停车的原因,根据不同情况按以下方法处理。
When current process or any breakdown in equipment it needs shut down. Find out the reason, according to the following methods to handle it.
4.4.10.1 计划停车
4.4.10.1 Shut down planning
首先停开工加热电炉,停供新鲜气,压缩机进行大回路循环,使床层温度降低50以上,并将塔内的水汽带出塔外。然后隔开大回路同小回路的联系,在小回路内自身进行循环。如需停压缩机,可在现场停开。
短时停车时,则可采用切断合成系统或合成塔与外界联系的阀门,保压保温的方法。
长期停车时,则需先用氮气进行置换。
First stop the start heating furnace, stop providing fresh air, the compressor will be in large loop cycle to make layer temperature more than 50℃ , then can take water vapor out of the tower. Then separated by big circuit with small loop connection, in a small loop cycle within itself. If you want to stop the compressor, then stop it at the scene.
1. Short time shutting down, cut off the synthesis system or synthesis tower connection with the outside, keep the heat pressure and temperature.
2. Stop time shutting down,it need to use nitrogen to replace first.
4.4.10.2 事故停车
4.4.10.2 Accident shut down
如非合成回路造成成的停车,可参照计划停车方法处理。
压缩机故障时,停开工加热电炉,停开压缩机,微开塔后放空阀,通过泄压把水汽带出塔外,。但泄压的速度应小于0.2Mpa/min。之后进行封塔。如停车时间长,则应用氮气进行置换。
法兰等泄漏时,若泄漏严重,应停开工加热炉,压缩机循环降温后停下压缩机,合成回路用氮气置换,并用氮气保持微正压,拆口处理,严禁氧气进入。并应随时监测催化剂床层的温度,若发现异常,应及时报告,并加大氮气量降温(应及时和检修人员及时取得联系)。
若情况严重,需将催化剂钝化,再进行处理。
If not the synthesis loop leads to shut down, shut down planning method as reference.
When compressor breakdown, stop the start heating furnace, stop driving compressors, drive tower a little and emptying valve, take water vapor pressure out of the tower by release pressure. But the speed of pressure should be less than 0.2 Mpa/min. After sealing tower. If shut down time is too long, use nitrogen for the displacement.
The leakage such as flange, if leakage is serious, should stop the start heating furnace, compressor cycle stop compressor after cooling, the synthesis loop with nitrogen replacement, and keep the micro positive pressure with nitrogen, make it open, oxygen is forbidden to enter. And observe temperature of the catalyst layer should at any time, if any unnormal, report timely, and increasing nitrogen cooling (shall promptly get in touch with maintenance personnel in a timely manner).
If the case is serious, the catalyst must be passivation, then to handle it.
4.4.11重新开车
4.4.11 production drive again
开压缩机,导入合成气进行循环,使其恢复到期停车前状态,若需要升温,则提高工开工加热出口停车前温度后,再按计划进行还原。
附件:还原时催化剂出水量的计算
熔铁氨合成催化剂(A110-1)理论出水量:
GO==18/55.86×[T%/(1+M)](M+3/2)W              (4-5)
式中   T----总铁百分含量,
M---铁比,Fe+2/Fe+3== Fe+2%/Fe+3%
W---待还原催化剂总重量
当累计出水量为G时,还原度θ=G/G0×100%
Open compressor, lead in cycle syngas, make its restore expire before parking state, if you need to heat up, then improve the outlet starts heating temperature before driving, then continue as planned .
Attachment: calculation of water yield from catalyst when reduction reaction.
Molten iron ammonia synthesis catalyst (A110-1) theoretical aquifer yield:
GO==18/55.86×[T%/(1+M)](M+3/2)W
T - total TieBai points content type,
M - iron content, Fe+2/Fe+3== Fe+2%/Fe+3%
W - total reduction catalyst quantity
When the cumulative water yield is G, reductive degreeθ = G/G0×100%
 
附升温还原计划参考表
Attached to the reduction plan reference table
period Heating stage Early reduction reaction Middle reduction reaction End reduction reaction
The highest temperat layer℃ 1st layer 20~300 300~360 360~440 440~470
2nd layer 20~300 300~360 360~440 440~470
3rd layer 20~300 300~360 360~440 440~470
Heating rate℃/h 1st layer 20~30 10~15 5~10 ~10
2nd layer 20~30 15~20 1~5 5~10
3rd layer 20~30 15~20 1~5 5~10
When enter Into the tower pressure Mpa ≤8 ≤8 8~9 9~10
When out of the tower water vapor concentration of PPM   ≤1000 ≤3000 ≤3000
Airspeed h-1 ≥1500 ≥2500 ≥5000 ≥6000
Into the towerH2 % 75~80 75~80 75~80 75~80