CN110255500A - A kind of recycle hydrogen deamination purification system and method - Google Patents
A kind of recycle hydrogen deamination purification system and method Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 140
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 140
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 238000000746 purification Methods 0.000 title claims abstract description 125
- 230000009615 deamination Effects 0.000 title claims abstract description 32
- 238000006481 deamination reaction Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 85
- 230000008929 regeneration Effects 0.000 claims abstract description 74
- 238000011069 regeneration method Methods 0.000 claims abstract description 74
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000002994 raw material Substances 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 239000003463 adsorbent Substances 0.000 claims abstract description 39
- 230000006837 decompression Effects 0.000 claims abstract description 37
- 238000000926 separation method Methods 0.000 claims abstract description 34
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 30
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 13
- 230000000694 effects Effects 0.000 claims abstract description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002808 molecular sieve Substances 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 4
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 4
- 230000007420 reactivation Effects 0.000 claims 2
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000002699 waste material Substances 0.000 abstract description 10
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 239000010842 industrial wastewater Substances 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 description 13
- 238000011049 filling Methods 0.000 description 10
- 239000003921 oil Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000295 fuel oil Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000003348 petrochemical agent Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/042—Purification by adsorption on solids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
本发明提供了一种循环氢脱氨提纯系统，包括：减压装置；入口与所述减压装置的出口相连的原料冷却器；入口与所述原料冷却器的出口相连的气液分离装置；入口与所述气液分离装置的出口相连的若干个并联的脱氨净化塔，所述脱氨净化塔顶部设置有氢气出口以及再生气体入口；与所述再生气体入口依次相连的再生气体加热器以及再生气体减压装置。本发明提供的装置主要利用变温吸附方法，采用低温低压下，利用吸附剂的吸附作用除去原料气中的氨，并回收利用，采用干燥还原的模式对吸附进行脱附，循环使用吸附剂，降低生产成本。该装置脱氨率高，不会造成氢气的浪费，并且不会产生大量的工业废水。
The invention provides a circulating hydrogen deammonization purification system, comprising: a decompression device; a raw material cooler whose inlet is connected to the outlet of the decompression device; a gas-liquid separation device whose inlet is connected to the outlet of the raw material cooler; Several parallel deamination purification towers whose inlet is connected to the outlet of the gas-liquid separation device, the top of the deammonization purification tower is provided with a hydrogen outlet and a regeneration gas inlet; a regeneration gas heater connected in sequence with the regeneration gas inlet And regeneration gas decompression device. The device provided by the present invention mainly utilizes the temperature swing adsorption method, adopts the adsorption effect of the adsorbent to remove the ammonia in the raw material gas under low temperature and low pressure, and recycles it. Cost of production. The device has a high ammonia removal rate, does not cause waste of hydrogen, and does not generate a large amount of industrial waste water.
Description
技术领域technical field
本发明属于石油化工技术领域，具体涉及一种循环氢脱氨提纯系统及方法。The invention belongs to the technical field of petrochemical industry, and in particular relates to a circulating hydrogen deammonization purification system and method.
背景技术Background technique
氢气是现代炼油工业和化学工业的基本原料之一，其应用领域广泛，其中最大的是石油化工原料，用于合成氨、甲醇以及石油炼制过程的加氢反应，此外，在电子工业，冶金工业、食品加工、精细有机合成、航空航天工业等领域都有广范应用。大部分是由天然气、石脑油或重油的蒸汽转化法制取。Hydrogen is one of the basic raw materials in the modern oil refining industry and chemical industry. It has a wide range of applications, the largest of which is petrochemical raw materials, which are used for hydrogenation reactions in the synthesis of ammonia, methanol and petroleum refining processes. In addition, in the electronics industry, metallurgical industry , food processing, fine organic synthesis, aerospace industry and other fields have a wide range of applications. Most of them are produced by steam reforming of natural gas, naphtha or heavy oil.
在现在石油化工加工过程中，氢气主要用于石脑油加氢脱硫、柴油加氢脱硫、燃料油加氢脱硫、改善飞机燃料的无火焰高度和加氢裂化等方面。加氢精制过程中，利用氢气的饱和功能，可以改善石油化学品的质量，增加最有价值的石油化学品的产量，减少重油残渣和焦油的生成，提高石油加工厂的适应性，从石油加工废物中可以得到有价值的石油化学产品，净化产品除去有害杂质，所以氢气又是现代石油化工工业产品最通用的净化剂，将不稳定的化合物转化为稳定的产物。所以在石油化工加氢过程中，反应系统对氢气的纯度要求很高，一般都要求补充氢气的纯度高于99％以上，循环氢中的氢纯度要求都高于90％。In the current petrochemical processing process, hydrogen is mainly used in hydrodesulfurization of naphtha, hydrodesulfurization of diesel oil, hydrodesulfurization of fuel oil, improvement of flame-free height of aircraft fuel and hydrocracking. In the process of hydrofining, the saturation function of hydrogen can be used to improve the quality of petrochemicals, increase the output of the most valuable petrochemicals, reduce the generation of heavy oil residue and tar, and improve the adaptability of petroleum processing plants. Valuable petrochemical products can be obtained from waste, and the purified products remove harmful impurities. Therefore, hydrogen is the most common purifying agent for modern petrochemical industrial products, converting unstable compounds into stable products. Therefore, in the petrochemical hydrogenation process, the reaction system has high requirements on the purity of hydrogen. Generally, the purity of supplementary hydrogen is required to be higher than 99%, and the purity of hydrogen in circulating hydrogen is required to be higher than 90%.
随着世界范围内石油资源的日益减少及对清洁燃料需求的不断提升，在加氢装置运行过程中，需要将原料中氮及化合物除去提高产品质量，反应后形成的氨随装置循环氢气循环使用，造成循环氢气中氨含超标是普遍现象，生产装置大部分采用注水或排放废氢的方式满足工艺条件，但是上述方式会产生大量的工业废水或者造成氢气的浪费。With the decrease of petroleum resources worldwide and the continuous improvement of the demand for clean fuels, during the operation of the hydrogenation unit, it is necessary to remove nitrogen and compounds in the raw material to improve product quality, and the ammonia formed after the reaction is recycled with the hydrogen in the unit. , It is a common phenomenon that the ammonia content in the circulating hydrogen exceeds the standard. Most of the production equipment adopts the method of water injection or waste hydrogen discharge to meet the process conditions, but the above methods will generate a large amount of industrial wastewater or cause waste of hydrogen.
发明内容Contents of the invention
有鉴于此，本发明要解决的技术问题在于提供一种循环氢脱氨提纯系统及方法，本发明提供的循环氢脱氨提纯系统采用低温低压的操作条件安全可靠，脱氨率高，可实现吸附剂的重复使用，不会造成氢气的浪费，并且不会产生大量的工业废水。In view of this, the technical problem to be solved by the present invention is to provide a circulating hydrogen deammonization purification system and method. The circulating hydrogen deammonization purification system provided by the present invention adopts safe and reliable operating conditions at low temperature and low pressure, and has a high deammonization rate, which can realize The repeated use of the adsorbent will not cause waste of hydrogen, and will not produce a large amount of industrial waste water.
本发明提供了一种循环氢脱氨提纯系统，包括：The invention provides a circulating hydrogen deammonization purification system, comprising:
原料减压装置；Raw material decompression device;
入口与所述减压装置的出口相连的原料冷却器；a raw material cooler whose inlet is connected to the outlet of the pressure reducing device;
入口与所述原料冷却器的出口相连的气液分离装置；A gas-liquid separation device whose inlet is connected to the outlet of the raw material cooler;
入口与所述气液分离装置的出口相连的若干个并联的脱氨净化塔，所述脱氨净化塔顶部设置有氢气出口以及再生气体入口；Several parallel deamination purification towers whose inlet is connected to the outlet of the gas-liquid separation device, the top of the deamination purification tower is provided with a hydrogen outlet and a regeneration gas inlet;
与所述再生气体入口依次相连的再生气体加热器以及再生气体减压装置。A regeneration gas heater and a regeneration gas decompression device sequentially connected to the regeneration gas inlet.
优选的，所述脱氨净化塔的个数为两个或以上。Preferably, the number of the deammonization purification towers is two or more.
优选的，所述脱氨净化塔内装填有吸附剂，所述吸附剂选自活性炭、氧化锌、5A分子筛。Preferably, the deammonization purification tower is filled with an adsorbent, and the adsorbent is selected from activated carbon, zinc oxide, and 5A molecular sieve.
本发明还提供了一种循环氢脱氨提纯的方法，包括以下步骤：The present invention also provides a method for circulating hydrogen deammonification purification, comprising the following steps:
采用上述循环氢脱氨提纯系统，将循环氢依次经过原料减压装置减压和原料冷却器冷却后，得到减压冷却后的循环氢；Using the above-mentioned circulating hydrogen deammonization purification system, after the circulating hydrogen is decompressed by the raw material decompression device and cooled by the raw material cooler, the circulating hydrogen after decompression and cooling is obtained;
所述减压冷却后的循环氢经过气液分离装置去除液体后，进入脱氨净化塔进行循环氢的脱氨提纯，得到脱氨提纯后的氢气；After the decompressed and cooled circulating hydrogen passes through the gas-liquid separation device to remove the liquid, it enters the deammonization purification tower for the deammonization and purification of the circulating hydrogen to obtain hydrogen after deammonization and purification;
当脱氨净化塔中的吸附剂活性降低后，将经过再生气体减压装置减压和再生气体加热器加热的再生气体通入脱氨净化塔进行吸附剂再生。When the activity of the adsorbent in the deammonization purification tower decreases, the regeneration gas decompressed by the regeneration gas decompression device and heated by the regeneration gas heater is passed into the deammonization purification tower to regenerate the adsorbent.
优选的，所述若干个脱氨净化塔中的部分净化塔进行脱氨提纯时，剩余部分的脱氨净化塔进行吸附剂再生。Preferably, when some of the purification towers among the several deammonization purification towers perform deammonization and purification, the remaining part of the deammonization purification towers perform adsorbent regeneration.
优选的，所述减压冷却后的循环氢的压力为2.0～2.2MPa，温度为40～50℃。Preferably, the pressure of the circulating hydrogen after decompression cooling is 2.0-2.2 MPa, and the temperature is 40-50°C.
优选的，所述减压加热后的再生气体的温度为150～160℃，压力为0.2～0.5MPa。Preferably, the temperature of the regeneration gas after depressurization and heating is 150-160° C., and the pressure is 0.2-0.5 MPa.
优选的，所述循环氢中氨气的含量≤20mg/m3，所述循环氢中硫化氢的含量≤1mg/m3。Preferably, the content of ammonia in the circulating hydrogen is ≤20 mg/m 3 , and the content of hydrogen sulfide in the circulating hydrogen is ≤1 mg/m 3 .
优选的，所述脱氨提纯后的氢气纯度大于98％，所述脱氨提纯后的氢气中氨气含量＜0.5ppm。Preferably, the hydrogen purity after deammonization and purification is greater than 98%, and the ammonia content in the deammonization and purification hydrogen is less than 0.5ppm.
与现有技术相比，本发明提供了一种循环氢脱氨提纯系统，包括：减压装置；入口与所述减压装置的出口相连的原料冷却器；入口与所述原料冷却器的出口相连的气液分离装置；入口与所述气液分离装置的出口相连的若干个并联的脱氨净化塔，所述脱氨净化塔顶部设置有氢气出口以及再生气体入口；与所述再生气体入口依次相连的再生气体加热器以及再生气体减压装置。本发明提供的装置主要利用变温吸附方法，采用低温低压下，利用吸附剂的吸附作用除去原料气中的氨，并回收利用，采用干燥还原的模式对吸附进行脱附，循环使用吸附剂，降低生产成本。该装置脱氨率高，不会造成氢气的浪费，并且不会产生大量的工业废水。Compared with the prior art, the present invention provides a circulating hydrogen deammonization purification system, comprising: a decompression device; a raw material cooler whose inlet is connected to an outlet of the decompression device; an inlet and an outlet of the raw material cooler A connected gas-liquid separation device; several parallel deamination purification towers whose inlet is connected to the outlet of the gas-liquid separation device, and the top of the deamination purification tower is provided with a hydrogen outlet and a regeneration gas inlet; Sequentially connected regeneration gas heaters and regeneration gas decompression devices. The device provided by the present invention mainly utilizes the temperature swing adsorption method, adopts the adsorption effect of the adsorbent to remove the ammonia in the raw material gas under low temperature and low pressure, and recycles it. Cost of production. The device has a high ammonia removal rate, does not cause waste of hydrogen, and does not generate a large amount of industrial waste water.
结果表明，所述脱氨提纯后的氢气纯度大于98％，所述脱氨提纯后的氢气中氨气含量＜0.5ppm。The results show that the hydrogen purity after deammonization and purification is greater than 98%, and the ammonia content in the deammonization and purification hydrogen is less than 0.5ppm.
附图说明Description of drawings
图1为本发明提供的循环氢脱氨提纯系统的结构示意图。Fig. 1 is a structural schematic diagram of the circulating hydrogen deammonization purification system provided by the present invention.
具体实施方式Detailed ways
本发明提供了一种循环氢脱氨提纯系统，包括：The invention provides a circulating hydrogen deammonization purification system, comprising:
原料减压装置；Raw material decompression device;
入口与所述减压装置的出口相连的原料冷却器；a raw material cooler whose inlet is connected to the outlet of the pressure reducing device;
入口与所述原料冷却器的出口相连的气液分离装置；A gas-liquid separation device whose inlet is connected to the outlet of the raw material cooler;
入口与所述气液分离装置的出口相连的若干个并联的脱氨净化塔，所述脱氨净化塔顶部设置有氢气出口以及再生气体入口；Several parallel deamination purification towers whose inlet is connected to the outlet of the gas-liquid separation device, the top of the deamination purification tower is provided with a hydrogen outlet and a regeneration gas inlet;
与所述再生气体入口依次相连的再生气体加热器以及再生气体减压装置。A regeneration gas heater and a regeneration gas decompression device sequentially connected to the regeneration gas inlet.
本发明提供的循环氢脱氨提纯系统包括原料减压装置，所述原料减压装置主要用于对原料循环氢进行减压，使循环氢以低压状态进入系统。The circulating hydrogen deammonization purification system provided by the present invention includes a raw material decompression device, and the raw material decompression device is mainly used to decompress the raw material circulating hydrogen so that the circulating hydrogen enters the system at a low pressure.
本发明提供的循环氢脱氨提纯系统还包括入口与所述减压装置的出口相连的原料冷却器。由于自生产装置来的原料循环氢温度较高，通过原料冷却器将循环氢进行降温，在本发明中，优选采用循环冷却水对原料循环氢进行降温冷却。The circulating hydrogen deammonization purification system provided by the present invention also includes a raw material cooler whose inlet is connected to the outlet of the decompression device. Since the temperature of the raw material circulating hydrogen from the production device is relatively high, the temperature of the circulating hydrogen is lowered through the raw material cooler. In the present invention, circulating cooling water is preferably used to cool down the temperature of the raw material circulating hydrogen.
本发明提供的循环氢脱氨提纯系统还包括入口与所述原料冷却器的出口相连的气液分离装置，循环氢经过气液分离装置，分离去除气体中夹带的油和水滴。所述气液分离装置底部设置有液体出口，所述液体出口与污油管道相连。The circulating hydrogen deammonization purification system provided by the present invention also includes a gas-liquid separation device whose inlet is connected to the outlet of the raw material cooler, and the circulating hydrogen passes through the gas-liquid separation device to separate and remove oil and water droplets entrained in the gas. A liquid outlet is provided at the bottom of the gas-liquid separation device, and the liquid outlet is connected to a dirty oil pipeline.
本发明提供的循环氢脱氨提纯系统还包括入口与所述气液分离装置的出口相连的若干个并联的脱氨净化塔。在本发明中，所述脱氨净化塔的个数为两个或以上。所述脱氨净化塔的根据生产能力和生产要求进行适量的增减。所述若干个脱氨净化塔中的部分净化塔进行脱氨提纯时，剩余部分的脱氨净化塔进行吸附剂再生。在本发明的一些具体实施方式中，所述脱氨净化塔的个数为两个。两个脱氨净化塔交替工作进行氢气的脱氨提纯，即当其中一台脱氨净化塔进行氢气脱氨提纯时，另一台脱氨净化塔进行吸附剂的再生。The circulating hydrogen deammonization purification system provided by the present invention also includes several parallel deammonization purification towers whose inlets are connected to the outlets of the gas-liquid separation device. In the present invention, the number of the deammonization purification towers is two or more. The deammonization purification tower is appropriately increased or decreased according to production capacity and production requirements. When some of the purification towers in the several deammonization purification towers are deammonized and purified, the remaining part of the deammonization purification towers are used for adsorbent regeneration. In some specific embodiments of the present invention, the number of the deammonization purification towers is two. The two deammonization purification towers work alternately for deammonization and purification of hydrogen, that is, when one of the deammonization purification towers performs hydrogen deammonization and purification, the other deammonization purification tower regenerates the adsorbent.
所述脱氨净化塔顶部设置有氢气出口以及再生气体入口，底部设置有氢气入口以及杂质气体出口。在本发明的一些具体实施方式中，为了减少设备主体的开口数量，所述氢气出口以及再生气体入口可以为同一个开口，并通过连接管路进行分支以及在管路上设置阀门进行气体流向的控制；氢气入口以及杂质气体出口可以为同一个开口，并通过连接管路进行分支以及在管路上设置阀门进行气体流向的控制。The top of the deammonization purification tower is provided with a hydrogen outlet and a regeneration gas inlet, and the bottom is provided with a hydrogen inlet and an impurity gas outlet. In some specific embodiments of the present invention, in order to reduce the number of openings in the main body of the equipment, the hydrogen outlet and the regeneration gas inlet can be the same opening, and branched by connecting pipelines and valves are set on the pipelines to control the direction of gas flow ; The hydrogen inlet and the impurity gas outlet can be the same opening, and branched by connecting pipelines and setting valves on the pipelines to control the gas flow direction.
在本发明中，所述气液分离装置和脱氨净化塔内均装填有吸附剂，所述吸附剂选自活性炭、氧化锌、5A分子筛。In the present invention, both the gas-liquid separation device and the deammonization purification tower are filled with an adsorbent, and the adsorbent is selected from activated carbon, zinc oxide, and 5A molecular sieve.
本发明对所述装填方式并没有特殊限制，本领域技术人员公知的装填方式即可，优选为疏相装填或布袋装填。其中，所述气液分离装置和脱氨净化塔内的吸附剂种类参见表1，表1为吸附剂种类和装填部位。The present invention has no special limitation on the filling method, and any filling method known to those skilled in the art is sufficient, preferably sparse phase filling or cloth bag filling. Wherein, the types of adsorbents in the gas-liquid separation device and the deammonization purification tower are shown in Table 1, and Table 1 shows the types of adsorbents and the filling positions.
表1Table 1
其中，吸附剂-3和吸附剂-4主要装填于原料气液分离罐，装填顺序按照进料方向依次为吸附剂-3、吸附剂-4和吸附剂-3；Among them, Adsorbent-3 and Adsorbent-4 are mainly loaded in the raw material gas-liquid separation tank, and the filling sequence is Adsorbent-3, Adsorbent-4 and Adsorbent-3 according to the feeding direction;
吸附剂-1、吸附剂-2、吸附剂-5装填于脱氨净化塔。装填顺序按照进料方向为吸附剂-1、吸附剂-5、吸附剂-2和吸附剂-1。Adsorbent-1, Adsorbent-2, and Adsorbent-5 are loaded in the deammonization purification tower. The loading sequence according to the feeding direction is adsorbent-1, adsorbent-5, adsorbent-2 and adsorbent-1.
本发明提供的循环氢脱氨提纯系统还包括与所述再生气体入口依次相连的再生气体加热器以及再生气体减压装置。即再生气体通过减压装置的减压后，在经过再生气体加热器的加热通过再生气体入口进入脱氨净化塔。The circulation hydrogen deammonization purification system provided by the present invention also includes a regeneration gas heater and a regeneration gas decompression device sequentially connected to the regeneration gas inlet. That is, after the regeneration gas is decompressed by the decompression device, it enters the deammonization purification tower through the regeneration gas inlet after being heated by the regeneration gas heater.
其中，所述再生气体优选为氮气，所述再生气体加热器的热源优选来自于管网的蒸汽。Wherein, the regeneration gas is preferably nitrogen, and the heat source of the regeneration gas heater is preferably steam from a pipe network.
本发明还提供了一种循环氢脱氨提纯的方法，包括以下步骤：The present invention also provides a method for circulating hydrogen deammonification purification, comprising the following steps:
采用上述循环氢脱氨提纯系统，将循环氢依次经过原料减压装置减压和原料冷却器冷却后，得到减压冷却后的循环氢；Using the above-mentioned circulating hydrogen deammonization purification system, after the circulating hydrogen is decompressed by the raw material decompression device and cooled by the raw material cooler, the circulating hydrogen after decompression and cooling is obtained;
所述减压冷却后的循环氢经过气液分离装置去除液体后，进入脱氨净化塔进行循环氢的脱氨提纯，得到脱氨提纯后的氢气；After the decompressed and cooled circulating hydrogen passes through the gas-liquid separation device to remove the liquid, it enters the deammonization purification tower for the deammonization and purification of the circulating hydrogen to obtain hydrogen after deammonization and purification;
当脱氨净化塔中的吸附剂活性降低后，将经过再生气体减压装置减压和再生气体加热器加热的减压加热后的再生气体通入脱氨净化塔进行吸附剂再生。When the activity of the adsorbent in the deammonization purification tower decreases, the decompressed and heated regeneration gas decompressed by the regeneration gas decompression device and heated by the regeneration gas heater is passed into the deammonization purification tower to perform regeneration of the adsorbent.
具体的，首先，来自生产装置的原料循环氢经过原料减压装置进行减压，得到减压后的循环氢。Specifically, firstly, the raw material circulating hydrogen from the production device is decompressed through the raw material decompression device to obtain the decompressed circulating hydrogen.
其中，所述来自生产装置的原料循环氢中氨气的含量≤20mg/m3，所述循环氢中硫化氢的含量≤1mg/m3。Wherein, the content of ammonia in the circulating hydrogen from the production device is ≤20 mg/m 3 , and the content of hydrogen sulfide in the circulating hydrogen is ≤1 mg/m 3 .
接着，减压后的循环氢经过原料冷却器冷却，得到减压冷却后的循环氢。Next, the decompressed circulating hydrogen is cooled by a raw material cooler to obtain decompressed and cooled circulating hydrogen.
所述减压冷却后的循环氢的压力为2.0～2.2MPa，温度为40～50℃。The pressure of the circulating hydrogen after decompression cooling is 2.0-2.2 MPa, and the temperature is 40-50°C.
然后，所述减压冷却后的循环氢经过气液分离装置去除液体，所述液体主要是循环氢气体中夹带的油和水滴。所述液体自所述气液分离装置底部设置的液体出口流出，通过与所述液体出口相连的污油管道排出系统。Then, the decompressed and cooled circulating hydrogen passes through a gas-liquid separation device to remove liquid, and the liquid is mainly oil and water droplets entrained in the circulating hydrogen gas. The liquid flows out from a liquid outlet provided at the bottom of the gas-liquid separation device, and is discharged from the system through a dirty oil pipeline connected to the liquid outlet.
经过气液分离的循环氢进入脱氨净化塔进行循环氢的脱氨提纯，得到脱氨提纯后的氢气。The circulating hydrogen after gas-liquid separation enters the deammonization purification tower for deammonization and purification of the circulating hydrogen to obtain hydrogen after deammonization and purification.
在本发明中，所述若干个脱氨净化塔中的部分净化塔进行脱氨提纯时，剩余部分的脱氨净化塔进行吸附剂再生，以保证整个脱氨系统处于持续脱氨状态，提高脱氨效率。In the present invention, when some of the purification towers in the several deammonization purification towers are deammonized and purified, the remaining part of the deammonization purification towers are subjected to adsorbent regeneration, so as to ensure that the whole deammonization system is in a continuous deammonization state and improve the ammonia efficiency.
其中，进行脱氨提纯的脱氨净化塔的塔底氢气入口开启，杂质气体出口关闭，而塔顶的氢气出口开启，再生气体入口关闭，循环氢由进行脱氨提纯的脱氨净化塔的塔底进入通过吸附剂的脱氨提纯后再由塔顶的氢气出口送至氢气管网，用于石油化工的加氢脱硫；而进行吸附剂再生的脱氨净化塔的塔底氢气入口关闭，杂质气体出口开启，而塔顶的氢气出口关闭，再生气体入口开启，再生气体由进行吸附剂再生的脱氨净化塔的塔顶再生气体入口进入脱氨净化塔对吸附剂进行再生，然后将吸附在吸附剂表面的氨以及重烃等杂质随再生气体一起从塔底的杂质气体出口排出，经过压力调节排至火炬管网。Among them, the hydrogen inlet at the bottom of the deammonization purification tower for deammonization purification is opened, the impurity gas outlet is closed, and the hydrogen outlet at the top of the tower is opened, the regeneration gas inlet is closed, and the circulating hydrogen is released from the tower of the deammonization purification tower for deammonization purification. The bottom enters through the deamination and purification of the adsorbent, and then is sent to the hydrogen pipeline network from the hydrogen outlet at the top of the tower, which is used for hydrodesulfurization in petrochemical industry; while the hydrogen inlet at the bottom of the deammonization purification tower for adsorbent regeneration is closed, impurities The gas outlet is opened, the hydrogen outlet at the top of the tower is closed, and the regeneration gas inlet is opened. The regeneration gas enters the deammonization purification tower from the regeneration gas inlet at the top of the deammonization purification tower for adsorbent regeneration to regenerate the adsorbent. Impurities such as ammonia and heavy hydrocarbons on the surface of the adsorbent are discharged from the impurity gas outlet at the bottom of the tower together with the regeneration gas, and are discharged to the flare pipe network after pressure regulation.
当进行脱氨提纯的脱氨净化塔中的吸附剂的吸附性能下降，无法进行脱氨提纯或者脱氨提纯效率低时，可以关闭脱氨净化塔顶部的氢气入口以及底部的氢气出口，打开顶部的再生气体入口和底部的杂质气体出口，将脱氨净化塔中的吸附剂进行再生；与此同时，进行吸附剂再生的脱氨净化塔的吸附剂再生完成，关闭顶部的再生气体入口和底部的杂质气体出口，脱氨净化塔顶部的氢气入口以及底部的氢气出口，对循环氢进行脱氨提纯。所述若干个脱氨净化塔循环交替进行吸附剂再生和脱氨提纯When the adsorption performance of the adsorbent in the deammonization purification tower for deammonization purification decreases, and the deammonization purification cannot be performed or the deammonization purification efficiency is low, the hydrogen inlet at the top of the deammonization purification tower and the hydrogen outlet at the bottom can be closed, and the top can be opened. At the regeneration gas inlet and the impurity gas outlet at the bottom, the adsorbent in the deammonization purification tower is regenerated; at the same time, the regeneration of the adsorbent in the deammonization purification tower for adsorbent regeneration is completed, and the regeneration gas inlet at the top and the bottom The impurity gas outlet, the hydrogen inlet at the top of the deammonization purification tower and the hydrogen outlet at the bottom are used for deammonization and purification of the circulating hydrogen. The several deammonization purification towers cycle and alternately perform adsorbent regeneration and deammonization purification
其中，再生气体通入脱氨净化塔进行吸附剂再生之前，需要经过再生气体减压装置减压和再生气体加热器加热，得到减压加热后的再生气体。所述减压加热后的再生气体的温度为120～150℃，压力为0.2～0.5MPa。进行再生时，脱氨净化塔内的再生温度为120～130℃。Among them, before the regeneration gas is passed into the deammonization purification tower to regenerate the adsorbent, it needs to be decompressed by the regeneration gas decompression device and heated by the regeneration gas heater to obtain the regeneration gas after decompression and heating. The temperature of the regeneration gas after the depressurization and heating is 120-150° C., and the pressure is 0.2-0.5 MPa. During regeneration, the regeneration temperature in the deammonization purification tower is 120-130°C.
最终，得到的脱氨提纯后的氢气纯度大于98％，所述脱氨提纯后的氢气中氨气含量＜0.5ppm。Finally, the obtained deammonized and purified hydrogen has a purity greater than 98%, and the ammonia content in the deammonized and purified hydrogen is less than 0.5 ppm.
本发明提供的循环氢脱氨提纯系统可以有效去除循环氢中氨和其他杂质，提高氢气纯度，使氢气中氨含量小于0.5ppm，杂质含量达到补充氢的标准，并回收利用脱氨后氢气，降低生产装置运行成本，减少加氢催化剂活性下降和冷换设备铵盐结垢腐蚀，保证生产装置长周期稳定运行，生产出优质的白油和基础油产品。The circulating hydrogen deammonization purification system provided by the present invention can effectively remove ammonia and other impurities in the circulating hydrogen, improve the purity of the hydrogen, make the ammonia content in the hydrogen less than 0.5ppm, and the impurity content reach the standard for supplementing hydrogen, and recycle and utilize the hydrogen after deammonization, Reduce the operating cost of the production unit, reduce the activity decline of the hydrogenation catalyst and the scaling and corrosion of the ammonium salt of the cold replacement equipment, ensure the long-term stable operation of the production unit, and produce high-quality white oil and base oil products.
本发明提供的装置主要利用变温吸附方法，采用低温低压下，利用吸附剂的吸附作用除去原料气中的氨，并回收利用，采用干燥还原的模式对吸附进行脱附，循环使用吸附剂，降低生产成本。该装置脱氨率高，不会造成氢气的浪费，并且不会产生大量的工业废水。The device provided by the present invention mainly utilizes the temperature swing adsorption method, adopts the adsorption effect of the adsorbent to remove the ammonia in the raw material gas under low temperature and low pressure, and recycles it. Cost of production. The device has a high ammonia removal rate, does not cause waste of hydrogen, and does not generate a large amount of industrial waste water.
结果表明，所述脱氨提纯后的氢气纯度大于98％，所述脱氨提纯后的氢气中氨气含量＜0.5ppm。The results show that the hydrogen purity after deammonization and purification is greater than 98%, and the ammonia content in the deammonization and purification hydrogen is less than 0.5ppm.
为了进一步理解本发明，下面结合实施例对本发明提供的循环氢脱氨提纯系统及方法进行说明，本发明的保护范围不受以下实施例的限制。In order to further understand the present invention, the cyclic hydrogen deammonization purification system and method provided by the present invention will be described below in conjunction with examples, and the scope of protection of the present invention is not limited by the following examples.
实施例1Example 1
本实施例提供了一种循环氢脱氨提纯系统，包括：This embodiment provides a circulating hydrogen deammonization purification system, including:
原料减压装置，所述原料减压装置主要用于对原料循环氢进行减压，使循环氢以低压状态进入系统；Raw material decompression device, the raw material decompression device is mainly used to decompress the raw material circulating hydrogen, so that the circulating hydrogen enters the system at a low pressure state;
入口与所述减压装置的出口相连的原料冷却器，由于自生产装置来的原料循环氢温度较高，通过原料冷却器将循环氢进行降温，本实施例采用循环冷却水对原料循环氢进行降温冷却；The raw material cooler whose inlet is connected to the outlet of the decompression device, because the temperature of the raw material circulating hydrogen from the production device is relatively high, the temperature of the circulating hydrogen is lowered through the raw material cooler. In this embodiment, circulating cooling water is used to cool the raw material circulating hydrogen. cooling down;
入口与所述原料冷却器的出口相连的气液分离装置，循环氢经过气液分离装置，分离去除气体中夹带的油和水滴。所述气液分离装置底部设置有液体出口，所述液体出口与污油管道相连；The inlet is connected to the gas-liquid separation device with the outlet of the raw material cooler, and the circulating hydrogen passes through the gas-liquid separation device to separate and remove the oil and water droplets entrained in the gas. A liquid outlet is provided at the bottom of the gas-liquid separation device, and the liquid outlet is connected to the dirty oil pipeline;
入口与所述气液分离装置的出口相连的2个并联的脱氨净化塔，两个脱氨净化塔交替工作进行氢气的脱氨提纯，即当其中一台脱氨净化塔进行氢气脱氨提纯时，另一台脱氨净化塔进行吸附剂的再生，所述脱氨净化塔顶部设置有氢气出口以及再生气体入口，所述脱氨净化塔顶部设置有氢气出口以及再生气体入口，底部设置有氢气入口以及杂质气体出口。为了减少设备主体的开口数量，所述氢气出口以及再生气体入口可以为同一个开口，并通过连接管路进行分支以及在管路上设置阀门进行气体流向的控制；氢气入口以及杂质气体出口可以为同一个开口，并通过连接管路进行分支以及在管路上设置阀门进行气体流向的控制。所述脱氨净化塔内装填有吸附剂。Two parallel deamination purification towers whose inlet is connected to the outlet of the gas-liquid separation device, the two deamination purification towers work alternately to carry out deammonization and purification of hydrogen, that is, when one of the deamination purification towers performs hydrogen deamination purification , another deammonization purification tower is used to regenerate the adsorbent, the top of the deammonization purification tower is provided with a hydrogen outlet and a regeneration gas inlet, the top of the deammonization purification tower is provided with a hydrogen outlet and a regeneration gas inlet, and the bottom is provided with a Hydrogen inlet and impurity gas outlet. In order to reduce the number of openings in the main body of the device, the hydrogen outlet and the regeneration gas inlet can be the same opening, and branched by connecting pipelines and valves are set on the pipelines to control the gas flow direction; the hydrogen inlet and the impurity gas outlet can be the same One opening, branched by connecting pipelines and setting valves on the pipelines to control the direction of gas flow. The deammonization purification tower is filled with adsorbent.
与所述再生气体入口依次相连的再生气体加热器以及再生气体减压装置。再生气体通过减压装置的减压后，在经过再生气体加热器的加热通过再生气体入口进入脱氨净化塔，所述再生气体为氮气，所述再生气体加热器的热源优选来自于管网的蒸汽。A regeneration gas heater and a regeneration gas decompression device sequentially connected to the regeneration gas inlet. After the regeneration gas is decompressed by the decompression device, it enters the deammonization purification tower through the regeneration gas inlet after being heated by the regeneration gas heater. The regeneration gas is nitrogen, and the heat source of the regeneration gas heater is preferably from the pipe network. steam.
所述气液分离装置和脱氨净化塔内的吸附剂种类参见表1，表1为吸附剂种类和装填部位。装填方式为布袋装填。The types of adsorbents in the gas-liquid separation device and the deammonization purification tower are shown in Table 1, and Table 1 shows the types of adsorbents and the filling positions. The filling method is cloth bag filling.
表1Table 1
其中，吸附剂-3和吸附剂-4主要装填于原料气液分离罐，装填顺序按照进料方向依次为吸附剂-3、吸附剂-4和吸附剂-3；Among them, Adsorbent-3 and Adsorbent-4 are mainly loaded in the raw material gas-liquid separation tank, and the filling sequence is Adsorbent-3, Adsorbent-4 and Adsorbent-3 according to the feeding direction;
吸附剂-1、吸附剂-2、吸附剂-5装填于脱氨净化塔。装填顺序按照进料方向为吸附剂-1、吸附剂-5、吸附剂-2和吸附剂-1。Adsorbent-1, Adsorbent-2, and Adsorbent-5 are loaded in the deammonization purification tower. The loading sequence according to the feeding direction is adsorbent-1, adsorbent-5, adsorbent-2 and adsorbent-1.
实施例2～4Embodiment 2-4
采用实施例1提供的循环氢脱氨提纯系统进行脱氨提纯。原料循环氢的主要成分和含量参见表2，经过脱氨提纯后的氢气参数以及工艺参数见表3。The cyclic hydrogen deammonization purification system provided in Example 1 was used for deammonization purification. See Table 2 for the main components and contents of raw material circulating hydrogen, and see Table 3 for hydrogen parameters and process parameters after deammonization and purification.
表2原料循环氢的主要成分和含量表Table 2 The main components and contents of raw material cycle hydrogen
表2中废氢的指标均是废氢经过原料冷却器和气液分离装置后的检测指标。The indicators of waste hydrogen in Table 2 are the detection indicators after the waste hydrogen passes through the raw material cooler and the gas-liquid separation device.
表3工艺参数以及产品性能参数Table 3 process parameters and product performance parameters
由表2可知：当操作压力低于1.8MPa时，原料气的纯度对产品气的纯度影响较大，压力降无法满足并入新氢系统的要求，氨含量无法达到我们的目标值≯0.5ppm；It can be seen from Table 2 that when the operating pressure is lower than 1.8MPa, the purity of the raw material gas has a great influence on the purity of the product gas, the pressure drop cannot meet the requirements of incorporating into the new hydrogen system, and the ammonia content cannot reach our target value≯0.5ppm ;
当操作压力高于2.3MPa时，能满足原料气纯度和氨含量要求，但是如果过高的操作压力，对吸附剂的强度和设备的选型、钢才的等级都提出了更高的要求，不建议使用。并且过高的产品气压力，并入新氢系统也需要减压才能完成，更重要的是对人身安全和设备安全不利。When the operating pressure is higher than 2.3MPa, it can meet the requirements of raw gas purity and ammonia content, but if the operating pressure is too high, higher requirements are put forward for the strength of the adsorbent, the selection of equipment, and the grade of steel. Not recommended for use. Moreover, if the product gas pressure is too high, the incorporation into the new hydrogen system also requires decompression to complete, and more importantly, it is detrimental to personal safety and equipment safety.
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, and it should be pointed out that for those of ordinary skill in the art, some improvements and modifications can be made without departing from the principle of the present invention. It should be regarded as the protection scope of the present invention.
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