TWI773979B - Ammonia purification apparatus and purification method - Google Patents

Ammonia purification apparatus and purification method Download PDF

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TWI773979B
TWI773979B TW109112064A TW109112064A TWI773979B TW I773979 B TWI773979 B TW I773979B TW 109112064 A TW109112064 A TW 109112064A TW 109112064 A TW109112064 A TW 109112064A TW I773979 B TWI773979 B TW I773979B
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liquid
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storage tank
ammonia
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TW202138302A (en
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詹益政
劉代宗
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詹益政
劉代宗
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Abstract

The invention provides an ammonia purification apparatus and purification method, including a heating and pressurizing unit, a first distillation unit, a first condensation unit, a second distillation unit, a second condensation unit, a storage tank unit, and a recycling unit. Through the design of double distillation unit and double condensation unit, crude ammonia with a concentration of 17 ~ 23% can be used as a raw material, and the purified ammonia gas with a purity greater than 5N can be obtained. In addition, with the arrangement of the recycling unit, the waste ammonia produced by the second distillation unit can be re-introduced into the recycling unit, and can be reheated and pressurized to be introduced into the first distillation unit as a raw material for recycling, which can be avoided due to the shortcomings of high concentration waste ammonia that needs to be diluted with water, and also achieve the purpose of circular economy.

Description

氨水純化裝置及純化方法 Ammonia water purification device and purification method

本發明是有關於一種純化裝置及純化方法,特別是指一種氨水純化裝置及純化方法。 The present invention relates to a purification device and a purification method, in particular to an ammonia water purification device and a purification method.

目前電子業或半導體業的製程中需使用到氣體,例如NH3(氨)氣體。對於先進製程而言,氣體的純度要求已由4N(99.99%)要求到5N(99.999%),甚至達6N5(99.99995%以上。目前純化NH3的現有技術是選用氨濃度為99%~99.99%的液相氨水做進料。目前最常用的是兩根塔,第一根塔除水,第二根塔除較氨氣為輕的氣體如N2、O2,及CH4;或第一根塔除較氨氣為輕的氣體,第二根塔除水。由於水分是較難除去的不純物,因此在除水的蒸餾塔後會接分子篩使水分能在規格以下,以符合半導體氣體的要求。 Gases, such as NH 3 (ammonia) gas, are currently used in the processes of the electronics industry or the semiconductor industry. For the advanced process, the purity requirement of the gas has been changed from 4N (99.99%) to 5N (99.999%), even up to 6N5 (99.99995% or more. The current technology for purifying NH 3 is to select ammonia concentration of 99% to 99.99%) The most commonly used liquid ammonia is two towers, the first tower removes water, and the second tower removes gases that are lighter than ammonia such as N 2 , O 2 , and CH 4 ; or the first tower removes water. The root tower removes gas that is lighter than ammonia, and the second tower removes water. Since water is an impurity that is difficult to remove, molecular sieves will be connected to the distillation tower for water removal so that the water can be below the specification to meet the requirements of semiconductor gases. Require.

由前述說明可知,目前純化NH3的現有技術是選用氨濃度為99%~99.99%的液相氨水做進料。然而,面對循環經濟的粗氨 水濃度只有17%~23%,倘用到前段所提到的這兩類蒸餾塔但沒有循環單元,則舊有的參數面對著進料是17~23%的變化是無法適用地,且舊有除水蒸餾塔的塔徑相對粗氨水純化所需的塔徑而言太小所以無法用在17~23%的進料,且廢氨水的濃度無法達到法定排放的標準,若要排放就需要用大量水來稀釋,則會浪費過多的水資源。 As can be seen from the foregoing description, the prior art of purifying NH at present is to select liquid-phase ammonia water with an ammonia concentration of 99% to 99.99% as the feed. However, the concentration of crude ammonia water in the face of circular economy is only 17%~23%. If the two types of distillation columns mentioned in the previous paragraph are used but there is no circulation unit, the old parameters are 17~23% for the feed. The change is not applicable, and the column diameter of the old water removal distillation column is too small relative to the column diameter required for the purification of crude ammonia water, so it cannot be used in 17~23% feed, and the concentration of waste ammonia water cannot reach the legal level. The standard of discharge, if it is to be discharged, it needs to be diluted with a large amount of water, which will waste too much water resources.

此外,由於目前高純度氨氣的純化其進料氨水濃度極高(液相進料濃度在99%~99.99%之間),為使產品的氣相達5N5或6N5以上,因此廢氨水中的氨濃度會大幅超過法規排放的標準,因此,並無法直接排放,必須另外儲存或找其它環保廠商處理或做為其他用途。 In addition, due to the extremely high concentration of ammonia water in the current purification of high-purity ammonia (the concentration of liquid phase feed is between 99% and 99.99%), in order to make the gas phase of the product reach 5N5 or 6N5 or more, the amount of ammonia in the waste ammonia water is extremely high. The concentration of ammonia will greatly exceed the emission standard of regulations. Therefore, it cannot be directly discharged. It must be stored separately or dealt with by other environmental protection manufacturers or used for other purposes.

因此,本發明的目的,即在提供一種用於純化濃度17%~23mole%的粗氨水的氨水純化裝置。 Therefore, the purpose of the present invention is to provide an ammonia water purification device for purifying the crude ammonia water with a concentration of 17% to 23 mole%.

於是,本發明的氨水純化裝置,包含一加熱加壓單元、一第一蒸餾單元、一第一冷凝單元、一第二蒸餾單元、一第二冷凝單元、一儲槽單元,及一再循環單元。 Therefore, the ammonia water purification device of the present invention includes a heating and pressurizing unit, a first distillation unit, a first condensation unit, a second distillation unit, a second condensation unit, a storage tank unit, and a recycling unit.

該加熱加壓單元用於將該粗氨水加熱加壓,使該粗氨水形成相對高壓的粗氨水。 The heating and pressurizing unit is used for heating and pressurizing the crude ammonia water to form relatively high pressure crude ammonia water.

該第一蒸餾單元包括一與該加熱加壓單元連通的第一蒸 餾塔,及一供該第一蒸餾塔加熱的煮沸加熱器,該相對高壓的粗氨水可進入該第一蒸餾塔進行蒸餾,得到第一混合氣體及第一排放液體。 The first distillation unit includes a first distillation unit in communication with the heating and pressurizing unit A distillation column, and a boiling heater for heating the first distillation column, the relatively high-pressure crude ammonia water can enter the first distillation column for distillation to obtain the first mixed gas and the first discharged liquid.

該第一冷凝單元用於冷凝該第一混合氣體,包括一與該第一蒸餾塔連通的第一冷凝器,及一位於該第一冷凝器下游的第一再冷凝器(re-condensor)。 The first condensing unit is used for condensing the first mixed gas, and includes a first condenser communicated with the first distillation column, and a first re-condensor located downstream of the first condenser.

該第二蒸餾單元對通過該第一再冷凝器後得到的冷凝液體進行蒸餾,以產生第二混合氣體及高濃度廢氨液,包括一與該第一再冷凝器連通的第二蒸餾塔,及一供該第二蒸餾塔加熱的再煮沸器。 The second distillation unit distills the condensed liquid obtained after passing through the first recondenser to generate the second mixed gas and high-concentration waste ammonia liquid, and includes a second distillation column communicated with the first recondenser, and a reboiler for heating the second distillation column.

該第二冷凝單元用於冷凝經該第二次蒸餾後的第二混合氣體,包括一與該第二蒸餾塔連通的第二冷凝器,及依序位於該第二冷凝器下游的一第二再冷凝器,及一過冷器,該過冷器接收經該第二再冷凝器冷凝後得到的液態氨並形成過冷液體。 The second condensing unit is used for condensing the second mixed gas after the second distillation, and includes a second condenser communicated with the second distillation column, and a second condenser sequentially located downstream of the second condenser A recondenser, and a subcooler that receives the liquid ammonia condensed by the second recondenser and forms a subcooled liquid.

該儲槽單元包括一與該過冷器連通,用於儲存通過該過冷器後的液態氨的精品儲存槽。 The storage tank unit includes a fine storage tank communicating with the subcooler for storing liquid ammonia after passing through the subcooler.

該再循環單元包括一分別與該第一蒸餾塔及第二蒸餾塔連通的氣液儲存槽、一加熱器,及一加壓幫浦,該第二蒸餾塔的高濃度氨液會排出進入該氣液儲存槽,該加熱器供該氣液儲存槽的液體加熱以提高壓力,使其具有與該第一蒸餾塔內的粗氨水大致相同 的壓力並具有飽和的氣液兩相,且該氣液儲存槽內的液相可再引入該第一蒸餾塔。 The recirculation unit includes a gas-liquid storage tank, a heater, and a pressurized pump respectively communicated with the first distillation column and the second distillation column. The high-concentration ammonia liquid of the second distillation column is discharged into the second distillation column. Gas-liquid storage tank, the heater is used for heating the liquid in the gas-liquid storage tank to increase the pressure, so that it has roughly the same value as the crude ammonia water in the first distillation column and has a saturated gas-liquid two-phase, and the liquid phase in the gas-liquid storage tank can be reintroduced into the first distillation column.

本發明的功效在於:透過本案創新的純化構想及簡單裝置的組合設計,而可應用於將半導體廠排出濃度為17%~23mole%的粗氨水進行純化,而可得到高純度(純度可達5N以上)的氨氣,且於第一次蒸餾的過程所產生的廢氨水濃度可符合政府規範直接排放,或是回製程循環利用,而可同時達成循環經濟的效益。 The effect of the present invention is: through the innovative purification concept and the combined design of the simple device in this case, it can be applied to purify the crude ammonia water with a concentration of 17% to 23 mole% discharged from a semiconductor factory, and high purity (purity up to 5N) can be obtained. The ammonia gas above), and the concentration of waste ammonia water produced in the first distillation process can be directly discharged in compliance with government regulations, or recycled back to the process, and at the same time, the benefits of circular economy can be achieved.

2:加壓單元 2: pressurization unit

21:桶槽 21: barrel tank

22:加壓幫浦 22: Pressurized pump

23:管路 23: Pipeline

24:壓力控制閥 24: Pressure control valve

25:溫度控制閥 25: Temperature control valve

3:第一蒸餾單元 3: The first distillation unit

31:第一蒸餾塔 31: The first distillation column

32:煮沸加熱器 32: Boil Heaters

4:第一冷凝單元 4: The first condensing unit

41:第一冷凝器 41: First condenser

42:第一再冷凝器 42: First Recondenser

5:第二蒸餾單元 5: Second distillation unit

51:第二蒸餾塔 51: Second distillation column

52:再煮沸器 52: Reboiler

6:第二冷凝單元 6: The second condensing unit

61:第二冷凝器 61: Second condenser

62:第二再冷凝器 62: Second Recondenser

63:過冷器 63: Subcooler

7:儲槽單元 7: Tank unit

71:精品儲存槽 71: Boutique Storage Tank

72:控壓裝置 72: Pressure control device

721:壓力計 721: Manometer

722:洩壓閥 722: Pressure relief valve

8:再循環單元 8: Recirculation unit

81:氣液儲存槽 81: Gas-liquid storage tank

82:加熱器 82: Heater

83:加壓幫浦 83: Pressurized pump

9:氣體吸收槽 9: Gas absorption tank

M:流量調節單元 M: flow adjustment unit

M1~M5:流量調節閥 M1~M5: Flow control valve

91~9:步驟 91~9: Steps

本發明的其他的特徵及功效,將於參照圖式的實施方式中清楚地呈現,其中:圖1是本發明氨水純化裝置之實施例的示意圖;及圖2是利用本發明氨水純化裝置之實施例進行氨水純化的步驟流程文字圖。 Other features and effects of the present invention will be clearly presented in the embodiments with reference to the drawings, wherein: FIG. 1 is a schematic diagram of an embodiment of the ammonia water purification device of the present invention; and FIG. 2 is the implementation of the ammonia water purification device of the present invention. Example of the process flow chart of the purification of ammonia water.

本發明的氨水純化裝置是用於供濃度17mole%~23mole%的粗氨水進行純化,而可得到氨氣濃度達5N以上的氨水純化裝置。其中,前述該濃度17%~23mole%的粗氨水的來源可以是來自半導體廠稀釋後排出的氨水。 The ammonia water purification device of the present invention is used for purifying crude ammonia water with a concentration of 17 mole% to 23 mole%, and can obtain an ammonia water purification device with an ammonia gas concentration of more than 5N. Wherein, the source of the aforementioned crude ammonia water with a concentration of 17% to 23 mole% can be the ammonia water discharged from the semiconductor factory after dilution.

參閱圖1,本發明氨水純化裝置的一實施例,包含一加熱加壓單元2、一第一蒸餾單元3、一第一冷凝單元4、一第二蒸餾單元5、一第二冷凝單元6、一儲槽單元7、一再循環單元8、一氣體吸收槽9,及一流量調節單元M。 Referring to FIG. 1, an embodiment of the ammonia water purification device of the present invention includes a heating and pressurizing unit 2, a first distillation unit 3, a first condensation unit 4, a second distillation unit 5, a second condensation unit 6, A storage tank unit 7, a recirculation unit 8, a gas absorption tank 9, and a flow adjustment unit M.

該加熱加壓單元2用於將濃度介於17~mole23%的粗氨水加熱加壓,使該粗氨水形成壓力大於該粗氨水的相對高壓的粗氨水。包含一用於供容置熱媒的桶槽21、一加壓幫浦22、一設置於該桶槽21可被該熱媒加熱的管路23、一壓力控制閥24,及一溫度控制閥25。粗氨水可經由該加壓幫浦22送入該管路23進入該第一蒸餾塔31。透過該壓力控制閥24可控制經由該管路23進入第一蒸餾塔31的粗氨水壓力,並利用該溫度控制閥25調整桶槽21中的熱媒流量,以控制該管路23中的粗氨水的溫度,使該粗氨水達到預期的熱力學狀態再進入第一蒸餾單元。 The heating and pressurizing unit 2 is used to heat and pressurize the crude ammonia water with a concentration of 17 to 23%, so that the crude ammonia water can be formed into a relatively high-pressure crude ammonia water with a pressure greater than that of the crude ammonia water. It includes a tank 21 for accommodating a heat medium, a pressurized pump 22, a pipeline 23 arranged in the tank 21 to be heated by the heat medium, a pressure control valve 24, and a temperature control valve 25. Crude ammonia water can be fed into the pipeline 23 via the pressurized pump 22 and into the first distillation column 31 . Through the pressure control valve 24, the pressure of the crude ammonia water entering the first distillation column 31 through the pipeline 23 can be controlled, and the temperature control valve 25 can be used to adjust the heat medium flow in the tank 21 to control the crude ammonia in the pipeline 23. The temperature of the ammonia water makes the crude ammonia water reach the expected thermodynamic state and then enters the first distillation unit.

該第一蒸餾單元3包括一與該加熱加壓單元2的桶槽21及管路23連通的第一蒸餾塔31,及一鄰近該第一蒸餾塔31底部設置,供該第一蒸餾塔31加熱的煮沸加熱器32。 The first distillation unit 3 includes a first distillation column 31 communicating with the barrel tank 21 and the pipeline 23 of the heating and pressurizing unit 2 , and a first distillation column 31 adjacent to the bottom of the first distillation column 31 for the first distillation column 31 Heated boil heater 32 .

經過該加熱加壓單元後的相對高壓的粗氨水可經由該管路23進入該第一蒸餾塔31,並利用該煮沸加熱器32煮沸氨水,飽和氣相往蒸餾塔上方流動而由蒸餾塔頂冷凝氣冷凝的液體往塔底流動進行蒸餾,而得到第一混合氣體及第一排放液體。此外,該第 一蒸餾塔31還可透過管路將回流得到而具有高溫的第一排放液體再引入該桶槽21,作為熱源以供該管路23中之粗氨水加熱的熱媒,而可節省能源。 The relatively high-pressure crude ammonia water after passing through the heating and pressurizing unit can enter the first distillation column 31 through the pipeline 23, and the ammonia water can be boiled by the boiling heater 32, and the saturated gas phase flows above the distillation column and flows from the top of the distillation column. The liquid condensed by the condensed gas flows to the bottom of the tower for distillation to obtain the first mixed gas and the first discharged liquid. Furthermore, this A distillation column 31 can also re-introduce the first discharge liquid obtained by reflux and with high temperature into the barrel tank 21 through the pipeline as a heat source for heating the crude ammonia water in the pipeline 23, thereby saving energy.

該第一冷凝單元4用於冷凝經該第一次蒸餾後排出的第一混合氣體,包括一與該第一蒸餾塔31連通的第一冷凝器41,及一位於該第一冷凝器41下游的第一再冷凝器42。 The first condensing unit 4 is used for condensing the first mixed gas discharged after the first distillation, and includes a first condenser 41 communicated with the first distillation column 31 , and a first condenser 41 downstream of the first condenser 41 . The first recondenser 42 .

該第二蒸餾單元5與該第一冷凝單元4及該再循環單元8連通,用於對通過該第一再冷凝器42後得到的冷凝液體進行第二次蒸餾。詳細地說,該第二蒸餾單元5包括一與該第一再冷凝器42及該再循環單元8連通的第二蒸餾塔51,及一鄰近該第二蒸餾塔51底部設置,提供該第二蒸餾塔51內的物質(氨水)加熱的再煮沸器52。透過該再煮沸器52對流到該第二蒸餾塔51底部的氨水(冷凝液體)進行加熱,並於該第二蒸餾塔51進行蒸餾以產生第二混合氣體及塔底高濃度的廢氨液。其中,該第二混合氣體會排出進入該第二冷凝單元6,而該廢氨液則可經管路引入該再循環單元8。 The second distillation unit 5 is in communication with the first condensation unit 4 and the recirculation unit 8, and is used for the second distillation of the condensed liquid obtained after passing through the first recondenser 42. In detail, the second distillation unit 5 includes a second distillation column 51 in communication with the first recondenser 42 and the recirculation unit 8, and a second distillation column 51 adjacent to the bottom of the second distillation column 51 to provide the second distillation column 51. The reboiler 52 for heating the substance (ammonia) in the distillation column 51. The ammonia water (condensed liquid) flowing to the bottom of the second distillation column 51 is heated through the reboiler 52, and is distilled in the second distillation column 51 to generate a second mixed gas and a high-concentration waste ammonia liquid at the bottom of the column. Wherein, the second mixed gas will be discharged into the second condensing unit 6 , and the waste ammonia liquid can be introduced into the recycling unit 8 through pipelines.

由於前述該第一、二蒸餾塔31、51的細部結構為本技術領域習知,因此,不再多加說明。此外,於本實施例中,該第一、二加熱器32、52是以熱交換管路為例說明但不以此為限。 Since the detailed structures of the aforementioned first and second distillation towers 31 and 51 are well known in the technical field, they will not be further described. In addition, in this embodiment, the first and second heaters 32 and 52 are illustrated by taking heat exchange pipes as an example, but not limited thereto.

該第二冷凝單元6與該第二蒸餾單元5連通,用於接收並冷凝經該第二次蒸餾後得到的第二混合氣體,包括一與該第二蒸餾 塔51連通用於接收並冷凝該第二混合氣體的第二冷凝器61,及依序位於該第二冷凝器61下游的一第二再冷凝器62,及一過冷器63,該第二再冷凝器62是對通過該第二冷凝器61後排出的氣體進行再冷凝,該過冷器63則是用於將經過該第二再冷凝器62冷凝後得到的液態氨進行過冷程序。 The second condensation unit 6 is communicated with the second distillation unit 5 for receiving and condensing the second mixed gas obtained after the second distillation, including a The column 51 is connected to a second condenser 61 for receiving and condensing the second mixed gas, a second recondenser 62 located downstream of the second condenser 61 in sequence, and a subcooler 63, the second The recondenser 62 is used for recondensing the gas discharged after passing through the second condenser 61 , and the subcooler 63 is used for subcooling the liquid ammonia obtained after passing through the second recondenser 62 condensed.

該儲槽單元7包括一與該過冷器63連通,用於儲存通過該過冷器63的液態氨的精品儲存槽71,以及一控壓裝置72,該控壓裝置72可具有一用於偵測該精品儲存槽71壓力的壓力計721及一洩壓閥722。該液態氨儲存於該精品儲存槽71時具有氣/液兩相,該儲槽單元7透過該控壓裝置72可用以控制該精品儲存槽71的壓力,以避免壓力過高。 The storage tank unit 7 includes a fine storage tank 71 communicating with the subcooler 63 for storing liquid ammonia passing through the subcooler 63, and a pressure control device 72, which may have a pressure control device 72 for A pressure gauge 721 and a pressure relief valve 722 for detecting the pressure of the fine storage tank 71 are provided. The liquid ammonia has gas/liquid two phases when stored in the fine-quality storage tank 71 , and the storage tank unit 7 can control the pressure of the fine-quality storage tank 71 through the pressure control device 72 to prevent the pressure from being too high.

該再循環單元8包括一氣液儲存槽81、一加熱器82,及一加壓幫浦83,該氣液儲存槽81分別與該第一蒸餾塔31、第二蒸餾塔51及氣體吸收槽9連通,其中,該第二蒸餾塔51冷凝回流的液體(廢氨液)可引入該氣液儲存槽81,該加熱器82及加壓幫浦83供加熱並加壓該氣液儲存槽81的液體,使其具有與該第一蒸餾塔31內的粗氨水大致相同的壓力並同時具有氣相及液相,該氣液儲存槽81內的液相可再引入該第一蒸餾塔31進行濃縮純化的蒸餾作業,而該氣液儲存槽81內的氣相可排出至該氣體吸收槽9。此外,要說明的是,該再循環單元8的加熱器82也可與該第一蒸餾塔31連通, 並透過將該第一蒸餾塔31回流得到的具有高溫的第一排放液體引入該加熱器82(熱交換器)做為部份熱源提供。 The recirculation unit 8 includes a gas-liquid storage tank 81 , a heater 82 , and a pressurized pump 83 . The gas-liquid storage tank 81 is connected to the first distillation column 31 , the second distillation column 51 and the gas absorption tank 9 respectively. Connected, wherein, the liquid (waste ammonia liquid) condensed and refluxed in the second distillation column 51 can be introduced into the gas-liquid storage tank 81, and the heater 82 and the pressurized pump 83 are provided for heating and pressurizing the gas-liquid storage tank 81. The liquid has approximately the same pressure as the crude ammonia water in the first distillation column 31 and has a gas phase and a liquid phase at the same time, and the liquid phase in the gas-liquid storage tank 81 can be reintroduced into the first distillation column 31 for concentration. Purified distillation operation, and the gas phase in the gas-liquid storage tank 81 can be discharged to the gas absorption tank 9 . In addition, it should be noted that the heater 82 of the recirculation unit 8 may also communicate with the first distillation column 31, And the first discharge liquid with high temperature obtained by refluxing the first distillation column 31 is introduced into the heater 82 (heat exchanger) as a partial heat source.

該氣體吸收槽9分別與該第一再冷凝器42、第二再冷凝器62、精品儲存槽71,及氣液儲存槽81連通,用於吸收自該第一、二再冷凝器42、62、該精品儲存槽71,及該氣液儲存槽81排出之氣體(NH3、H2、N2、O2、CH4等),並調節各桶槽的壓力避免桶槽壓力過高的危險,而具純化及工安的目的。 The gas absorption tank 9 communicates with the first recondenser 42 , the second recondenser 62 , the fine product storage tank 71 , and the gas-liquid storage tank 81 respectively, and is used for absorbing from the first and second recondensers 42 , 62 , the high-quality storage tank 71, and the gas (NH 3 , H 2 , N 2 , O 2 , CH 4 , etc.) discharged from the gas-liquid storage tank 81 , and adjust the pressure of each barrel to avoid the danger of excessive pressure in the barrel , and has the purpose of purification and industrial safety.

該流量調節單元M可視需求,而對應前述第一、二蒸餾單元3、5,第一、二冷凝單元4、6,儲槽單元7,再循環單元8,及氣體吸收槽9的其中至少任一者設置依據壓力或溫度設定用於調節氣體或液體的流量調節閥,以調節並控制排出之氣體或液體的流量。於本實施例中是以該流量調節單元M具有分別對應設置於該第一蒸餾塔31的流量調節閥M1、設置於該第一冷凝器41與該第一再冷凝器42之間的流量調節閥M2、設置於該第一再冷凝器42與該第二蒸餾塔51之間的流量調節閥M3、設置於該第二冷凝器61與該第二再冷凝器62之間的流量調節閥M4,以及設置於該第二再冷凝器62與過冷器63之間的流量調節閥M5,以調節進入第一再冷凝器42、第二再冷凝器62,及過冷器63的氣體及液體流量。然而,要說明的是,於實際實施時,該流量調節單元M的設置位置並不以此為限,這些裝置或許會有沒有畫出來的其他裝置,如緩衝桶與之相 連,用以維持穩定壓力的流動。 The flow adjustment unit M may correspond to at least any of the aforementioned first and second distillation units 3 and 5, first and second condensing units 4 and 6, storage tank unit 7, recirculation unit 8 and gas absorption tank 9, depending on requirements. One is to set a flow regulating valve for regulating gas or liquid according to pressure or temperature, so as to regulate and control the flow rate of discharged gas or liquid. In this embodiment, the flow regulating unit M has a flow regulating valve M1 corresponding to the first distillation column 31 and a flow regulating valve M1 arranged between the first condenser 41 and the first recondenser 42 respectively. The valve M2, the flow regulating valve M3 arranged between the first recondenser 42 and the second distillation column 51, the flow regulating valve M4 arranged between the second condenser 61 and the second recondenser 62 , and the flow regulating valve M5 disposed between the second recondenser 62 and the subcooler 63 to adjust the gas and liquid entering the first recondenser 42, the second recondenser 62, and the subcooler 63 flow. However, it should be noted that, in actual implementation, the setting position of the flow adjustment unit M is not limited to this, and these devices may have other devices that are not shown, such as buffer buckets. connected to maintain a stable pressure flow.

配合參閱圖1、2,茲將利用前述本發明該氨水純化裝置的實施例進行粗氨水純化的方法說明如下。 Referring to FIGS. 1 and 2 in conjunction, the method for purifying crude ammonia water by using the embodiment of the ammonia water purification device of the present invention will be described as follows.

首先,進行步驟91,將濃度介於17~23mole%的粗氨水溶液加壓加熱。 First, step 91 is performed, and the crude ammonia aqueous solution with a concentration of 17-23 mole% is heated under pressure.

詳細的說,該步驟91是將位於外界之儲槽內,壓力/溫度約為1bar/20℃,且濃度介於17~23mole%的粗氨水溶液透過流量調節閥調節流量並利用該加壓幫浦22加壓,使其變成壓力約為4.4bar的粗氨水溶液進入該管路23,再藉由該桶槽21的熱媒對內有粗氨水流動的管路23加熱,令該粗氨水溶液的溫度達到約30℃,而得到相對高壓的粗氨水。該步驟的目的即是在避免飽和蒸汽在該管路23裡的產生及流動。 In detail, the step 91 is to adjust the flow rate of the crude ammonia aqueous solution with a pressure/temperature of about 1 bar/20°C and a concentration of 17-23 mole% in an external storage tank through a flow control valve and use the pressurized aid to adjust the flow rate. Pu 22 is pressurized so that it becomes a crude ammonia solution with a pressure of about 4.4 bar and enters the pipeline 23, and then the pipeline 23 in which the crude ammonia flows is heated by the heating medium of the barrel 21, so that the crude ammonia solution is heated. The temperature reaches about 30 °C, and relatively high pressure crude ammonia water is obtained. The purpose of this step is to avoid the generation and flow of saturated steam in the pipeline 23 .

接著,進行步驟92,將該相對高壓的粗氨水引入該第一蒸餾單元3進行第一次蒸餾。 Next, step 92 is performed, and the relatively high-pressure crude ammonia water is introduced into the first distillation unit 3 for first distillation.

詳細的說,該步驟92是將該相對高壓的粗氨水引入該第一蒸餾塔31,並利用位於該第一蒸餾塔31底部的該煮沸加熱器32將該第一蒸餾塔內流入的液體進行煮沸,在煮沸槽中形成飽和氣體及液體(廢氨水)。飽和氣體往上流動,液體則由流量控制閥M1進行排放或做能源再利用。該第一蒸餾塔31內為氣液兩相做逆向流動,液體往下流動,氣體往上流動,並同時進行熱傳、質傳及相平 衡。因此,第一次蒸餾後的該第一混合氣體由該第一蒸餾塔31的頂部排出並經由管路進入該第一冷凝器41,而其它氣體則被冷凝回流到該第一蒸餾塔31。 In detail, the step 92 is to introduce the relatively high-pressure crude ammonia water into the first distillation column 31, and use the boiling heater 32 located at the bottom of the first distillation column 31 to carry out the liquid flow in the first distillation column. Boil to form saturated gas and liquid (waste ammonia water) in the boiling tank. The saturated gas flows upward, and the liquid is discharged or reused for energy by the flow control valve M1. In the first distillation column 31, the gas-liquid two-phase flow is reversed, the liquid flows down, and the gas flows up, and heat transfer, mass transfer and phase leveling are carried out at the same time. balance. Therefore, the first mixed gas after the first distillation is discharged from the top of the first distillation column 31 and enters the first condenser 41 through a pipeline, while other gases are condensed and refluxed to the first distillation column 31 .

要說明的是,該第一排放液體(即氨水廢液)的氨濃度可利用自該第一蒸餾塔31的頂部排出的該第一混合氣體的多寡控制,而得以讓該第一排放液體的氨濃度符合政府排放規範直接進行排放或再引用回製程循環應用,且該第一排放液體利用流量調節閥M2調節其排出量,使符合質量守恆。 It should be noted that, the ammonia concentration of the first discharge liquid (ie, ammonia water waste liquid) can be controlled by the amount of the first mixed gas discharged from the top of the first distillation column 31, so that the concentration of the first discharge liquid can be controlled. The ammonia concentration is directly discharged in accordance with the government discharge specification or re-referenced to the process cycle application, and the discharge amount of the first discharged liquid is adjusted by the flow regulating valve M2, so as to meet the quality conservation.

於一些實施例中,該第一排放液體的氨濃度可控制在不大於政府排放規範內。於一些實施例中,該第一排放液體的氨濃度可控制在低於政府法規的排放限制,並可直接排放。 In some embodiments, the ammonia concentration of the first discharge liquid can be controlled to be no greater than government discharge specifications. In some embodiments, the ammonia concentration of the first discharge liquid can be controlled below the discharge limit of government regulations and can be discharged directly.

此外,要再說明的是,由於經過該第一蒸餾塔31蒸餾後得到的該第一排放液體具有較高的溫度,因此,利用將該第一排放液體循環引至進入該加熱加壓單元2的桶槽21,並做為熱媒使用後再加以排放,可節省能源並具經濟價值。 In addition, it should be noted that, because the first discharge liquid obtained after distillation through the first distillation column 31 has a relatively high temperature, therefore, the first discharge liquid is circulated and introduced into the heating and pressurizing unit 2 It can save energy and have economic value.

接著,進行步驟93,利用該第一冷凝單元4將該第一混合氣體進行冷凝。 Next, step 93 is performed, and the first mixed gas is condensed by the first condensation unit 4 .

該步驟93是先將進入該第一冷凝器41的第一混合氣體進行冷凝。冷凝後得到的飽和氣體會經由管路排出至該第一再冷凝器42進行再冷凝,而經該第一冷凝器41冷凝後得到液體則可藉由 管路再回流至該第一蒸餾塔31。 Step 93 is to condense the first mixed gas entering the first condenser 41 first. The saturated gas obtained after condensation will be discharged to the first recondenser 42 for recondensation through the pipeline, and the liquid obtained after condensation through the first condenser 41 can be obtained by The line returns to the first distillation column 31 again.

接著,將通過該第一冷凝器41並進入該第一再冷凝器42的飽和氣體進行再冷凝,得到一冷凝液體及一排出氣體。其中,該飽和氣體可透過該流量調節閥M2以控制進入該第一再冷凝器42的氣體流量,經冷凝後的該冷凝液體則可經由流量調節閥M3控制流量並引入該第二蒸餾塔51。該第一再冷凝器42的排出氣體為含有如N2、O2、H2及CH4等雜氣,以及極少的H2O,可透過管路引入該氣體吸收槽9。 Next, the saturated gas passing through the first condenser 41 and entering the first recondenser 42 is recondensed to obtain a condensed liquid and an exhaust gas. Wherein, the saturated gas can pass through the flow regulating valve M2 to control the gas flow entering the first re-condenser 42 , and the condensed liquid can be controlled by the flow regulating valve M3 and introduced into the second distillation column 51 through the flow regulating valve M3 . The exhaust gas of the first recondenser 42 contains impurities such as N 2 , O 2 , H 2 and CH 4 , and very little H 2 O, which can be introduced into the gas absorption tank 9 through a pipeline.

然後,再進行步驟94,利用該第二蒸餾單元5將該冷凝液體進行第二次蒸餾。 Then, step 94 is performed again, and the condensed liquid is subjected to a second distillation by the second distillation unit 5 .

詳細的說,該步驟94是將由該第二再冷凝器42進入該第二蒸餾塔51的冷凝液體,利用位於該第二蒸餾塔51底部的再煮沸器52加熱成氣相後再進行冷凝形成氣液兩相,以濃縮並純化氨氣。冷凝後的第二混合氣體(氣相)由該第二蒸餾塔51的塔頂排出並經由管路進入該第二冷凝器61,而被冷凝回流到該第二蒸餾塔51塔底的液相因為含水量低,為高濃度的廢氨液無法直接排放,因此,該高濃度廢氨液可透過管路回流至該再循環單元8的加熱氣液儲存槽81,並利用該加熱器82及加壓幫浦83使該高濃度廢氨液在桶槽81內成為飽和氣液體,具有與進入該第一蒸餾塔31的相對高壓的粗氨水約相近的溫度及壓力後,即可將桶槽81內的飽和液體引入該 第一蒸餾塔31再進行循環蒸餾。 In detail, in step 94, the condensed liquid entering the second distillation column 51 from the second recondenser 42 is heated into a gas phase by the reboiler 52 at the bottom of the second distillation column 51 and then condensed to form a gas phase. Gas-liquid two-phase to concentrate and purify ammonia. The condensed second mixed gas (gas phase) is discharged from the top of the second distillation column 51 and enters the second condenser 61 through the pipeline, and is condensed and refluxed to the liquid phase at the bottom of the second distillation column 51 Because of the low water content, the high-concentration waste ammonia liquid cannot be directly discharged. Therefore, the high-concentration waste ammonia liquid can be returned to the heating gas-liquid storage tank 81 of the recirculation unit 8 through the pipeline, and the heater 82 and the The pressurized pump 83 makes this high-concentration waste ammonia liquid become a saturated gas liquid in the barrel tank 81, and after having a temperature and pressure approximately similar to the relatively high-pressure crude ammonia water entering the first distillation column 31, the barrel tank can be replaced. The saturated liquid in 81 is introduced into the The first distillation column 31 is again subjected to circulating distillation.

要說明的是,該第二蒸餾塔51的廢氨液的氨莫耳濃度遠高於政府法規所規範的排放數值,尤其當進料氨的濃度是在17~23mole%變動,蒸餾塔底排放的廢氨水濃度變化將非常大,且由各蒸餾塔頂排放的氨氣量將不易控制,若以傳統的氨水純化裝置並無法得到高純度(純度>5N)的液態氨精品,這也是目前一般都是以氨濃度99mole%~99.99mole%作為純化進料的限制。此外,該第二蒸餾塔51的廢氨液若沒有經過該再循環單元8再進入第一蒸餾塔31,則所得到的氨氣純度會因進料濃度的變化而有大幅度的改變,而在操作上要時時調整排出氣量的大小,此非習知的氨水純化裝置所能達成,因此,本發明透過該再循環單元8,進料濃度在17~23mole%,而可維持第二蒸餾塔51頂出來的氨氣可達5N以上的純度。 It should be noted that the ammonia molar concentration of the waste ammonia liquid of the second distillation column 51 is much higher than the discharge value regulated by government regulations, especially when the concentration of feed ammonia varies between 17 and 23 mole%, the bottom of the distillation column discharges The concentration change of the waste ammonia water will be very large, and the amount of ammonia discharged from the top of each distillation tower will be difficult to control. The limit is that the ammonia concentration is 99mole%~99.99mole% as the purification feed. In addition, if the waste ammonia liquid of the second distillation column 51 does not pass through the recycling unit 8 and then enters the first distillation column 31, the purity of the obtained ammonia gas will be greatly changed due to the change of the feed concentration, and In operation, it is necessary to adjust the size of the exhaust gas from time to time, which is not achieved by the conventional ammonia water purification device. Therefore, the present invention can maintain the second distillation through the recirculation unit 8, and the feed concentration is 17-23 mole%. The ammonia gas from the top of the tower 51 can reach a purity of more than 5N.

於本實施例中,是將自該第二蒸餾塔51塔底的冷凝回流的液相引入該氣液儲存槽81,並將其加熱加壓到4.4bar/60℃,即可再引入該第一蒸餾塔31濃縮純化,而該氣液儲存槽81的飽和氣體的氨濃度為90mole%以上,並可再進入氣體吸收槽單元9。 In this embodiment, the condensed and refluxed liquid phase from the bottom of the second distillation column 51 is introduced into the gas-liquid storage tank 81, and then heated and pressurized to 4.4 bar/60° C. A distillation column 31 concentrates and purifies, and the ammonia concentration of the saturated gas in the gas-liquid storage tank 81 is more than 90 mole%, and it can enter the gas absorption tank unit 9 again.

接著,進行步驟95,利用該第二冷凝單元6將該第二混合氣體進行冷凝,得到精製液態氨。 Next, step 95 is performed, and the second mixed gas is condensed by the second condensation unit 6 to obtain purified liquid ammonia.

該步驟95是先將進入該第二冷凝器61的第二混合氣體 進行冷凝。冷凝後得到的飽和氣體會經由管路排出至該第二再冷凝器62進行再冷凝,而經該第二冷凝器61冷凝後得到液體則可藉由管路再回流至該第二蒸餾塔51。 In step 95, the second mixed gas entering the second condenser 61 is firstly Condensate. The saturated gas obtained after condensation will be discharged to the second recondenser 62 for recondensation through the pipeline, and the liquid obtained after condensation through the second condenser 61 can be refluxed to the second distillation column 51 through the pipeline. .

接著,將通過該第二冷凝器61並進入該第二再冷凝器62的飽和氣體進行再冷凝,得到一液態氨及一排出氣體。其中,該飽和氣體可經由流量調節閥M4以控制進入該第二再冷凝器62的流量,該第二再冷凝器62排出的氣體可透過管路引入至該氣體吸收槽9,該液態氨可經由流量調節閥M5控制進入該過冷器63的流量。該過冷器63接收經該第二再冷凝器62冷凝後得到精製過冷的液態氨。 Next, the saturated gas passing through the second condenser 61 and entering the second recondenser 62 is recondensed to obtain a liquid ammonia and an exhaust gas. Wherein, the saturated gas can control the flow rate entering the second recondenser 62 through the flow regulating valve M4, the gas discharged from the second recondenser 62 can be introduced into the gas absorption tank 9 through the pipeline, and the liquid ammonia can be The flow into the subcooler 63 is controlled via a flow regulating valve M5. The subcooler 63 receives the refined and subcooled liquid ammonia obtained after being condensed by the second recondenser 62 .

最後,進行步驟96,儲存精製液態氨。 Finally, step 96 is performed to store the refined liquid ammonia.

該步驟96是透過管路將通過該過冷器63後得到的精製過冷的液態氨引入該精品儲存槽71中,而形成低壓的氣液兩相氨液進行儲存。此外,可進一步透過該控壓裝置72監控並調整該精品儲存槽71的壓力。當該精品儲存槽71受環境的溫度影響致使壓力超過設定值時,則可經由該洩壓閥722洩壓,將該精品儲存槽71內的氣態氨透過管路排出至該氣體吸收槽9,以維持該精品儲存槽71的壓力。 In step 96 , the purified and subcooled liquid ammonia obtained after passing through the subcooler 63 is introduced into the high-quality storage tank 71 through a pipeline to form a low-pressure gas-liquid two-phase ammonia liquid for storage. In addition, the pressure of the boutique storage tank 71 can be further monitored and adjusted through the pressure control device 72 . When the high-quality storage tank 71 is affected by the temperature of the environment and causes the pressure to exceed the set value, the pressure can be released through the pressure relief valve 722, and the gaseous ammonia in the high-quality storage tank 71 is discharged to the gas absorption tank 9 through the pipeline, In order to maintain the pressure of the boutique storage tank 71 .

此外,要再說明的是,經該第二次蒸餾後排出的該第二混合氣體的含水量已極低,而該第二混合氣體中的雜氣含有如N2、 H2、O2、CH4,因此,為了提昇最終製得之氨氣的純度,可在該第二冷凝單元62中將該第二混合氣體進一步進行排放蒸餾(詳細步驟請參考TW I413891)。該排放蒸餾的排放氣體可再引入該氣體吸收槽9。此外,該桶槽71也可以為達更高純度進行絕熱排放蒸餾,而排放的氨氣可透過洩壓閥722進入氣體吸收槽9。此外,該氣體吸收槽9的氨水到一定量後,也可再加水稀釋成濃度為17~23%的液氨,而再引入該第一蒸餾塔31進行濃縮純化循環。 In addition, it should be noted that the water content of the second mixed gas discharged after the second distillation is extremely low, and the impurity gas in the second mixed gas contains such as N 2 , H 2 , O 2 , CH 4 , therefore, in order to improve the purity of the final ammonia gas, the second mixed gas can be further discharged and distilled in the second condensing unit 62 (for detailed steps, please refer to TW I413891). The exhaust gas from the exhaust distillation can be reintroduced into the gas absorption tank 9 . In addition, the barrel tank 71 can also perform adiabatic exhaust distillation for higher purity, and the exhausted ammonia gas can enter the gas absorption tank 9 through the pressure relief valve 722 . In addition, after the ammonia water in the gas absorption tank 9 reaches a certain amount, it can also be diluted with water to form liquid ammonia with a concentration of 17-23%, and then introduced into the first distillation column 31 for concentration and purification cycle.

本發明透過雙蒸餾塔(第一、二蒸餾單元3、5)、雙冷凝單元(第一、二冷凝單元4、6)的組成設計,因此,可利用濃度為17~23mole%的粗氨水為原料,而純化得到純度大於5N的氨氣,並引用本案最具創意構想的再循環單元8,令該第二蒸餾塔51的廢氨水可重新導入該再循環單元8,使重新加熱達到所需要的壓力,在單元81的桶槽形成氣液兩相,液相再導入該第一蒸餾塔31作為原料再循環利用,而可避免因高濃度廢氨液需加水稀釋排放的缺點。此外,利用控制該第一蒸餾單元3排出的混合氣體量即可控制該第一排放液體的氨濃度,使該第一排放液體的氨濃度可符合法規直接排放,而無需再加水稀釋。再者,本發明還同時利用將該第一蒸餾單元3回流得到的第一排放液體循環引至該加熱加壓單元2及該再循環單元8,以做為該加熱加壓單元2的加熱器23及/或該再循環單元8的加熱器82的部份熱源來源使用,而可節省能源並達成循 環經濟的效果,故確實能達成本發明的目的。 The present invention passes through the composition design of double distillation towers (first, second distillation units 3, 5) and double condensation units (first and second condensation units 4, 6), therefore, the available concentration is 17 ~ 23 mole% of crude ammonia water is The raw material is purified to obtain ammonia with a purity greater than 5N, and the most creatively conceived recycling unit 8 in this case is used, so that the waste ammonia water of the second distillation column 51 can be re-introduced into the recycling unit 8, so that the reheating can reach the required level. At the same pressure, gas-liquid two-phase is formed in the barrel of unit 81, and the liquid phase is re-introduced into the first distillation column 31 as a raw material for recycling, which can avoid the disadvantage that high-concentration waste ammonia liquid needs to be diluted and discharged with water. In addition, by controlling the amount of mixed gas discharged from the first distillation unit 3, the ammonia concentration of the first discharged liquid can be controlled, so that the ammonia concentration of the first discharged liquid can be directly discharged in compliance with regulations without adding water for dilution. Furthermore, the present invention also utilizes the first discharge liquid obtained by refluxing the first distillation unit 3 to be circulated to the heating and pressurizing unit 2 and the recirculation unit 8 to serve as the heater of the heating and pressurizing unit 2. 23 and/or part of the heat source of the heater 82 of the recirculation unit 8 can be used to save energy and achieve cycle Therefore, the purpose of the present invention can indeed be achieved.

惟以上所述者,僅為本發明的實施例而已,當不能以此限定本發明實施的範圍,凡是依本發明申請專利範圍及專利說明書內容所作的簡單的等效變化與修飾,皆仍屬本發明專利涵蓋的範圍內。 However, the above are only examples of the present invention, and should not limit the scope of implementation of the present invention. Any simple equivalent changes and modifications made according to the scope of the patent application of the present invention and the contents of the patent specification are still included in the scope of the present invention. within the scope of the invention patent.

2:加壓單元2: pressurization unit

21:桶槽21: barrel tank

22:壓幫浦22: Pressure Pump

23:管路23: Pipeline

3:第一蒸餾單元3: The first distillation unit

31:第一蒸餾塔31: The first distillation column

32:煮沸加熱器32: Boil Heaters

4:第一冷凝單元4: The first condensing unit

41:第一冷凝器41: First condenser

42:第一再冷凝器42: First Recondenser

5:第二蒸餾單元5: Second distillation unit

51:第二蒸餾塔51: Second distillation column

52:再煮沸器52: Reboiler

6:第二冷凝單元6: The second condensing unit

61:第二冷凝器61: Second condenser

62:第二再冷凝器62: Second Recondenser

63:過冷器63: Subcooler

7:儲槽單元7: Tank unit

71:精品儲存槽71: Boutique Storage Tank

72:控壓裝置72: Pressure control device

721:壓力計721: Manometer

722:洩壓閥722: Pressure relief valve

8:再循環單元8: Recirculation unit

81:氣液儲存槽81: Gas-liquid storage tank

82:加熱器82: Heater

83:加壓幫浦83: Pressurized pump

9:氣體吸收槽9: Gas absorption tank

M:流量調節單元M: flow adjustment unit

M1~M6:流量調節閥M1~M6: Flow control valve

Claims (10)

一種氨水純化裝置,用於純化濃度介於17~23mole%的粗氨水,包含:一加熱加壓單元,用於將該粗氨水加熱加壓使該粗氨水形成壓力大於該粗氨水的相對高壓的粗氨水;一第一蒸餾單元,包括一與該加熱加壓單元連通的第一蒸餾塔,及一供該第一蒸餾塔加熱的煮沸加熱器,該第一蒸餾塔可供該相對高壓的粗氨水進行蒸餾,得到第一混合氣體及第一排放液體;一第一冷凝單元,用於冷凝該第一混合氣體,包括一與該第一蒸餾塔連通的第一冷凝器,及一位於該第一冷凝器下游的第一再冷凝器;一第二蒸餾單元,用於供通過該第一再冷凝器後得到的冷凝液體進行蒸餾,以產生第二混合氣體及廢氨液,包括一與該第一再冷凝器連通的第二蒸餾塔,及一供該第二蒸餾塔加熱的再煮沸器;一第二冷凝單元,用於冷凝該第二混合氣體,包括一與該第二蒸餾塔連通的第二冷凝器,及依序位於該第二冷凝器下游的一第二再冷凝器,及一過冷器,該過冷器接收經該第二再冷凝器冷凝後得到的液態氨並形成過冷液體;一儲槽單元,包括一與該過冷器連通,用於儲存通過該過冷器的液態氨的精品儲存槽;及 一再循環單元,包括一分別與該第一蒸餾塔及第二蒸餾塔連通的氣液儲存槽、一加熱器,及一加壓幫浦,該第二蒸餾塔的廢氨液會引入該氣液儲存槽,該加熱器及加壓幫浦供該氣液儲存槽的液體加熱以提高壓力,使其具有與該第一蒸餾塔內的粗氨水大致相同的壓力並具有飽和的氣液兩相,且該氣液儲存槽內的液相可再引入該第一蒸餾塔。 A kind of ammonia water purification device, is used for purifying the thick ammonia water that concentration is between 17~23 mole%, comprises: a heating and pressurizing unit, is used for this thick ammonia water heating and pressurizing to make this thick ammonia water form pressure is greater than the relative high pressure of this thick ammonia water Crude ammonia water; a first distillation unit, including a first distillation column communicated with the heating and pressurizing unit, and a boiling heater for heating the first distillation column, the first distillation column can be used for the relatively high pressure crude Ammonia water is distilled to obtain a first mixed gas and a first discharge liquid; a first condensation unit for condensing the first mixed gas, including a first condenser communicated with the first distillation column, and a first condenser located in the first A first recondenser downstream of the condenser; a second distillation unit for distilling the condensed liquid obtained after passing through the first recondenser to produce a second mixed gas and waste ammonia liquid, including a a second distillation column communicated with the first recondenser, and a reboiler for heating the second distillation column; a second condensing unit for condensing the second mixed gas, including a second distillation column communicated with the second distillation column a second condenser, and a second re-condenser sequentially located downstream of the second condenser, and a sub-cooler, the sub-cooler receives the liquid ammonia obtained after condensation by the second re-condenser and forms subcooled liquid; a storage tank unit including a fine storage tank in communication with the subcooler for storing liquid ammonia passing through the subcooler; and A recirculation unit, including a gas-liquid storage tank, a heater, and a pressurized pump respectively communicated with the first distillation column and the second distillation column, and the waste ammonia liquid of the second distillation column will be introduced into the gas-liquid The storage tank, the heater and the pressurized pump supply the liquid heating of the gas-liquid storage tank to increase the pressure, so that it has approximately the same pressure as the crude ammonia water in the first distillation column and has a saturated gas-liquid two-phase, And the liquid phase in the gas-liquid storage tank can be reintroduced into the first distillation column. 如請求項1所述的氨水純化裝置,還包含一與該再循環單元的氣液儲存槽連通,用於吸收自該氣液儲存槽排出之氨氣的氣體吸收槽。 The ammonia water purification device according to claim 1, further comprising a gas absorption tank communicating with the gas-liquid storage tank of the recycling unit for absorbing the ammonia gas discharged from the gas-liquid storage tank. 如請求項2所述的氨水純化裝置,其中,該儲槽單元的精品儲存槽與該氣體吸收槽連通,且該儲槽單元還包括一用以控制該精品儲存槽壓力的控壓裝置。 The ammonia water purification device according to claim 2, wherein the fine product storage tank of the storage tank unit is communicated with the gas absorption tank, and the storage tank unit further includes a pressure control device for controlling the pressure of the fine product storage tank. 如請求項2所述的氨水純化裝置,其中,該氣體吸收槽還與第一再冷凝器、第二再冷凝器,及該精品儲存槽連通,供吸收自該第一再冷凝器、第二再冷凝器,及該精品儲存槽排出之氣體。 The ammonia water purification device according to claim 2, wherein the gas absorption tank is also communicated with the first re-condenser, the second re-condenser, and the fine-quality storage tank for absorption from the first re-condenser, the second re-condenser Recondenser, and the gas discharged from the fine storage tank. 如請求項1所述的氨水純化裝置,其中,該加熱加壓單元包含一用於供容置熱媒的桶槽、一加壓幫浦,及一容置在該桶槽並可被該熱媒加熱的管路,該第一蒸餾單元與該桶槽連通,供該第一排放液體排入至該桶槽並作為該熱媒。 The ammonia water purification device according to claim 1, wherein the heating and pressurizing unit comprises a barrel for accommodating a heat medium, a pressurized pump, and a barrel that is accommodated in the barrel and can be heated by the heat The first distillation unit is communicated with the barrel tank, and the first discharge liquid is discharged into the barrel tank and used as the heat medium. 如請求項1所述的氨水純化裝置,其中,該第一蒸餾單元 的第一排放液體與該再循環單元連通並供作為該再循環單元的部份熱源。 The ammonia water purification device according to claim 1, wherein the first distillation unit The first discharge liquid of 100 is in communication with the recirculation unit and serves as part of the heat source for the recirculation unit. 一種氨水純化方法,包含:將一濃度介於17~23mole%的粗氨水溶液經由一加熱加壓單元加熱加壓後引入至一第一蒸餾單元,進行第一次蒸餾,得到一第一混合氣體及一第一排放液體;利用一第一冷凝單元將該第一混合氣體進行冷凝得到一冷凝液體及一排出氣體;將該冷凝液體引入至一第二蒸餾塔進行第二次蒸餾,得到第二混合氣體及廢氨液,並將該廢氨液透過管路回流至一再循環單元的氣液儲存槽,且該氣液儲存槽的液體可再引入該第一蒸餾塔,其中,該再循環單元包含一氣液儲存槽、一加熱器及一加壓幫浦,該方法還包含:利用該再循環單元的加熱器及加壓幫浦將該氣液儲存槽的液體加熱以提高壓力,使其具有與該第一蒸餾塔內的粗氨水相同的壓力,並引入該第一蒸餾塔;將該第二混合氣體引入至一第二冷凝單元進行冷凝,得到高壓過冷的精製液態氨;及將該精製液態氨引入至一精品儲存槽儲存。 A method for purifying ammonia water, comprising: introducing a crude ammonia solution with a concentration of 17 to 23 mole% into a first distillation unit after being heated and pressurized by a heating and pressurizing unit, and performing first distillation to obtain a first mixed gas and a first discharge liquid; use a first condensation unit to condense the first mixed gas to obtain a condensed liquid and a discharge gas; introduce the condensed liquid into a second distillation column for the second distillation to obtain a second Mix gas and waste ammonia liquid, and return the waste ammonia liquid to a gas-liquid storage tank of a recycling unit through a pipeline, and the liquid in the gas-liquid storage tank can be reintroduced into the first distillation tower, wherein the recycling unit It includes a gas-liquid storage tank, a heater and a pressurized pump, and the method also includes: using the heater and the pressurized pump of the recirculation unit to heat the liquid in the gas-liquid storage tank to increase the pressure, so that it has The same pressure as the crude ammonia water in the first distillation column is introduced into the first distillation column; the second mixed gas is introduced into a second condensing unit for condensation to obtain high-pressure subcooled refined liquid ammonia; and the Refined liquid ammonia is introduced into a fine storage tank for storage. 如請求項7所述的氨水純化方法,還包含,將該第一排放液體引入該加熱加壓單元或再循環單元的其中至少一者,並做為熱媒來源。 The ammonia water purification method according to claim 7, further comprising: introducing the first discharge liquid into at least one of the heating and pressurizing unit or the recycling unit, and using it as a heat medium source. 如請求項7所述的氨水純化方法,其中,該氨水純化裝置還包含一分別與該氣液儲存槽、第一冷凝單元、第二冷凝單元,及精品儲存槽連通的氣體吸收槽,該氨水純化方法還包含將該氣液儲存槽、第一冷凝單元、第二冷凝單元,及精品儲存槽的其中任一者對外排出之氣體透過管路引入該氣體吸收槽。 The ammonia water purification method as claimed in claim 7, wherein the ammonia water purification device further comprises a gas absorption tank respectively communicated with the gas-liquid storage tank, the first condensing unit, the second condensing unit, and the fine-quality storage tank. The purification method also includes introducing the gas discharged from any one of the gas-liquid storage tank, the first condensation unit, the second condensation unit, and the fine-quality storage tank into the gas absorption tank through a pipeline. 如請求項9所述的氨水純化方法,還包含:將該氣體吸收槽的氨水稀釋成與該粗氨水相同濃度後,透過管路引入該加熱加壓單元。 The ammonia water purification method according to claim 9, further comprising: after diluting the ammonia water in the gas absorption tank to the same concentration as the crude ammonia water, introducing it into the heating and pressurizing unit through a pipeline.
TW109112064A 2020-04-09 2020-04-09 Ammonia purification apparatus and purification method TWI773979B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20010010286A1 (en) * 2000-02-01 2001-08-02 Karl-Heinz Wostbrock Purification of ammonia by distillation
TWM533642U (en) * 2016-07-14 2016-12-11 Asia An Technics Co Ltd Electronic grade ammonia hydroxide manufacture system
TWI580638B (en) * 2016-05-26 2017-05-01 隆達電子股份有限公司 Ammonia concentration increment system and method thereof
CN110436545A (en) * 2019-07-16 2019-11-12 临涣焦化股份有限公司 A kind of remained ammonia distilling apparatus of heat energy recycling

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20010010286A1 (en) * 2000-02-01 2001-08-02 Karl-Heinz Wostbrock Purification of ammonia by distillation
TWI580638B (en) * 2016-05-26 2017-05-01 隆達電子股份有限公司 Ammonia concentration increment system and method thereof
TWM533642U (en) * 2016-07-14 2016-12-11 Asia An Technics Co Ltd Electronic grade ammonia hydroxide manufacture system
CN110436545A (en) * 2019-07-16 2019-11-12 临涣焦化股份有限公司 A kind of remained ammonia distilling apparatus of heat energy recycling

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