CN114146532B - Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process - Google Patents
Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process Download PDFInfo
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Abstract
Description
技术领域Technical Field
本发明属于多晶硅技术领域，具体涉及一种多晶硅尾气回收工序活性炭吸附塔的运行工艺。The invention belongs to the technical field of polysilicon, and in particular relates to an operating process of an activated carbon adsorption tower in a polysilicon tail gas recovery process.
背景技术Background technique
多晶硅尾气回收工序中回收氢活性炭吸附提纯工艺是：将含有氯硅烷、氯化氢等少量杂质的回收氢，从吸附塔底部输入，利用活性炭吸附剂疏松多孔结构的物理特性对氯硅烷、HCL等杂质进行吸附，以此净化氢气。吸附完成后通过降压、加热、吹扫等方式对吸附塔活性炭进行再生，活性炭微孔中的杂质因压力和温度等变化以及外作用力而脱附，活性炭从而达到循环利用的效果。The activated carbon adsorption purification process for recovered hydrogen in the polysilicon tail gas recovery process is: the recovered hydrogen containing a small amount of impurities such as chlorosilane and hydrogen chloride is input from the bottom of the adsorption tower, and the physical characteristics of the loose porous structure of the activated carbon adsorbent are used to adsorb impurities such as chlorosilane and HCL to purify the hydrogen. After the adsorption is completed, the activated carbon in the adsorption tower is regenerated by reducing pressure, heating, purging, etc. The impurities in the micropores of the activated carbon are desorbed due to changes in pressure and temperature and external forces, so that the activated carbon can be recycled.
在多晶硅行业回收氢吸附工艺中，每一套吸附系统由三座吸附塔组成，在运行过程中，一塔处于吸附过程，一塔处于加热解吸过程，一塔处于冷却过程，三座塔操作循环周期约为5小时。对于单座塔而言，其运行步骤为：吸附、减压加热、加热吹扫、充压冷却、冷却、下一次吸附。但是，在该过程中，存在以下缺点：(1)由于活性炭在周期性的重复吸附和再生的过程，其寿命会随着时间的推移衰减，具体表现为吸附塔会出现加热/冷却延时的现象。这样就无形中增加了吸附工况下的吸附塔的吸附时间。(2)现有工艺方案(控制时序)在吸附后期氢气中磷含量显著上升，严重制约多晶硅产量和品质。(3)若三台吸附塔中有一台吸附塔因故障检修，则剩下的两台吸附塔通常需要降量至少30％后交替运行，才能保证氢气质量不受影响，从而降低了装置产量。In the hydrogen recovery adsorption process in the polysilicon industry, each adsorption system consists of three adsorption towers. During operation, one tower is in the adsorption process, one tower is in the heating and desorption process, and one tower is in the cooling process. The operation cycle of the three towers is about 5 hours. For a single tower, its operation steps are: adsorption, reduced pressure heating, heating and purging, pressurized cooling, cooling, and the next adsorption. However, in this process, there are the following disadvantages: (1) Due to the periodic repeated adsorption and regeneration process of activated carbon, its life will decay over time, which is specifically manifested as the heating/cooling delay of the adsorption tower. This invisibly increases the adsorption time of the adsorption tower under adsorption conditions. (2) The existing process scheme (control sequence) significantly increases the phosphorus content in hydrogen in the later stage of adsorption, which seriously restricts the production and quality of polysilicon. (3) If one of the three adsorption towers is repaired due to a fault, the remaining two adsorption towers usually need to reduce the volume by at least 30% and then operate alternately to ensure that the hydrogen quality is not affected, thereby reducing the output of the device.
有鉴于此，本发明提出一种新的多晶硅尾气回收工序活性炭吸附塔的运行工艺，可有效解决上述问题。In view of this, the present invention proposes a new operating process of an activated carbon adsorption tower in a polysilicon tail gas recovery process, which can effectively solve the above problems.
发明内容Summary of the invention
本发明的目的在于提供一种多晶硅尾气回收工序活性炭吸附塔的运行工艺，通过四塔吸附技术，实现周期性切换，对吸附和再生进行了优化。The object of the present invention is to provide an operating process of an activated carbon adsorption tower in a polysilicon tail gas recovery process, which realizes periodic switching through a four-tower adsorption technology and optimizes adsorption and regeneration.
为了实现上述目的，所采用的技术方案为：In order to achieve the above purpose, the technical solution adopted is:
一种多晶硅尾气回收工序活性炭吸附塔的运行工艺，所述的运行工艺中设置有并联的四座吸附塔，分别为吸附塔1、吸附塔2、吸附塔3和吸附塔4；An operating process of an activated carbon adsorption tower in a polysilicon tail gas recovery process, wherein four adsorption towers connected in parallel are arranged in the operating process, namely, adsorption tower 1, adsorption tower 2, adsorption tower 3 and adsorption tower 4;
在运行过程中，四座吸附塔分别处于吸附、加热、吹扫、冷却的状态。During operation, the four adsorption towers are in the states of adsorption, heating, purging and cooling respectively.
进一步的，所述的运行工艺包括以下步骤：Furthermore, the operation process comprises the following steps:
(1)所述的吸附塔1进行吸附，吸附塔2-4分别处于冷却、加热、充压冷却的状态，在该状态下运行至少1min；(1) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of cooling, heating, and pressurized cooling, and operate in this state for at least 1 minute;
(2)所述的吸附塔1进行吸附，吸附塔2-4分别处于降压加热、加热、充压冷却的状态，在该状态下运行至少3min；(2) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of pressure reduction heating, heating, and pressure charging cooling, and operate in this state for at least 3 minutes;
(3)所述的吸附塔1进行吸附，吸附塔2-4分别处于降压加热、加热、充压冷却的状态，在该状态下运行至少50min；(3) The adsorption tower 1 is performing adsorption, and the adsorption towers 2-4 are respectively in the state of pressure reduction heating, heating, and pressure charging cooling, and operate in this state for at least 50 minutes;
(4)所述的吸附塔1进行吸附，吸附塔2-4分别处于降压加热、加热吹扫、均压冷却的状态，在该状态下运行至少100min；(4) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of pressure reduction heating, heating and purging, and pressure equalization cooling, and operate in this state for at least 100 minutes;
(5)所述的吸附塔1进行吸附，吸附塔2-4分别处于加热吹扫、冷却、均压冷却的状态，在该状态下运行至少10min；(5) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of heating and purging, cooling, and pressure equalization cooling, and operate in this state for at least 10 minutes;
(6)所述的吸附塔1进行吸附，吸附塔2-4分别处于加热吹扫、冷却、均压冷却的状态，在该状态下运行至少70min；(6) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of heating and purging, cooling, and pressure equalization cooling, and operate in this state for at least 70 minutes;
(7)所述的吸附塔1进行吸附，吸附塔2-4分别处于加热、充压冷却、吸附的状态，在该状态下运行至少1min；(7) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of heating, pressurizing, cooling, and adsorption, and operate in this state for at least 1 minute;
(8)所述的吸附塔1进行冷却，吸附塔2-4分别处于加热、充压冷却、吸附的状态，在该状态下运行至少1min；(8) The adsorption tower 1 is cooled, and the adsorption towers 2-4 are respectively in the state of heating, pressurizing cooling, and adsorption, and operate in this state for at least 1 minute;
(9)所述的吸附塔1进行降压加热，吸附塔2-4分别处于加热、充压冷却、吸附的状态，在该状态下运行至少3min；(9) The adsorption tower 1 is depressurized and heated, and the adsorption towers 2-4 are respectively in the state of heating, pressurizing and cooling, and adsorption, and operate in this state for at least 3 minutes;
(10)所述的吸附塔1进行降压加热，吸附塔2-4分别处于加热、充压冷却、吸附的状态，在该状态下运行至少50min；(10) The adsorption tower 1 is depressurized and heated, and the adsorption towers 2-4 are respectively in the state of heating, pressurization cooling, and adsorption, and operate in this state for at least 50 minutes;
(11)所述的吸附塔1进行降压加热，吸附塔2-4分别处于加热吹扫、均压冷却、吸附的状态，在该状态下运行至少100min；(11) The adsorption tower 1 is depressurized and heated, and the adsorption towers 2-4 are respectively in the state of heating and purging, equalizing pressure cooling, and adsorption, and operate in this state for at least 100 minutes;
(12)所述的吸附塔1进行加热吹扫，吸附塔2-4分别处于冷却、均压冷却、吸附的状态，在该状态下运行至少10min；(12) The adsorption tower 1 is heated and purged, and the adsorption towers 2-4 are respectively in the state of cooling, equalizing cooling, and adsorption, and operate in this state for at least 10 minutes;
(13)所述的吸附塔1进行加热吹扫，吸附塔2-4分别处于冷却、均压冷却、吸附的状态，在该状态下运行至少70min；(13) The adsorption tower 1 is heated and purged, and the adsorption towers 2-4 are respectively in the state of cooling, equalizing cooling, and adsorption, and operate in this state for at least 70 minutes;
(14)所述的吸附塔1进行加热，吸附塔2-4分别处于充压冷却、吸附、吸附的状态，在该状态下运行至少1min；(14) The adsorption tower 1 is heated, and the adsorption towers 2-4 are respectively in the state of pressurized cooling, adsorption, and adsorption, and operate in this state for at least 1 minute;
(15)所述的吸附塔1进行加热，吸附塔2-4分别处于充压冷却、吸附、冷却的状态，在该状态下运行至少1min；(15) The adsorption tower 1 is heated, and the adsorption towers 2-4 are respectively in the state of pressurized cooling, adsorption, and cooling, and operate in this state for at least 1 minute;
(16)所述的吸附塔1进行加热，吸附塔2-4分别处于充压冷却、吸附、降压加热的状态，在该状态下运行至少3min；(16) The adsorption tower 1 is heated, and the adsorption towers 2-4 are respectively in the state of pressurized cooling, adsorption, and pressure reduction heating, and operate in this state for at least 3 minutes;
(17)所述的吸附塔1进行加热，吸附塔2-4分别处于充压冷却、吸附、降压加热的状态，在该状态下运行至少50min；(17) The adsorption tower 1 is heated, and the adsorption towers 2-4 are respectively in the state of pressurized cooling, adsorption, and pressure reduction heating, and operate in this state for at least 50 minutes;
(18)所述的吸附塔1进行加热吹扫，吸附塔2-4分别处于均压冷却、吸附、降压加热的状态，在该状态下运行至少100min；(18) The adsorption tower 1 is heated and purged, and the adsorption towers 2-4 are respectively in the state of equalizing pressure cooling, adsorption, and depressurizing heating, and operate in this state for at least 100 minutes;
(19)所述的吸附塔1进行冷却，吸附塔2-4分别处于均压冷却、吸附、加热吹扫的状态，在该状态下运行至少10min；(19) The adsorption tower 1 is cooled, and the adsorption towers 2-4 are respectively in the state of equalizing pressure cooling, adsorption, and heating and purging, and operate in this state for at least 10 minutes;
(20)所述的吸附塔1进行冷却，吸附塔2-4分别处于均压冷却、吸附、加热吹扫的状态，在该状态下运行至少70min；(20) The adsorption tower 1 is cooled, and the adsorption towers 2-4 are respectively in the state of equalizing pressure cooling, adsorption, and heating and purging, and operate in this state for at least 70 minutes;
(21)所述的吸附塔1进行充压冷却，吸附塔2-4分别处于吸附、吸附、加热的状态，在该状态下运行至少1min；(21) The adsorption tower 1 is pressurized and cooled, and the adsorption towers 2-4 are respectively in the adsorption, absorption, and heating states, and operate in this state for at least 1 minute;
(22)所述的吸附塔1进行充压冷却，吸附塔2-4分别处于吸附、冷却、加热的状态，在该状态下运行至少1min；(22) The adsorption tower 1 is pressurized and cooled, and the adsorption towers 2-4 are respectively in the state of adsorption, cooling, and heating, and operate in this state for at least 1 minute;
(23)所述的吸附塔1进行充压冷却，吸附塔2-4分别处于吸附、降压加热、加热的状态，在该状态下运行至少3min；(23) The adsorption tower 1 is pressurized and cooled, and the adsorption towers 2-4 are respectively in the state of adsorption, pressure reduction and heating, and heating, and operate in this state for at least 3 minutes;
(24)所述的吸附塔1进行充压冷却，吸附塔2-4分别处于吸附、降压加热、加热的状态，在该状态下运行至少50min；(24) The adsorption tower 1 is pressurized and cooled, and the adsorption towers 2-4 are respectively in the state of adsorption, pressure reduction and heating, and heating, and operate in this state for at least 50 minutes;
(25)所述的吸附塔1进行均压冷却，吸附塔2-4分别处于吸附、降压加热、加热吹扫的状态，在该状态下运行至少100min；(25) The adsorption tower 1 is subjected to equalized pressure cooling, and the adsorption towers 2-4 are respectively in the state of adsorption, pressure reduction heating, and heating and purging, and operate in this state for at least 100 minutes;
(26)所述的吸附塔1进行均压冷却，吸附塔2-4分别处于吸附、加热吹扫、冷却的状态，在该状态下运行至少10min；(26) The adsorption tower 1 is subjected to equalized pressure cooling, and the adsorption towers 2-4 are respectively in the state of adsorption, heating and purging, and cooling, and operate in this state for at least 10 minutes;
(27)所述的吸附塔1进行均压冷却，吸附塔2-4分别处于吸附、加热吹扫、冷却的状态，在该状态下运行至少70min；(27) The adsorption tower 1 is subjected to equalized pressure cooling, and the adsorption towers 2-4 are respectively in the state of adsorption, heating and purging, and cooling, and operate in this state for at least 70 minutes;
(28)所述的吸附塔1进行吸附，吸附塔2-4分别处于吸附、加热、充压冷却的状态，在该状态下运行至少1min。(28) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of adsorption, heating, and pressurization cooling, and operate in this state for at least 1 minute.
再进一步的，所述的步骤(2)、(9)、(16)、(23)中，水路隔离充压冷却状态下的吸附塔，降压加热状态下的吸附塔热水进冷水出，加热状态下的吸附塔冷水进热水出，至冷热水温度平衡后，将水路切回正常管路，进行下一步骤。Furthermore, in the steps (2), (9), (16) and (23), the water circuit isolates the adsorption tower in the pressurized cooling state, the adsorption tower in the pressure-reduced heating state has hot water in and cold water out, and the adsorption tower in the heating state has cold water in and hot water out. After the temperatures of the cold and hot water are balanced, the water circuit is switched back to the normal pipeline to proceed to the next step.
进一步的，所述的运行工艺中，当其中一座吸附塔出现故障，切至三塔运行模式。Furthermore, in the operation process, when one of the adsorption towers fails, the operation mode is switched to a three-tower operation mode.
与现有技术相比，本发明的有益效果在于：Compared with the prior art, the present invention has the following beneficial effects:
本发明将吸附系统的运行模式由三座一组升级为四座一组，具有以下优点：(1)四塔同时投入运行，确保一座吸附塔处于吸附状态，其它三座塔处于再生的不同阶段。通过优化吸附塔吸附和再生时间，延长活性碳的使用寿命，提高吸附塔处理量。The present invention upgrades the operation mode of the adsorption system from a group of three towers to a group of four towers, which has the following advantages: (1) The four towers are put into operation at the same time, ensuring that one adsorption tower is in an adsorption state and the other three towers are in different stages of regeneration. By optimizing the adsorption and regeneration time of the adsorption tower, the service life of the activated carbon is extended and the processing capacity of the adsorption tower is increased.
(2)降低吸附过程中存留在吸附塔中的杂质总量，同时确保被吸附的杂质能更好地脱附，保证吸附全过程氢气质量稳定，不出现吸附后期杂质含量陡增的情况。(2) Reduce the total amount of impurities remaining in the adsorption tower during the adsorption process, while ensuring that the adsorbed impurities can be better desorbed, ensuring that the hydrogen quality is stable throughout the adsorption process, and preventing a sharp increase in impurity content in the later stage of adsorption.
(3)实现四塔运行和三塔运行的无缝切换，当四座吸附塔中的一座出现故障时，可切至三塔运行模式，保证装置不降量。(3) Realize seamless switching between four-tower operation and three-tower operation. When one of the four adsorption towers fails, it can be switched to the three-tower operation mode to ensure that the device does not reduce its output.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为现有技术三塔运行示意图；Fig. 1 is a schematic diagram of the operation of three towers in the prior art;
图2为三塔吸附运行模式开关阀控制程序；Figure 2 is a three-tower adsorption operation mode switch valve control program;
图3为本发明四塔吸附技术运行示意图；FIG3 is a schematic diagram of the operation of the four-tower adsorption technology of the present invention;
图4为本发明四塔吸附运行模式开关阀控制程序。FIG. 4 is a four-tower adsorption operation mode switch valve control program of the present invention.
具体实施方式Detailed ways
为了进一步阐述本发明一种多晶硅尾气回收工序活性炭吸附塔的运行工艺，达到预期发明目的，以下结合较佳实施例，对依据本发明提出的一种多晶硅尾气回收工序活性炭吸附塔的运行工艺，其具体实施方式、结构、特征及其功效，详细说明如后。在下述说明中，不同的“一实施例”或“实施例”指的不一定是同一实施例。此外，一或多个实施例中的特定特征、结构或特点可由任何合适形式组合。In order to further explain the operation process of an activated carbon adsorption tower in a polysilicon tail gas recovery process of the present invention and achieve the intended purpose of the invention, the following is a detailed description of the operation process of an activated carbon adsorption tower in a polysilicon tail gas recovery process proposed by the present invention, its specific implementation method, structure, characteristics and efficacy in combination with the preferred embodiment. In the following description, different "one embodiment" or "embodiment" does not necessarily refer to the same embodiment. In addition, specific features, structures or characteristics in one or more embodiments may be combined in any suitable form.
在详细阐述本发明一种多晶硅尾气回收工序活性炭吸附塔的运行工艺之前，有必要对本发明中提及的相关背景做进一步说明，以达到更好的效果。Before elaborating in detail the operating process of an activated carbon adsorption tower in a polysilicon tail gas recovery process of the present invention, it is necessary to further explain the relevant background mentioned in the present invention in order to achieve better results.
对于单座塔而言，其运行步骤为：吸附、减压加热、加热吹扫、充压冷却、冷却、下一次吸附。具体流程简述如下：For a single tower, the operation steps are: adsorption, decompression heating, heating and purging, pressurization cooling, cooling, and next adsorption. The specific process is briefly described as follows:
(1)吸附过程：含有氯硅烷、氯化氢等少量杂质的回收氢从吸附塔塔底进入处于吸附工况下的吸附塔内，在活性炭吸附剂的选择吸附下，其中的氯硅烷和氯化氢等组分被吸附下来，未被吸附的氢气(纯度可达到99.9％)从塔顶经过滤器后送入还原工序。当被吸附杂质的传质区前沿(称为吸附前沿)到达床层出口预留段时，关掉该吸附塔的进气阀和氢气出口阀，停止吸附。吸附塔开始转入再生过程。(1) Adsorption process: The recovered hydrogen containing a small amount of impurities such as chlorosilane and hydrogen chloride enters the adsorption tower under adsorption conditions from the bottom of the adsorption tower. Under the selective adsorption of the activated carbon adsorbent, the components such as chlorosilane and hydrogen chloride are adsorbed, and the unadsorbed hydrogen (purity can reach 99.9%) is sent to the reduction process from the top of the tower through the filter. When the front of the mass transfer zone of the adsorbed impurities (called the adsorption front) reaches the reserved section of the bed outlet, the air inlet valve and hydrogen outlet valve of the adsorption tower are turned off to stop the adsorption. The adsorption tower begins to enter the regeneration process.
(2)减压加热过程：在吸附过程结束后，打开吹扫出口阀，关闭冷水进口阀，打开热水进口阀和冷水出口阀，热水赶冷水5分钟完成后，打开热水出口阀，关闭冷水出口阀，通过热水(约176℃)加热吸附塔，使被吸附的气体减压解吸，从吸附塔的底部经压力调节阀调节后平稳地进入再生压缩系统。当吸附塔压力小于0.1MPaG时，吸附塔进入加热吹扫过程。(2) Decompression and heating process: After the adsorption process is completed, open the purge outlet valve, close the cold water inlet valve, open the hot water inlet valve and the cold water outlet valve. After the hot water drives the cold water for 5 minutes, open the hot water outlet valve and close the cold water outlet valve. The adsorption tower is heated by hot water (about 176°C) to decompress the adsorbed gas and desorb it. The gas enters the regeneration compression system smoothly from the bottom of the adsorption tower after being adjusted by the pressure regulating valve. When the pressure of the adsorption tower is less than 0.1MPaG, the adsorption tower enters the heating and purge process.
(3)加热吹扫过程：在减压加热过程结束后，打开吹扫进口阀，用经吸附提纯后的氢气经吸附塔热水间接加热，吹扫吸附剂床层，将吸附在吸附剂上的氯硅烷和氯化氢完全解吸出来，使活性炭吸附剂得到再生。当吸附塔底部温度大于120℃时可认为加热吹扫完成，吸附塔进入回压冷却过程。(3) Heating and purging process: After the decompression and heating process is completed, the purge inlet valve is opened, and the hydrogen gas purified by adsorption is used to indirectly heat the adsorption tower hot water to purge the adsorbent bed, completely desorb the chlorosilane and hydrogen chloride adsorbed on the adsorbent, and regenerate the activated carbon adsorbent. When the temperature at the bottom of the adsorption tower is greater than 120°C, the heating and purging is considered to be completed, and the adsorption tower enters the back pressure cooling process.
(4)回压冷却过程：为了使吸附塔可以平稳地切换至下一次吸附并保证产品纯度在这一过程中不发生波动，需要将吸附塔压力升至吸附压力，以保证产品升压过程的充分和减少对吸附压力波动的影响。当加热吹扫过程完成后，关闭吹扫出口阀和热水进口阀，打开冷水进口阀，当冷水赶热水完成后，关闭热水出口阀，打开冷水出口阀，当吸附塔上下压差小于0.06MPaG时，回压冷却过程完成，吸附塔进入冷却过程。(4) Back pressure cooling process: In order to enable the adsorption tower to smoothly switch to the next adsorption and ensure that the product purity does not fluctuate during this process, the pressure of the adsorption tower needs to be raised to the adsorption pressure to ensure the adequacy of the product pressure-raising process and reduce the impact on the adsorption pressure fluctuation. When the heating and purging process is completed, close the purge outlet valve and the hot water inlet valve, and open the cold water inlet valve. When the cold water drives the hot water, close the hot water outlet valve and open the cold water outlet valve. When the upper and lower pressure difference of the adsorption tower is less than 0.06MPaG, the back pressure cooling process is completed and the adsorption tower enters the cooling process.
(5)冷却过程：利用氢气经吸附塔冷水间接冷却对吸附塔自上而下进行吹冷，当吸附塔内温度小于50℃时冷却过程完成。经这一过程后吸附塔便完成了一个完整的“吸附—再生”循环，又为下一次吸附做好了准备。三座吸附塔交替进行上述的吸附、再生操作(始终有一座吸附塔处于吸附状态)，即可实现氢气中杂质的连续分离与净化。(5) Cooling process: The adsorption tower is cooled from top to bottom by indirect cooling of hydrogen through cold water in the adsorption tower. The cooling process is completed when the temperature in the adsorption tower is less than 50°C. After this process, the adsorption tower has completed a complete "adsorption-regeneration" cycle and is ready for the next adsorption. The three adsorption towers perform the above-mentioned adsorption and regeneration operations alternately (one adsorption tower is always in the adsorption state), which can achieve continuous separation and purification of impurities in hydrogen.
在了解了本发明中提及的相关材料之后，下面将结合具体的实施例，对本发明一种多晶硅尾气回收工序活性炭吸附塔的运行工艺做进一步的详细介绍：After understanding the relevant materials mentioned in the present invention, the operation process of an activated carbon adsorption tower in a polysilicon tail gas recovery process of the present invention will be further described in detail below in combination with specific embodiments:
本发明的技术方案为：The technical solution of the present invention is:
一种多晶硅尾气回收工序活性炭吸附塔的运行工艺，所述的运行工艺中设置有并联的四座吸附塔，分别为吸附塔1、吸附塔2、吸附塔3和吸附塔4；An operating process of an activated carbon adsorption tower in a polysilicon tail gas recovery process, wherein four adsorption towers connected in parallel are arranged in the operating process, namely, adsorption tower 1, adsorption tower 2, adsorption tower 3 and adsorption tower 4;
在运行过程中，四座吸附塔分别处于吸附、加热、吹扫、冷却的状态。During operation, the four adsorption towers are in the states of adsorption, heating, purging and cooling respectively.
优选的，所述的运行工艺包括以下步骤：Preferably, the operation process comprises the following steps:
(1)所述的吸附塔1进行吸附，吸附塔2-4分别处于冷却、加热、充压冷却的状态，在该状态下运行至少1min；(1) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of cooling, heating, and pressurized cooling, and operate in this state for at least 1 minute;
(2)所述的吸附塔1进行吸附，吸附塔2-4分别处于降压加热、加热、充压冷却的状态，在该状态下运行至少3min；(2) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of pressure reduction heating, heating, and pressure charging cooling, and operate in this state for at least 3 minutes;
(3)所述的吸附塔1进行吸附，吸附塔2-4分别处于降压加热、加热、充压冷却的状态，在该状态下运行至少50min；(3) The adsorption tower 1 is performing adsorption, and the adsorption towers 2-4 are respectively in the state of pressure reduction heating, heating, and pressure charging cooling, and operate in this state for at least 50 minutes;
(4)所述的吸附塔1进行吸附，吸附塔2-4分别处于降压加热、加热吹扫、均压冷却的状态，在该状态下运行至少100min；(4) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of pressure reduction heating, heating and purging, and pressure equalization cooling, and operate in this state for at least 100 minutes;
(5)所述的吸附塔1进行吸附，吸附塔2-4分别处于加热吹扫、冷却、均压冷却的状态，在该状态下运行至少10min；(5) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of heating and purging, cooling, and pressure equalization cooling, and operate in this state for at least 10 minutes;
(6)所述的吸附塔1进行吸附，吸附塔2-4分别处于加热吹扫、冷却、均压冷却的状态，在该状态下运行至少70min；(6) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of heating and purging, cooling, and pressure equalization cooling, and operate in this state for at least 70 minutes;
(7)所述的吸附塔1进行吸附，吸附塔2-4分别处于加热、充压冷却、吸附的状态，在该状态下运行至少1min；(7) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of heating, pressurizing, cooling, and adsorption, and operate in this state for at least 1 minute;
(8)所述的吸附塔1进行冷却，吸附塔2-4分别处于加热、充压冷却、吸附的状态，在该状态下运行至少1min；(8) The adsorption tower 1 is cooled, and the adsorption towers 2-4 are respectively in the state of heating, pressurizing cooling, and adsorption, and operate in this state for at least 1 minute;
(9)所述的吸附塔1进行降压加热，吸附塔2-4分别处于加热、充压冷却、吸附的状态，在该状态下运行至少3min；(9) The adsorption tower 1 is depressurized and heated, and the adsorption towers 2-4 are respectively in the state of heating, pressurizing and cooling, and adsorption, and operate in this state for at least 3 minutes;
(10)所述的吸附塔1进行降压加热，吸附塔2-4分别处于加热、充压冷却、吸附的状态，在该状态下运行至少50min；(10) The adsorption tower 1 is depressurized and heated, and the adsorption towers 2-4 are respectively in the state of heating, pressurization cooling, and adsorption, and operate in this state for at least 50 minutes;
(11)所述的吸附塔1进行降压加热，吸附塔2-4分别处于加热吹扫、均压冷却、吸附的状态，在该状态下运行至少100min；(11) The adsorption tower 1 is depressurized and heated, and the adsorption towers 2-4 are respectively in the state of heating and purging, equalizing pressure cooling, and adsorption, and operate in this state for at least 100 minutes;
(12)所述的吸附塔1进行加热吹扫，吸附塔2-4分别处于冷却、均压冷却、吸附的状态，在该状态下运行至少10min；(12) The adsorption tower 1 is heated and purged, and the adsorption towers 2-4 are respectively in the state of cooling, equalizing cooling, and adsorption, and operate in this state for at least 10 minutes;
(13)所述的吸附塔1进行加热吹扫，吸附塔2-4分别处于冷却、均压冷却、吸附的状态，在该状态下运行至少70min；(13) The adsorption tower 1 is heated and purged, and the adsorption towers 2-4 are respectively in the state of cooling, equalizing cooling, and adsorption, and operate in this state for at least 70 minutes;
(14)所述的吸附塔1进行加热，吸附塔2-4分别处于充压冷却、吸附、吸附的状态，在该状态下运行至少1min；(14) The adsorption tower 1 is heated, and the adsorption towers 2-4 are respectively in the state of pressurized cooling, adsorption, and adsorption, and operate in this state for at least 1 minute;
(15)所述的吸附塔1进行加热，吸附塔2-4分别处于充压冷却、吸附、冷却的状态，在该状态下运行至少1min；(15) The adsorption tower 1 is heated, and the adsorption towers 2-4 are respectively in the state of pressurized cooling, adsorption, and cooling, and operate in this state for at least 1 minute;
(16)所述的吸附塔1进行加热，吸附塔2-4分别处于充压冷却、吸附、降压加热的状态，在该状态下运行至少3min；(16) The adsorption tower 1 is heated, and the adsorption towers 2-4 are respectively in the state of pressurized cooling, adsorption, and pressure reduction heating, and operate in this state for at least 3 minutes;
(17)所述的吸附塔1进行加热，吸附塔2-4分别处于充压冷却、吸附、降压加热的状态，在该状态下运行至少50min；(17) The adsorption tower 1 is heated, and the adsorption towers 2-4 are respectively in the state of pressurized cooling, adsorption, and pressure reduction heating, and operate in this state for at least 50 minutes;
(18)所述的吸附塔1进行加热吹扫，吸附塔2-4分别处于均压冷却、吸附、降压加热的状态，在该状态下运行至少100min；(18) The adsorption tower 1 is heated and purged, and the adsorption towers 2-4 are respectively in the state of equalizing pressure cooling, adsorption, and depressurizing heating, and operate in this state for at least 100 minutes;
(19)所述的吸附塔1进行冷却，吸附塔2-4分别处于均压冷却、吸附、加热吹扫的状态，在该状态下运行至少10min；(19) The adsorption tower 1 is cooled, and the adsorption towers 2-4 are respectively in the state of equalizing pressure cooling, adsorption, and heating and purging, and operate in this state for at least 10 minutes;
(20)所述的吸附塔1进行冷却，吸附塔2-4分别处于均压冷却、吸附、加热吹扫的状态，在该状态下运行至少70min；(20) The adsorption tower 1 is cooled, and the adsorption towers 2-4 are respectively in the state of equalizing pressure cooling, adsorption, and heating and purging, and operate in this state for at least 70 minutes;
(21)所述的吸附塔1进行充压冷却，吸附塔2-4分别处于吸附、吸附、加热的状态，在该状态下运行至少1min；(21) The adsorption tower 1 is pressurized and cooled, and the adsorption towers 2-4 are respectively in the adsorption, absorption, and heating states, and operate in this state for at least 1 minute;
(22)所述的吸附塔1进行充压冷却，吸附塔2-4分别处于吸附、冷却、加热的状态，在该状态下运行至少1min；(22) The adsorption tower 1 is pressurized and cooled, and the adsorption towers 2-4 are respectively in the state of adsorption, cooling, and heating, and operate in this state for at least 1 minute;
(23)所述的吸附塔1进行充压冷却，吸附塔2-4分别处于吸附、降压加热、加热的状态，在该状态下运行至少3min；(23) The adsorption tower 1 is pressurized and cooled, and the adsorption towers 2-4 are respectively in the state of adsorption, pressure reduction and heating, and heating, and operate in this state for at least 3 minutes;
(24)所述的吸附塔1进行充压冷却，吸附塔2-4分别处于吸附、降压加热、加热的状态，在该状态下运行至少50min；(24) The adsorption tower 1 is pressurized and cooled, and the adsorption towers 2-4 are respectively in the state of adsorption, pressure reduction and heating, and heating, and operate in this state for at least 50 minutes;
(25)所述的吸附塔1进行均压冷却，吸附塔2-4分别处于吸附、降压加热、加热吹扫的状态，在该状态下运行至少100min；(25) The adsorption tower 1 is subjected to equalized pressure cooling, and the adsorption towers 2-4 are respectively in the state of adsorption, pressure reduction heating, and heating and purging, and operate in this state for at least 100 minutes;
(26)所述的吸附塔1进行均压冷却，吸附塔2-4分别处于吸附、加热吹扫、冷却的状态，在该状态下运行至少10min；(26) The adsorption tower 1 is subjected to equalized pressure cooling, and the adsorption towers 2-4 are respectively in the state of adsorption, heating and purging, and cooling, and operate in this state for at least 10 minutes;
(27)所述的吸附塔1进行均压冷却，吸附塔2-4分别处于吸附、加热吹扫、冷却的状态，在该状态下运行至少70min；(27) The adsorption tower 1 is subjected to equalized pressure cooling, and the adsorption towers 2-4 are respectively in the state of adsorption, heating and purging, and cooling, and operate in this state for at least 70 minutes;
(28)所述的吸附塔1进行吸附，吸附塔2-4分别处于吸附、加热、充压冷却的状态，在该状态下运行至少1min。(28) The adsorption tower 1 is subjected to adsorption, and the adsorption towers 2-4 are respectively in the state of adsorption, heating, and pressurization cooling, and operate in this state for at least 1 minute.
进一步优选的，所述的步骤(2)、(9)、(16)、(23)中，水路隔离充压冷却状态下的吸附塔，降压加热状态下的吸附塔热水进冷水出，加热状态下的吸附塔冷水进热水出，至冷热水温度平衡后，将水路切回正常管路，进行下一步骤。Further preferably, in the steps (2), (9), (16) and (23), the water circuit isolates the adsorption tower in the pressurized cooling state, the adsorption tower in the pressure-reduced heating state has hot water inlet and cold water outlet, and the adsorption tower in the heating state has cold water inlet and hot water outlet. After the temperatures of the cold and hot water are balanced, the water circuit is switched back to the normal pipeline to proceed to the next step.
优选的，所述的运行工艺中，当其中一座吸附塔出现故障，切至三塔运行模式。Preferably, in the operation process, when one of the adsorption towers fails, the operation mode is switched to a three-tower operation mode.
本发明将吸附系统的运行模式由三座一组升级为四座一组，带来的有益效果主要有：(1)四塔同时投入运行，确保一座吸附塔处于吸附状态，其余三座塔处于再生的不同阶段。缩短了单座吸附塔的吸附时间，延长了活性炭的再生时间，确保了活性炭再生效果，使其能有效吸附氢气中杂质，提高氢气品质。(2)实现四塔运行和三塔运行的无缝切换，当四座吸附塔中的一座出现故障时，可切至三塔运行模式，确保吸附系统不降量运行。The present invention upgrades the operation mode of the adsorption system from a group of three towers to a group of four towers, and the main beneficial effects are: (1) The four towers are put into operation at the same time, ensuring that one adsorption tower is in the adsorption state and the other three towers are in different stages of regeneration. The adsorption time of a single adsorption tower is shortened, the regeneration time of activated carbon is prolonged, and the regeneration effect of activated carbon is ensured, so that it can effectively adsorb impurities in hydrogen and improve the quality of hydrogen. (2) A seamless switch between four-tower operation and three-tower operation is achieved. When one of the four adsorption towers fails, it can be switched to the three-tower operation mode to ensure that the adsorption system operates without reducing the capacity.
实施例1.Example 1.
现有技术：回收氢吸附工艺中，吸附系统是靠各个管线上的开关阀的周期性开关来实现各座吸附塔交替进行吸附、减压加热、加热吹扫、充压冷却、冷却、下一次吸附等步骤的(如图1所示)。其中三塔吸附运行模式开关阀控制程序如下表所示(o表示开，c表示关，时间单位分钟)，三塔运行模式分15步，各步骤根据预设好的时间对阀门进行切换，从而实现周期性运行(如图2所示)。Prior art: In the hydrogen recovery adsorption process, the adsorption system relies on the periodic switching of the switch valves on each pipeline to realize the steps of alternate adsorption, decompression heating, heating and purging, pressurization cooling, cooling, and the next adsorption of each adsorption tower (as shown in Figure 1). The switch valve control program of the three-tower adsorption operation mode is shown in the following table (o means open, c means closed, and the time unit is minutes). The three-tower operation mode is divided into 15 steps. Each step switches the valve according to the preset time to achieve periodic operation (as shown in Figure 2).
本发明：四塔吸附技术与三塔吸附不同(如图3所示)。运行工艺中设置有并联的四座吸附塔，分别为吸附塔A、吸附塔B、吸附塔C和吸附塔D，即表1中的T-101A、T-101B、T-101C、T-101D。The present invention: The four-tower adsorption technology is different from the three-tower adsorption (as shown in Figure 3). Four adsorption towers are arranged in parallel in the operation process, namely adsorption tower A, adsorption tower B, adsorption tower C and adsorption tower D, namely T-101A, T-101B, T-101C and T-101D in Table 1.
为了实现周期性切换，其运行模式由15步上升至28步(具体见表1和图4)，同时对吸附和再生时间进行了优化。In order to achieve periodic switching, the operation mode was increased from 15 steps to 28 steps (see Table 1 and Figure 4 for details), and the adsorption and regeneration time were optimized.
表1Table 1
三塔运行模式下，吸附塔吸附时间为323分钟，加热吹扫时间为321分钟；四塔运行模式下，吸附塔吸附时间为236分钟，加热吹扫时间为388分钟。四塔运行模式，吸附时间更短，加热时间更长，这样的调整在降低了活性炭吸附负荷的同时，还延长了吸附塔的再生时间，从而延长了吸附塔的使用寿命，同时还能提高单位时间吸附塔进气量，提高装置产量。In the three-tower operation mode, the adsorption time of the adsorption tower is 323 minutes, and the heating and purging time is 321 minutes; in the four-tower operation mode, the adsorption time of the adsorption tower is 236 minutes, and the heating and purging time is 388 minutes. In the four-tower operation mode, the adsorption time is shorter and the heating time is longer. This adjustment not only reduces the adsorption load of activated carbon, but also prolongs the regeneration time of the adsorption tower, thereby prolonging the service life of the adsorption tower. At the same time, it can also increase the air intake of the adsorption tower per unit time and increase the output of the device.
另外，在四塔运行模式下，一旦有一座吸附塔出现泄漏等故障，可以将故障塔切出系统，将四塔运行模式切换至原来的三塔运行模式，从而保证吸附系统不降量。提高了吸附系统的稳定性。In addition, in the four-tower operation mode, once one of the adsorption towers has a fault such as leakage, the faulty tower can be cut out of the system and the four-tower operation mode can be switched to the original three-tower operation mode, thereby ensuring that the adsorption system does not drop in volume and improving the stability of the adsorption system.
由本发明实施例可知，四塔运行模式运行稳定可靠，因单塔吸附时间变短，再生时间变长，在保证氢气品质不变的前提下，能进一步提升吸附系统的氢气处理量。同时，因能在单塔故障的情况下切换回三塔运行模式，故杜绝了因单塔故障而导致的减产风险，工艺较三塔运行模式有明显的优势和先进性。It can be seen from the embodiments of the present invention that the four-tower operation mode is stable and reliable. Because the single-tower adsorption time is shortened and the regeneration time is prolonged, the hydrogen processing capacity of the adsorption system can be further improved while ensuring the quality of hydrogen. At the same time, because it can switch back to the three-tower operation mode in the event of a single-tower failure, the risk of production reduction caused by a single-tower failure is eliminated, and the process has obvious advantages and advancement compared to the three-tower operation mode.
实施例2.Example 2.
在实施例1本发明四塔运行的28个操作步骤的基础上，进一步细化混水过程。Based on the 28 operation steps of the four-tower operation of the present invention in Example 1, the water mixing process is further refined.
现有技术中其他公司四塔吸附水路切换流程如表2所示：The switching process of the four-tower adsorption water channel of other companies in the prior art is shown in Table 2:
表2Table 2
以第一步B塔切换至A塔吸附为例。切换之前(27、28步)，B塔处于吸附状态，冷水只进不出，维持吸附塔低温状态；C塔处于加热状态，热水进热水出；D塔处于冷却状态，冷水进冷水出；A塔处于冷却状态，冷水进冷水出。原四塔程序中切换至下一步，A塔进入吸附状态，冷水只进不出；B塔进入加热再生状态，将由冷水切换为热水；C塔保持加热状态不变，热水进热水出；D塔保持冷却状态不变，冷水进冷水出。原程序混水步骤中，仅有B塔单塔混水，导致撬块水路系统紊乱，管道和平衡水罐出现剧烈震动。Take the first step of switching from tower B to tower A for adsorption as an example. Before the switch (steps 27 and 28), tower B is in the adsorption state, with cold water only entering but not exiting, maintaining the low temperature state of the adsorption tower; tower C is in the heating state, with hot water entering and hot water exiting; tower D is in the cooling state, with cold water entering and cold water exiting; tower A is in the cooling state, with cold water entering and cold water exiting. In the original four-tower program, switch to the next step, tower A enters the adsorption state, with cold water only entering and not exiting; tower B enters the heating regeneration state, switching from cold water to hot water; tower C maintains the heating state unchanged, with hot water entering and hot water exiting; tower D maintains the cooling state unchanged, with cold water entering and cold water exiting. In the water mixing step of the original program, only tower B mixes water, causing the skid water system to be disordered, and the pipes and the balancing water tank to vibrate violently.
即在现有的四塔程序的混水过程中存在着水击现象。本发明为了解决该技术问题，通过隔离出冷却状态的塔，吸附转加热的塔和原加热状态的塔交互混水。改动如表3所示，为关闭D塔冷水出口，冷水只进不出，从而隔离D塔；原加热状态的C塔改为冷水进热水出，参与B塔混水。当冷热水温度相等后，再将B塔切为加热状态、C塔切回加热状态，D塔开冷水出口，切回冷却状态。That is, water hammer occurs in the water mixing process of the existing four-tower program. In order to solve this technical problem, the present invention isolates the tower in the cooling state, and the tower that is adsorbed and heated is mixed with the tower in the original heating state. The changes are shown in Table 3. The cold water outlet of Tower D is closed, and cold water only enters but not exits, thereby isolating Tower D; Tower C in the original heating state is changed to cold water in and hot water out, and participates in the water mixing of Tower B. When the temperatures of cold and hot water are equal, Tower B is switched to the heating state, Tower C is switched back to the heating state, and Tower D opens the cold water outlet and switches back to the cooling state.
表3table 3
以下为具体控制步骤说明：The following are the specific control steps:
(1)程序第1-3步，由B塔吸附切换为A塔吸附。(1) Steps 1-3 of the procedure switch from adsorption in tower B to adsorption in tower A.
将各塔状态切换至以下状态(程序第2步)：Switch the tower status to the following status (procedure step 2):
A塔：吸附B塔：热水进冷水出C塔：冷水进热水出D塔：水路隔离(热水进出关，冷水出口关)Tower A: Adsorption Tower B: Hot water in, cold water out Tower C: Cold water in, hot water out Tower D: Waterway isolation (hot water in and out closed, cold water outlet closed)
即以下开关阀同时动作：That is, the following switch valves act simultaneously:
冷热水温度平衡后(约105℃)，将水路切回正常管路(程序第3步)：After the hot and cold water temperatures are balanced (about 105°C), switch the water line back to the normal line (Step 3 of the procedure):
即以下开关阀同时动作：That is, the following switch valves act simultaneously:
(2)程序第8-10步，由A塔吸附切换为D塔吸附。(2) In steps 8-10 of the procedure, the adsorption in tower A is switched to that in tower D.
将各塔状态切换至以下状态(程序第9步)：Switch the tower status to the following status (step 9 of the program):
A塔：热水进冷水出 B塔：冷水进热水出 C塔：水路隔离(热水进出关，冷水出口关)D塔：吸附Tower A: hot water in, cold water out Tower B: cold water in, hot water out Tower C: water isolation (hot water in and out closed, cold water outlet closed) Tower D: adsorption
即以下开关阀同时动作：That is, the following switch valves act simultaneously:
冷热水温度平衡后(约105℃)，将水路切回正常管路(程序第10步)：After the hot and cold water temperatures are balanced (about 105°C), switch the water line back to the normal line (step 10 of the procedure):
即以下开关阀同时动作：That is, the following switch valves act simultaneously:
(3)程序第15-17步，由D塔吸附切换为C塔吸附。(3) In steps 15-17 of the procedure, the adsorption in tower D is switched to that in tower C.
将各塔状态切换至以下状态(程序第16步)：Switch the tower status to the following status (step 16 of the program):
A塔：冷水进热水出 B塔：水路隔离(热水进出关，冷水出口关)C塔：吸附 D塔：热水进冷水出Tower A: cold water in, hot water out Tower B: water isolation (hot water in and out closed, cold water outlet closed) Tower C: adsorption Tower D: hot water in, cold water out
即以下开关阀同时动作：That is, the following switch valves act simultaneously:
冷热水温度平衡后(约105℃)，将水路切回正常管路(程序第17步)：After the hot and cold water temperatures are balanced (about 105°C), switch the water line back to the normal line (step 17 of the procedure):
即以下开关阀同时动作：That is, the following switch valves act simultaneously:
(4)程序第22-24步，由C塔吸附切换为B塔吸附。(4) In steps 22-24 of the procedure, the adsorption in tower C is switched to that in tower B.
将各塔状态切换至以下状态(程序第23步)：Switch the status of each tower to the following status (step 23 of the program):
A塔：水路隔离(热水进出关，冷水出口关) B塔：吸附 C塔：热水进冷水出 D塔：冷水进热水出Tower A: Water isolation (hot water inlet and outlet closed, cold water outlet closed) Tower B: Adsorption Tower C: Hot water in, cold water out Tower D: Cold water in, hot water out
即以下开关阀同时动作：That is, the following switch valves act simultaneously:
冷热水温度平衡后(约105℃)，将水路切回正常管路(程序第24步)：After the hot and cold water temperatures are balanced (about 105°C), switch the water line back to the normal line (step 24 of the procedure):
即以下开关阀同时动作：That is, the following switch valves act simultaneously:
本发明通过该水路切换方法(即第2、9、16、23步的开关阀动作步骤)可以防止吸附塔四塔运行工艺中为水击现象的产生。The present invention can prevent the occurrence of water hammer in the operation process of the four adsorption towers through the water circuit switching method (i.e. the switch valve action steps of steps 2, 9, 16 and 23).
以上所述，仅是本发明实施例的较佳实施例而已，并非对本发明实施例作任何形式上的限制，依据本发明实施例的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明实施例技术方案的范围内。The above is only a preferred embodiment of the embodiment of the present invention, and does not impose any form of limitation on the embodiment of the present invention. Any simple modification, equivalent changes and modifications made to the above embodiment based on the technical essence of the embodiment of the present invention are still within the scope of the technical solution of the embodiment of the present invention.
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