TWI586842B - Plant for fluorine production and a process using it - Google Patents

Plant for fluorine production and a process using it Download PDF

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TWI586842B
TWI586842B TW100130272A TW100130272A TWI586842B TW I586842 B TWI586842 B TW I586842B TW 100130272 A TW100130272 A TW 100130272A TW 100130272 A TW100130272 A TW 100130272A TW I586842 B TWI586842 B TW I586842B
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slider
factory
plant
gas
sliding
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TW201224218A (en
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菲立普 摩瑞里
歐利維羅 迪安那
彼德 普里狄肯特
喬勤 蘭吉
霍革 皮尼斯
法蘭西斯 費思
亞連 弗貝雷茲
莫瑞里歐 帕根尼
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首威公司
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • C25B1/24Halogens or compounds thereof
    • C25B1/245Fluorine; Compounds thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/68Halogens or halogen compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/19Fluorine; Hydrogen fluoride
    • C01B7/20Fluorine
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00Operating or servicing cells
    • C25B15/02Process control or regulation
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00Operating or servicing cells
    • C25B15/08Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases
    • Y02C20/30Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Description

氟之製造工廠及使用彼之方法Fluorine manufacturing plant and method of using the same

本發明要求於2010年9月15日提交的美國臨時專利申請號61/383204以及於2010年9月16日提交的美國臨時專利申請號61/383533的優先權,該等申請的全部內容出於所有的目的藉由引用結合在此,本發明涉及一種處於多個組裝的滑動件的形式用於氟生產的工廠以及其中應用它的一方法。The present invention claims the priority of U.S. Provisional Patent Application No. 61/383,204, filed on Sep. 15, 2010, and U.S. Provisional Patent Application No. 61/383,533, filed on Sep. All of the objects are hereby incorporated by reference, the present invention relates to a factory for the production of fluorine in the form of a plurality of assembled slides and a method in which it is applied.

在半導體、光伏達電池、薄膜電晶體(TFT)液晶顯示器、以及微機電系統(MEMS)的製造過程中,經常在合適的腔室中進行連續沉積材料的多個步驟以及蝕刻對應的物品;該等過程通常是等離子體輔助的。在該沉積步驟中,沉積物不僅經常在該物品上形成而且還在該腔室的該等壁和其他多個內部零件上形成。據觀察元素氟係一非常有效的試劑既用於蝕刻又用於清潔該等腔室以去除不希望的沉積物。此類方法例如在WO 2007/116033(它說明了使用氟和某些混合物作為蝕刻劑和腔室清潔劑)、WO 2009/080615(它說明了MEMS的製造)、2009/092453(它說明了太陽能電池的製造)中,並且在未公開的歐洲申請09174034.0(它涉及TFT的製造)中進行了說明。In the fabrication of semiconductors, photovoltaic cells, thin film transistor (TFT) liquid crystal displays, and microelectromechanical systems (MEMS), multiple steps of continuously depositing materials and etching corresponding articles are often performed in suitable chambers; The processes are usually plasma assisted. In this deposition step, deposits are not only often formed on the article but also on the walls and other interior parts of the chamber. It has been observed that the elemental fluorine-based very effective reagent is used both for etching and for cleaning the chambers to remove undesirable deposits. Such methods are for example in WO 2007/116033 (which describes the use of fluorine and certain mixtures as etchants and chamber cleaners), WO 2009/080615 (which illustrates the manufacture of MEMS), 2009/092453 (which illustrates solar energy) The manufacture of batteries is described in the unpublished European application 09174034.0, which relates to the manufacture of TFTs.

美國專利申請描述了一製造設施中氟的產生以及分配。現場提供氟減少了與從一產生氟的設施中將其運輸到使用點的相關的風險。U.S. Patent Application describes the production and distribution of fluorine in a manufacturing facility. The provision of fluoride on site reduces the risks associated with transporting it from a facility that produces fluorine to a point of use.

仍然存在很多與現場構思中使用的裝置相相關的有待解決的問題,例如,在漏泄、或者設備破壞的情況下更大量的純氟(F2)和HF的銷毀。There are still many problems to be solved related to the devices used in the on-site concept, such as the destruction of a larger amount of pure fluorine (F 2 ) and HF in the event of leakage or equipment damage.

本發明提供一改進的工廠適合用於現場產生氟特別用作在半導體、光伏達電池、薄膜電晶體液晶顯示器、以及微機電系統的製造中的蝕刻劑以及腔室清潔劑。The present invention provides an improved plant suitable for use in the field of fluorine production, particularly as an etchant and chamber cleaner in the fabrication of semiconductors, photovoltaic cells, thin film transistor liquid crystal displays, and microelectromechanical systems.

本發明的工廠向一工具提供氟氣體,該工具應用氟氣體作為反應物來在該裝置中進行化學作用,該裝置包括多個滑動安裝模組,其中包括至少一個選自下組的滑動安裝模組,該組的組成為The plant of the present invention supplies a tool to a fluorine gas that uses fluorine gas as a reactant to chemically act in the apparatus, the apparatus comprising a plurality of sliding mounting modules including at least one sliding mounting die selected from the group consisting of Group, the composition of the group is

- 包括至少一個HF儲存槽之滑動安裝模組,表示為滑動件1,- a sliding mounting module comprising at least one HF storage tank, represented as a slide 1,

- 包括至少一個產生F2的電解池之滑動安裝模組,表示為滑動件2,- the installation comprises at least one sliding module of the cell F 2, showing the sliding member 2,

- 包括用於純化F2的純化裝置之滑動安裝模組,表示為滑動件3,- a sliding mounting module comprising a purification device for purifying F 2 , represented as a slide 3,

-包括將氟氣體遞送到使用點的裝置之滑動安裝模組,表示為滑動件4,a sliding mounting module comprising means for delivering fluorine gas to the point of use, designated as slide 4,

- 包括冷卻水迴路之滑動安裝模組,表示為滑動件5,- a sliding mounting module comprising a cooling water circuit, represented as a slide 5,

- 包括處理廢氣的裝置之滑動安裝模組,表示為滑動件6,- a sliding mounting module comprising means for treating exhaust gases, represented as a slide 6,

- 包括用於分析F2的裝置之滑動安裝模組,表示為滑動件7,以及- mounting module comprising means for analyzing the slide F 2, showing the sliding member 7, and

- 包括操作該等電解池的裝置之滑動安裝模組,表示為滑動件8。- A sliding mounting module comprising means for operating the electrolytic cells, designated as a slider 8.

本發明的較佳的工廠向一工具提供氟氣體,該工具應用氟氣體作為反應物來在該工具中進行化學作用,該裝置包括多個滑動安裝模組,其中包括以下各項:The preferred plant of the present invention provides a gas to a tool that uses fluorine gas as a reactant to chemically act in the tool. The device includes a plurality of sliding mounting modules including the following:

- 包括至少一個HF儲存槽之滑動安裝模組,表示為滑動件1,- a sliding mounting module comprising at least one HF storage tank, represented as a slide 1,

- 包括至少一個產生F2的電解池之滑動安裝模組,表示為滑動件2,- the installation comprises at least one sliding module of the cell F 2, showing the sliding member 2,

- 包括用於純化F2的純化裝置之滑動安裝模組,表示為滑動件3,- a sliding mounting module comprising a purification device for purifying F 2 , represented as a slide 3,

- 包括將氟氣體遞送到使用點的裝置之滑動安裝模組,表示為滑動件4,- a sliding mounting module comprising means for delivering fluorine gas to the point of use, designated as slide 4,

- 包括冷卻水迴路之滑動安裝模組,表示為滑動件5,- a sliding mounting module comprising a cooling water circuit, represented as a slide 5,

- 包括處理廢氣的裝置之滑動安裝模組,表示為滑動件6,- a sliding mounting module comprising means for treating exhaust gases, represented as a slide 6,

- 包括用於分析F2的裝置之滑動安裝模組,表示為滑動件7,以及- mounting module comprising means for analyzing the slide F 2, showing the sliding member 7, and

- 包括操作該等電解池的裝置之滑動安裝模組,表示為滑動件8。- A sliding mounting module comprising means for operating the electrolytic cells, designated as a slider 8.

該工廠較佳的是還包括滑動件式模組,該等模組可以位於滑動件式模組1至8的附近但是可以與它們分開,即Preferably, the factory further includes a slider module, which may be located adjacent to the slider modules 1 to 8 but may be separated therefrom, ie

- 滑動件模組9,其係將中電壓轉化成低電壓之變電站,和/或- a slider module 9, which converts the medium voltage into a low voltage substation, and/or

- 滑動件模組10,其將實用設施(控制室、實驗室、休息室)容納在內。- Sliding module 10, which houses utility facilities (control room, laboratory, lounge).

此外,該裝置可以包括用於供應惰性氣體的裝置,例如用於提供液氮以及氣氮的裝置:用於提供壓縮的空氣以及水的裝置;以及輔助品和便利設施。至少,滑動件1、2、3、4以及7,較佳的是所有滑動件,包括為了安全原因的殼體。Furthermore, the apparatus may comprise means for supplying an inert gas, such as means for providing liquid nitrogen and gaseous nitrogen: means for providing compressed air and water; and aids and amenities. At least, the sliders 1, 2, 3, 4 and 7, preferably all sliders, including the housing for safety reasons.

在本發明的背景中,術語“氟氣體”具體地是指分子氟(F2)以及其的多種混合物(特別是與惰性氣體)。惰性氣體較佳的是例如選自:氬氣、氮氣、氧氣、以及N2O。一較佳的氟氣體由或者主要由F2組成。In the context of the present invention, the term "fluorine gas" specifically refers to molecular fluorine (F 2 ) and various mixtures thereof (particularly with inert gases). The inert gas is preferably selected, for example, from the group consisting of argon, nitrogen, oxygen, and N 2 O. A preferred fluorine gas consists of or consists essentially of F 2 .

以下,詳細地說明了圖1中所示的一較佳的工廠。Hereinafter, a preferred factory shown in Fig. 1 will be described in detail.

圖1示出了根據本發明的一工廠P。其尺寸係39 m×23 m。圖1中的參考號1表示包括了HF儲存和蒸發的滑動件1。參考號2表示了由一虛線表示的滑動件2,它包括該等電解池;它位於模組5和7下面的工廠地下室中。圖1的參考號3係指滑動件3,它包括對所生產的F2進行純化的純化裝置。圖1的參考號4表示滑動件4,它包括用於氟氣體的儲存裝置。根據一實施方式,滑動件4還包括對備用的或者最終儲存的純化的F2的最終分析的一單槽FT-IR。圖1的參考號5表示滑動件5,它容納了冷卻水的裝置。它位於滑動件2的上面。圖1中的參考號6A係指滑動件6A,它包含應急回應滌氣器ERS,並且參考號6B表示帶有F2滌氣器和H2滌氣器的滑動件6B。圖1中的參考號7表示滑動件7,它包括可隨意的用於F2分析的裝置(它可以例如包含一FT-IR和/或一紫外光譜儀)。圖1中的參考號8係指滑動件8中的整流器盒(cabinet)。參考號9A和9B係指中電壓電的子滑動件9A和低電壓電的子滑動件9B。參考號10A表示包括一實驗室以及一控制室的滑動件10A,參考號10B係指帶有多個的舒適設施(像休息室以及更衣室)的滑動件10B。參考號11a和11b表示用於步行以便到達上層的滑動件(尤其是滑動件5和7)的自動扶梯和平臺。參考號12示出了活動中的叉式起重機。參考號13表示一用於KOH溶液以及其他所需化學品的貯料場,並且參考號14係指一應急淋浴器。如果希望的話,該工廠可以用圍欄圍起,如圖1中的黑線所指示的。一有圍欄的工廠具有多個優點,因為避免了對沒有預見的操作F2生產工廠的工作人員進入其中,因此降低了對該等工作人員的風險。在這種情況下,該氟氣體工廠可以在消耗該氟氣體的半導體製造工廠的現場進行構建,並且氟氣體的遞送越過該圍欄而發生。Figure 1 shows a factory P in accordance with the present invention. Its size is 39 m × 23 m. Reference numeral 1 in Fig. 1 denotes a slider 1 including HF storage and evaporation. Reference numeral 2 denotes a slider 2, indicated by a broken line, which comprises the electrolytic cells; it is located in the factory basement below the modules 5 and 7. Reference numeral 3 of Fig. 1 denotes a slider 3 which comprises a purifying device for purifying the produced F 2 . Reference numeral 4 of Fig. 1 denotes a slider 4 which includes a storage device for fluorine gas. According to one embodiment, the slide 4 further comprises a single slot FT-IR analysis of the final spare or final storage of purified F 2. Reference numeral 5 of Fig. 1 denotes a slider 5 which houses means for cooling water. It is located above the slider 2. Reference numeral 6A in Fig. 1 denotes a slider 6A which includes an emergency response scrubber ERS, and reference numeral 6B denotes a slider 6B with an F 2 scrubber and a H 2 scrubber. In Figure 1 reference numeral 7 denotes a sliding member 7, comprising means F 2 can be freely used for analysis (which may comprise, for example, a FT-IR and / or a UV spectrometer). Reference numeral 8 in Fig. 1 refers to a rectifier box in the slider 8. Reference numerals 9A and 9B refer to a medium voltage electric sub-slider 9A and a low voltage electric sub-slider 9B. Reference numeral 10A denotes a slider 10A including a laboratory and a control room, and reference numeral 10B denotes a slider 10B having a plurality of comfort facilities such as a restroom and a dressing room. Reference numerals 11a and 11b denote escalators and platforms for walking to reach the upper sliding members (especially the sliding members 5 and 7). Reference numeral 12 shows the forklift in action. Reference numeral 13 denotes a stockyard for the KOH solution and other required chemicals, and reference numeral 14 denotes an emergency shower. If desired, the plant can be fenced, as indicated by the black line in Figure 1. A fenced facility has several advantages, since the staff to avoid unforeseen operation into the F 2 production facility wherein, thus reducing the risk of the staff and the like. In this case, the fluorine gas plant can be constructed on site at a semiconductor manufacturing plant that consumes the fluorine gas, and delivery of fluorine gas occurs over the fence.

包括在幾個滑動件中所組裝的多個零件的這樣一工廠具有許多優點。例如,該等滑動件可以在一設備中進行預組裝並且測試;因此,它們係一“現成的”產品並且僅需要在現場安裝。這節省了時間。拆卸多個特定的滑動件以便維護、維修、或者由其他滑動件(它們包括具有相同的功能但具有改進的性能的零件,或者具有更低或者更高的輸出)替代也是非常容易的。安全上還存在多種改進:例如,如以上說明的,滑動件2包括至少一個電解池;較佳的是,所有的電解池係已經填充了電解質的並且然後被遞送到現場用於組裝到滑動件2中。因此,該填充可以在對應的安全考慮下進行,並且不必在一局部的位置上進行,在這個地方這種安全預防措施可能不是可獲得的。該工廠的容量可以藉由添加模組來進行擴展。較佳的是,該等滑動件具有海運集裝箱的尺寸,因此允許很容易地運輸模組。一很大的優點係每週7天每天24小時的高純度F2的可靠的生產。Such a plant comprising a plurality of parts assembled in several sliders has many advantages. For example, the sliders can be pre-assembled and tested in a device; therefore, they are a "off the shelf" product and only need to be installed in the field. This saves time. It is also very easy to disassemble a plurality of specific sliders for maintenance, repair, or replacement by other sliders, which include parts having the same function but with improved performance, or having a lower or higher output. There are also a number of improvements in safety: for example, as explained above, the slider 2 comprises at least one electrolytic cell; preferably, all of the electrolytic cells have been filled with electrolyte and then delivered to the field for assembly to the slide 2 in. Thus, the filling can be carried out under corresponding safety considerations and does not have to be performed at a local location where such safety precautions may not be available. The capacity of the plant can be expanded by adding modules. Preferably, the sliders are of the size of a shipping container, thus permitting easy transport of the module. A great advantage is the reliable production of high purity F 2 24 hours a day, 7 days a week.

現在將詳細地來說明該等滑動件。The sliders will now be described in detail.

總體上較佳的是該等池係成塊的並且連接到該結構上以避免移動,例如作為一地震保護。還較佳的是,該工廠包括檢測地震並且給控制室發出信號的裝置,該控制室將該設備自動關閉或者個人手動關閉。較佳的是,該工廠包括至少一台地震檢波器,例如強地動的地震檢波器(加速度測量儀)它可以檢測該設備的振動加速,並且如果達到了一水平,例如0.5 G,的話就發送一對應的信號,該信號觸發了一警報和/或該設備的一自動關閉。It is generally preferred that the cells are lumped and attached to the structure to avoid movement, for example as a seismic protection. It is also preferred that the plant includes means for detecting an earthquake and signaling the control room that automatically shuts down the device or manually shuts it down manually. Preferably, the plant includes at least one geophone, such as a geodetic geophone (accelerometer) that detects vibration acceleration of the device and transmits if a level, such as 0.5 G, is reached. A corresponding signal that triggers an alarm and/or an automatic shutdown of the device.

所有連接該等池的並且連接到該等池上的管線必須是電絕緣的,例如藉由多個凸緣之間的隔離件。地板也必須是電絕緣的。All lines connecting the cells and connected to the cells must be electrically insulating, for example by spacers between the plurality of flanges. The floor must also be electrically insulated.

較佳的是,所有的進程滑動件(滑動件1至8)係包括在一封閉的空間中的。Preferably, all of the process sliders (sliders 1 to 8) are included in a closed space.

滑動件1:用於HF儲存的滑動件模組(滑動件1)包括至少一個HF(氟化氫)儲存槽,該儲存槽用於儲存HF並且將其遞送到該等電解池。用於HF的儲罐總體上是空心體,該等空心體可隨意地可以被安裝在多個輪子上或者它們可以例如藉由一升降叉車來進行運輸。較佳的是,該滑動件包括幾個儲罐,更佳的是2、3、4、5或6個儲罐。較佳的是,該HF係以液體形式儲存在該罐中的。滑動件1係可連接到一包括加壓的N2的罐中的。液體HF係用N2加壓的並且被遞送到一蒸發器中,在該蒸發器中它被蒸發了。所生成的包含HF的氣相被遞送到這個電解池或者該等電解池中。如果希望的話,對於每一電解池可以安裝一蒸發器。Slide 1: The slider module for HF storage (slider 1) includes at least one HF (hydrogen fluoride) storage tank for storing HF and delivering it to the electrolytic cells. The tanks for HF are generally hollow bodies which can optionally be mounted on a plurality of wheels or they can be transported, for example, by a forklift. Preferably, the slider comprises several storage tanks, more preferably 2, 3, 4, 5 or 6 storage tanks. Preferably, the HF is stored in the tank in liquid form. The slider 1 is connectable to a can comprising pressurized N 2 . HF-based liquid pressurized with N 2 and is delivered to an evaporator, in which the evaporator is evaporated. The resulting gas phase containing HF is delivered to this electrolytic cell or to such electrolytic cells. If desired, an evaporator can be installed for each cell.

蒸發器較佳的是包含一加熱裝置,例如一電加熱裝置或者一熱交換器(使用熱冷卻水的熱量)以便產生該蒸發的HF。更佳的是,該HF儲存容器可以藉由具有一封閉的隔離空間的雙隔離閥而與該HF供應線隔離開。在那種情況下,滑動件1適合地進一步包括至少一個與一或多個封閉的隔離空間相連接的空隙通氣閥。該空隙通氣閥總體上是可操作的以便從該封閉的隔離空間中可隨意地除去所存在的氟化氫。去除可以例如藉由施加真空來進行。在另一方面,去除可以例如藉由使用一惰性氣體和/或一加壓的清掃氣體(例如像無水的空氣,較佳的是氮氣)來沖洗該封閉的隔離空間而進行。The evaporator preferably comprises a heating means such as an electric heating means or a heat exchanger (heat using hot cooling water) to produce the evaporated HF. More preferably, the HF storage container can be isolated from the HF supply line by a dual isolation valve having a closed isolation space. In that case, the slider 1 suitably further comprises at least one gap venting valve connected to the one or more enclosed spaces. The gap vent valve is generally operable to freely remove hydrogen fluoride present from the enclosed isolation space. Removal can be performed, for example, by applying a vacuum. In another aspect, the removal can be performed, for example, by rinsing the enclosed isolated space using an inert gas and/or a pressurized sweeping gas (e.g., like anhydrous air, preferably nitrogen).

在一方面,去除係連續進行的。In one aspect, the removal is performed continuously.

較佳的是,去除係不連續進行的,特別是當一HF儲存容器係連接到供應線上和/或與其斷開連接的時候。從該封閉的隔離空間中回收的氣體適當地被放出至一HF銷毀單元中,例如滑動件6中的一滌氣器。Preferably, the removal is discontinuous, particularly when an HF storage container is attached to and/or disconnected from the supply line. The gas recovered from the enclosed isolated space is suitably discharged to an HF destruction unit, such as a scrubber in the slide 6.

在根據本發明的工廠中,其多個零件(被假定與氣體相接觸),例如像,如果適當的話,空心體、閥門、以及用於裝料和/或排出氣體的管線,是用耐分子氟的材料來適合地製成的或者塗覆有這種材料。此類材料的實例包括蒙乃爾合金金屬、不銹鋼、銅,以及較佳的是,鎳。In a plant according to the invention, a plurality of parts thereof (presumed to be in contact with a gas), such as, for example, hollow bodies, valves, and lines for charging and/or venting gases, are resistant to molecules Fluorine materials are suitably made or coated with such materials. Examples of such materials include Monel metal, stainless steel, copper, and, preferably, nickel.

在滑動件1的一較佳的方面,氟化氫儲存容器被包含在一封閉式的空間中,該封閉式的空間具有至少一個可關閉的門,該可關閉的門允許一氟化氫儲存容器從該封閉的空間進入或者或移除。在這個方面的一實施方式中,該封閉式的空間包含該等氟化氫儲存容器以及到該氟化氫供應管線上的連接件。在另一實施方式中,該封閉式的空間此外包含一用於蒸發液體HF的蒸發器。在這個較佳的方面以及它的實施方式中,該封閉式的空間適合地包括一HF感測器,該HF感測器能夠觸發該封閉的空間到以下所說明的一滌氣器上的連接。In a preferred aspect of the slider 1, the hydrogen fluoride storage container is contained in a closed space having at least one closable door that allows a hydrogen fluoride storage container to be closed from the The space enters or is removed. In an embodiment of this aspect, the enclosed space comprises the hydrogen fluoride storage container and a connection to the hydrogen fluoride supply line. In a further embodiment, the enclosed space further comprises an evaporator for evaporating the liquid HF. In this preferred aspect, and in its embodiment, the enclosed space suitably includes an HF sensor capable of triggering the enclosed space to a connection on a scrubber as described below. .

滑動件1總體上具有至少一根液體管線以及一根氣體管線。在那種情況下,該液體管線可以連接(如果適當的話)到該氟化氫供應管線上,例如藉由一凸緣連接。該氣體管線另外可以連接到一惰性氣體(例如,無水的空氣、氮氣,等)供應管線上,它允許對氟化氫儲存容器進行加壓。The slider 1 generally has at least one liquid line and one gas line. In that case, the liquid line can be connected, if appropriate, to the hydrogen fluoride supply line, for example by a flange connection. The gas line may additionally be connected to an inert gas (e.g., anhydrous air, nitrogen, etc.) supply line which allows for pressurization of the hydrogen fluoride storage vessel.

在滑動件1中,每個氟化氫儲存容器總體上具有從10到5000升、通常500到4000升、較佳的是從500到3000升的容量。氟化氫儲存容器的具體實例係由RID/ADR-IMDG認可的罐,UN T22類型或較佳的是UN T20類型。此類罐係可商購的。In the slider 1, each of the hydrogen fluoride storage containers has a capacity of generally from 10 to 5,000 liters, usually from 500 to 4,000 liters, preferably from 500 to 3,000 liters. A specific example of a hydrogen fluoride storage container is a tank approved by RID/ADR-IMDG, of the UN T22 type or preferably of the UN T20 type. Such cans are commercially available.

滑動件1中的每個HF儲存容器可以通過一歧管被適當地連接到氟化氫供應管線上。Each of the HF storage containers in the slider 1 can be suitably connected to the hydrogen fluoride supply line through a manifold.

滑動件1中的每個HF儲存容器較佳的是與氟化氫供應管線單獨可隔離的。Each of the HF storage containers in the slider 1 is preferably separately separable from the hydrogen fluoride supply line.

滑動件1中的HF儲存容器可以總體上與氟化氫供應管線藉由一遙控裝置、較佳的是一遙控閥來分離。更佳的是,每個儲存容器配備有一遙控裝置、較佳的是一遙控閥,允許將容器與氟化氫供應管線分離。The HF storage container in the slider 1 can be generally separated from the hydrogen fluoride supply line by a remote control, preferably a remote control valve. More preferably, each storage container is provided with a remote control, preferably a remote control valve, which allows the container to be separated from the hydrogen fluoride supply line.

當存在遙控閥時,另外適當地安裝手動閥。該等遙控閥例如允許從一遙控室操作該HF儲存容器。When a remote control valve is present, a manual valve is additionally installed. Such remote control valves, for example, allow operation of the HF storage container from a remote control room.

在一較佳的實施方式中,該等HF儲存容器包括一自動的HF水平感測器。具體地,該等HF儲存容器可以被安裝在磅秤上。在那種情況下,較佳的是,一過程處理系統、具體一自動程序控制系統係可操作的以關閉一第一遙控閥、將HF容器排空的並且打開另一第二含HF氟化氫儲存容器的遙控閥。這個實施方式對於避免HF閥的手動操作並且對於確保持續的HF供應是特別有效的。In a preferred embodiment, the HF storage containers include an automatic HF level sensor. In particular, the HF storage containers can be mounted on a scale. In that case, preferably, a process processing system, specifically an automatic program control system, is operable to close a first remote control valve, evacuate the HF vessel, and open another second HF-containing hydrogen fluoride storage. Remote valve for the container. This embodiment is particularly effective for avoiding manual operation of the HF valve and for ensuring a continuous HF supply.

在一較佳的方面,該等閥係可操作的以在異常操作狀態的情況下(例如與HF供應管線相連接的一過程設備中的一過程中斷)自動關閉。In a preferred aspect, the valves are operable to automatically close in the event of an abnormal operating condition (e.g., a process interruption in a process equipment coupled to the HF supply line).

在另一較佳的方面,該等閥係可操作的以在滑動件1中的HF洩漏情況下自動關閉。這種HF洩漏可能例如由HF儲存容器內部的可隨意的凸緣連接的洩漏而引起,存在藉由遙控來關閉該等閥的可能性。這具體避免了在這種情況下接近氟化氫供應管線的必要性。In another preferred aspect, the valves are operable to automatically close in the event of an HF leak in the slider 1. Such HF leakage may be caused, for example, by leakage of a freely flanged connection inside the HF storage container, and there is a possibility that the valves are closed by remote control. This specifically avoids the necessity of approaching the hydrogen fluoride supply line in this case.

該滑動件還包括閥門用於關掉HF和氮的供應。較佳的是,滑動件1包括3到10個HF容器;特別佳的是,它包括4、5、6、7或8個容器。對於150噸F2/年的生產率,4個HF容器係適合的。特別地,具有更小尺寸的罐(如果它們可以藉由單獨的閥門來關閉)改進了工廠的安全性。該等罐可以由耐受HF的材料製成或至少內襯耐受HF的材料。該等壁應該是足夠厚的;較佳的是,它們具有10 mm IMDG碼(國際海運危險貨物規則)等值的厚度。The slider also includes a valve for shutting off the supply of HF and nitrogen. Preferably, the slider 1 comprises from 3 to 10 HF containers; particularly preferably, it comprises 4, 5, 6, 7 or 8 containers. For a productivity of 150 tons F 2 /year, 4 HF containers are suitable. In particular, tanks with smaller sizes (if they can be closed by separate valves) improve plant safety. The cans may be made of a material that is resistant to HF or at least lined with a material that is resistant to HF. The walls should be thick enough; preferably, they have a thickness equivalent to a 10 mm IMDG code (International Maritime Dangerous Goods Code).

在一具體實施方式中,滑動件1較佳的是永久性包括至少一個HF緊急情況容器。這種HF緊急情況容器較佳的是一較佳的是連接到HF供應管線上的如在此所述的空的HF儲存容器。該HF緊急情況容器通常是可操作的以接收來自一洩漏HF儲存容器的HF。將該HF緊急情況容器適當地保持在一惰性氣體壓力下或保持在真空下。In a specific embodiment, the slider 1 preferably permanently includes at least one HF emergency container. Preferably, such an HF emergency container is an empty HF storage container as described herein attached to the HF supply line. The HF emergency container is typically operable to receive HF from a leaking HF storage container. The HF emergency container is suitably maintained under an inert gas pressure or maintained under vacuum.

該等罐較佳的是可便攜的從而它們可以由貨車來運輸和/或可以由一叉形起重機來舉起。The cans are preferably portable so that they can be transported by trucks and/or can be lifted by a forklift.

滑動件1包括一通風系統,並且環境空氣較佳的是永久地通氣到一滌氣器、特別是用於去除HF和F2(如以下所述)的ERS滌氣器。The slider 1 includes a ventilation system, and the ambient air is preferably permanently vented to a scrubber, particularly an ERS scrubber for removing HF and F 2 (as described below).

滑動件2:現在詳細地對包括電解池2個或更多個電解池的滑動件(滑動件2)進行描述。它包含至少一個電解池。較佳的是,它包含至少兩個電解池。更佳的是,它包含至少6個電解池。具有8個電解池的一滑動件2係非常適合的。該滑動件較佳的是構造為使得(如果希望的話)若氟氣體的需要增加時可以增加另外的電解池。該等池包括多個夾套,可以穿過它們循環冷卻水。如果希望的話,滑動件2能以單獨的子滑動件2A、2B等形式被提供。在該等子滑動件中,組裝了確定數量的電解池。將單獨的子滑動件2A和2B(以及任何其他的子滑動件)連接到一起以形成一電解池室。通常,該電解池室將包含4個、6個或更多個電解池,例如8個電解池或甚至更多。提供若干個電解池的優點在於為了維護或修理而進行的一或甚至多個池的關閉可以藉由提高其他池的輸出而進行補償。為了組裝若干子滑動件具有的優點係,尺寸可以保持在用於平常道路運輸的可允許的最大尺寸之內。將該等電解池連接到用於產生的F2和H2的收集器上。應該注意到,每個池可以包括1個或多個陽極。典型地,每個池包括20至30個陽極。在其他實施方式中,該等電解池的每個中陽極的數目可以是大於30;每個池可以例如具有多於60個陽極,多達70個或者甚至多達80個陽極。一電纜將每個陽極與該整流器連接。每個電解池陰極通過一銅或鋁匯流線連接到該整流器上。一整流器可以向一或多個池供應電流。較佳的是每個陽極應用一整流器。優點係,取決於具體的陽極特徵,在每個單獨的陽極處的強度可以被微調,在一具體陽極處的異常情況(例如,過電壓、短路、或壞掉的陽極)可以被立即檢測,從而允許在所有氣體陽極和電解池繼續產生F2的同時自動關掉有故障的陽極。因此,滑動件2較佳的是包括帶有多個陽極的至少4個電解池,其中滑動件8中的多個整流器中的每個係分配給一個單一的陽極,或者其中滑動件8中的多個雙整流器中的每個係分配給兩個陽極的。Slide 2: The slider (slider 2) including the electrolytic cell 2 or more electrolytic cells will now be described in detail. It contains at least one electrolytic cell. Preferably, it comprises at least two electrolytic cells. More preferably, it contains at least 6 electrolytic cells. A slider 2 with 8 electrolytic cells is very suitable. The slider is preferably constructed such that, if desired, additional electrolytic cells can be added if the need for fluorine gas is increased. The pools include a plurality of jackets through which cooling water can be circulated. If desired, the slider 2 can be provided in the form of separate sub-sliders 2A, 2B and the like. In the sub-sliders, a determined number of electrolytic cells are assembled. The individual sub-sliders 2A and 2B (and any other sub-sliders) are joined together to form an electrolytic cell chamber. Typically, the cell compartment will contain 4, 6 or more electrolytic cells, such as 8 electrolytic cells or even more. The advantage of providing several electrolytic cells is that the closure of one or even more of the cells for maintenance or repair can be compensated by increasing the output of the other cells. In order to assemble several sub-sliders, the advantages are that the dimensions can be maintained within the maximum allowable size for normal road transport. The electrolytic cells are connected to a collector for the F 2 and H 2 produced. It should be noted that each cell may include one or more anodes. Typically, each cell comprises between 20 and 30 anodes. In other embodiments, the number of anodes in each of the electrolytic cells may be greater than 30; each cell may, for example, have more than 60 anodes, up to 70 or even up to 80 anodes. A cable connects each anode to the rectifier. The cathode of each cell is connected to the rectifier via a copper or aluminum bus. A rectifier can supply current to one or more cells. Preferably, a rectifier is applied to each anode. The advantage is that depending on the specific anode characteristics, the intensity at each individual anode can be fine-tuned, and anomalies at a particular anode (eg, overvoltage, short circuit, or broken anode) can be detected immediately, while continuing to produce F 2 so as to allow all of the gas in the anode and the electrolytic cell anode off automatically faulty. Accordingly, the slider 2 preferably includes at least four electrolytic cells with a plurality of anodes, wherein each of the plurality of rectifiers in the slider 8 is assigned to a single anode, or wherein the slider 8 Each of the plurality of dual rectifiers is assigned to two anodes.

滑動件2包括一冷卻水迴路(由滑動件5的冷卻水迴路來進料或者連接到其上),該冷卻水迴路供應冷卻水到該等池的夾套中。The slider 2 includes a cooling water circuit (either fed or connected thereto by a cooling water circuit of the slider 5) that supplies cooling water into the jacket of the cells.

滑動件2還包括一沉降箱;較佳的是,將一用於F2的沉降箱和一用於H2的沉降箱與每個池相連。該等沉降箱用來減小池中產生的F2和H2的氣體速度,以避免電解質粉塵被帶走。較佳的是,該等沉降箱包括一振動器以及一加熱裝置來熔化該等分離的電解質粉塵以便於去除。The slider 2 also includes a settling tank; preferably, a settling tank for F 2 and a settling tank for H 2 are connected to each tank. These settling tanks are used to reduce the gas velocity of the F 2 and H 2 produced in the tank to prevent the electrolyte dust from being carried away. Preferably, the settling tanks include a vibrator and a heating device to melt the separated electrolyte dust for removal.

收集所產生的F2的收集器係通過一管與滑動件3相連的,用於產生的H2的收集器係通過一管與滑動件6B(這將在以下詳細描述)中的對於H2的一滌氣器相連的。在一較佳的實施方式中,滑動件2還包括一通風系統以處理F2和/或H2的事故性釋放。The collector for collecting the generated F 2 is connected to the slider 3 through a tube, and the collector for generating H 2 is passed through a tube and slider 6B (which will be described in detail below) for H 2 A scrubber is connected. In a preferred embodiment, the slider 2 also includes a ventilation system to handle the accidental release of F 2 and/or H 2 .

滑動件2的環境空氣係與一滌氣器通氣的,特別是出於安全原因的ERS滌氣器(以下描述了該滌氣器)。The ambient air of the slide 2 is vented with a scrubber, especially for safety reasons (the scrubber is described below).

滑動件3:它包括用於純化所產生的F2的裝置。它包括一冷卻器,其中將F2預冷卻。滑動件3還包括一HF洗滌器,其中預冷卻的F2與保持在非常低溫度下的HF進行接觸。該HF洗滌器包括一冷卻夾套,一冷卻劑循環穿過該夾套。滑動件3進一步包括一緩衝罐、一壓縮機,例如一隔膜壓縮機、以及在低溫下操作的一HF冷凝器以及至少一HF吸收劑管柱,較佳的是含有NaF作為用於HF的吸收劑。較佳的是,至少兩個吸收劑管柱包含在滑動件3中。如果希望的話,該等吸附柱係多餘的從而一組係在吸收模式,另一組可以進行再生。該等吸附柱包括一加熱裝置。如果希望的話,另一組的吸收劑管柱可以存在於滑動件3中或在用於再裝入吸附劑的位置上。通過多個管將該HF冷凝器連接到電解滑動件2上。較佳的是,至少一組柱安裝在一有輪的推車上以保持它們從該滑動件可移動(可去除)。Slider 3: which comprises purifying the means for generating the F 2. It includes a cooler in which F 2 is pre-cooled. The slider 3 also includes an HF scrubber in which the pre-cooled F 2 is contacted with HF maintained at a very low temperature. The HF scrubber includes a cooling jacket through which a coolant circulates. The slider 3 further includes a buffer tank, a compressor such as a diaphragm compressor, and an HF condenser operating at a low temperature and at least one HF absorbent column, preferably containing NaF as an absorption for HF. Agent. Preferably, at least two absorbent column columns are contained in the slider 3. If desired, the columns are superfluous so that one group is in absorption mode and the other group can be regenerated. The adsorption columns include a heating device. If desired, another set of absorbent cartridges may be present in the slider 3 or at a location for reloading the adsorbent. The HF condenser is connected to the electrolysis slide 2 by a plurality of tubes. Preferably, at least one set of posts is mounted on a wheeled cart to keep them movable (removable) from the slider.

這種HF冷凝器可以被冷卻到一溫度,其中HF冷凝以形成一液體或甚至一固體。較佳的是如果它被冷凝以形成液體HF。非常合適的是冷卻該阱到-60℃到-80℃的溫度,較佳的是冷卻到大約-70℃。作為冷卻介質,在所希望的低溫下可操作的所熟知的冷卻液體係合適的。較佳的是應用一N2氣體,該氣體係藉由將液N2與氣N2以合適的量混合來獲得的。這種冷卻方式係非常可靠的。因此,滑動件3包括多個管線以遞送並且抽取冷卻介質。This HF condenser can be cooled to a temperature where HF condenses to form a liquid or even a solid. It is preferred if it is condensed to form a liquid HF. It is highly desirable to cool the trap to a temperature of from -60 ° C to -80 ° C, preferably to about -70 ° C. As a cooling medium, well-known coolant systems that are operable at the desired low temperatures are suitable. It is preferred to apply a N 2 gas obtained by mixing liquid N 2 and gas N 2 in an appropriate amount. This cooling method is very reliable. Thus, the slider 3 includes a plurality of lines to deliver and extract the cooling medium.

滑動件3的環境空氣係與一滌氣器通氣的,特別是出於安全原因的ERS滌氣器(以下描述)。The ambient air of the slide 3 is vented with a scrubber, especially for safety reasons (described below).

滑動件4:這種滑動件用作儲存氟氣體並且遞送氟氣體到使用點處。滑動件4包括多個過濾器用於去除任何剩餘的夾帶的固體。例如,在電解池中所產生的F2可能包括來自電解池的夾帶的固體電解質,通常,KF與HF的加合物。該過濾器較佳的是從耐受HF和氟的材料構造的;不銹鋼、銅、蒙乃爾合金金屬以及尤其鎳是特別適合的。從該等金屬的燒結的顆粒製成的過濾器係非常合適的,該等顆粒包括奈米級的孔徑以提供半導體等級F2,例如具有等於或小於5 nm的孔徑,並且更佳的是,具有等於或小於3 nm的孔徑。Slide 4: This slide serves to store fluorine gas and deliver fluorine gas to the point of use. The slider 4 includes a plurality of filters for removing any remaining entrained solids. For example, in an electrolytic cell generated F 2 may include a solid electrolyte entrained from the electrolysis cell, generally, KF to HF adducts. The filter is preferably constructed from materials resistant to HF and fluorine; stainless steel, copper, Monel metal and especially nickel are particularly suitable. Filters made from the particles of such a metal-based sintered very appropriate, nanoscale particles comprise those of the aperture to provide a semiconductor grade F 2, for example equal to or less than 5 nm pore diameter, and more preferably is, Has a pore size equal to or less than 3 nm.

如果希望的話,滑動件4包括一預過濾器以去除具有等於或小於1 μm的孔徑的F2粗粒。If desired, the slider 4 includes a pre-filter to remove F 2 coarse particles having a pore diameter equal to or smaller than 1 μm.

滑動件4還包括一個單槽FT-IR。在這個單槽FT-IR中,可以對純化的F2(它係為儲存或者遞送到使用點而準備的)進行分析。在這種情況下,沒有必要在滑動件7中提供紫外光譜儀和/或多池FT-IR。The slider 4 also includes a single slot FT-IR. In this single-slot FT-IR, purified F 2 (which is prepared for storage or delivery to the point of use) can be analyzed. In this case, it is not necessary to provide an ultraviolet spectrometer and/or a multi-cell FT-IR in the slider 7.

滑動件4較佳的是包括用於儲存氟氣體的裝置。它可以例如包含一用於氟氣體的緩衝罐。The slider 4 preferably includes means for storing fluorine gas. It may, for example, comprise a buffer tank for fluorine gas.

除了緩衝罐之外,但是較佳的是代替緩衝罐,滑動件4還包括處於多個空心體形式的一永久性的或臨時性的氟氣體貯存單元用於貯存F2。該貯存單元係與其他滑動件可連接的。In addition to the buffer tank, but preferably in place of the buffer tank, the slide 4 further comprises a permanent or temporary fluorine gas storage unit in the form of a plurality of hollow bodies for storing F 2 . The storage unit is connectable to other slides.

“永久性氟氣體貯存單元”應理解為具體是指整合到氟工廠中的一氟氣體貯存單元。例如,該氟氣體貯存單元可以是一可傳送的或較佳的是一固定的單元,該單元貫穿氟工廠的操作存在於滑動件4中。較佳的是,該永久性氟氣體貯存單元被設計為包含相對於貯存在該工廠中的氟氣體的總重量的多於90 wt%、更佳的是多於95 wt%、最佳的是大於100 wt%的氟氣體。"Permanent fluorine gas storage unit" is understood to mean specifically a fluorine-containing gas storage unit integrated into a fluorine plant. For example, the fluorine gas storage unit may be a transferable or preferably a fixed unit that is present in the slider 4 throughout the operation of the fluorine plant. Preferably, the permanent fluorine gas storage unit is designed to contain more than 90 wt%, more preferably more than 95 wt%, based on the total weight of the fluorine gas stored in the plant, and most preferably More than 100 wt% of fluorine gas.

滑動件4進一步能夠將氟氣體從滑動件2傳送到使用點處。滑動件4的可能的部件包括但不局限於供應管線、壓縮機、混合機以及緩衝罐。The slider 4 is further capable of transferring fluorine gas from the slider 2 to the point of use. Possible components of the slider 4 include, but are not limited to, supply lines, compressors, mixers, and buffer tanks.

“可連接的”應理解為具體是指該永久性氟氣體貯存單元被裝備為能夠連接到滑動件4的一部件上。較佳的是,該永久性氟氣體貯存單元被裝配為能夠連接到一氟氣體供應管線上。在一較佳的方面,貫穿該氟氣體工廠的操作,該氟氣體貯存單元係連接到滑動件4的一部件上、具體是一氟氣體供應管線上。在一進一步較佳的方面,氟氣體貯存單元係與滑動件4的一部件直接相連的。"Connectable" is understood to mean in particular that the permanent fluorine gas storage unit is equipped to be connectable to a part of the slide 4. Preferably, the permanent fluorine gas storage unit is assembled to be connectable to a fluorine gas supply line. In a preferred aspect, the fluorine gas storage unit is coupled to a component of the slider 4, specifically a fluorine gas supply line, throughout operation of the fluorine gas plant. In a further preferred aspect, the fluorine gas storage unit is directly coupled to a component of the slider 4.

用於將連接到滑動件4的一部件上的氟氣體貯存單元連接的合適的設備包括一歧管,該歧管通過一管線連接到氟氣體貯存單元的每個空心體上並且較佳的是在每個管線上具有一關閉閥門從而允許單獨分開每個空心體,並且所述歧管係進一步連接到滑動件4的一部件上的。A suitable apparatus for connecting a fluorine gas storage unit connected to a component of the slider 4 includes a manifold connected to each of the hollow bodies of the fluorine gas storage unit via a line and preferably There is a shut-off valve on each line to allow for separate separation of each hollow body, and the manifold is further connected to a component of the slider 4.

滑動件4較佳的是包括從4到25個空心體、更佳的是從5到8個空心體。該等空心體較佳的是具有實質上相同的形狀和尺寸。柱形形狀空心體(管)係較佳的。氟氣體貯存的每個空心體較佳的是具有一關閉閥門。The slider 4 preferably comprises from 4 to 25 hollow bodies, more preferably from 5 to 8 hollow bodies. The hollow bodies preferably have substantially the same shape and size. A cylindrical shape hollow body (tube) is preferred. Preferably, each hollow body of the fluorine gas storage has a shut-off valve.

氟氣體貯存單元的多個空心體可以藉由一適當的框架被合適地固定在一起。具體的框架幾何形狀包括三角形、正方形、以及矩形幾何形狀。The plurality of hollow bodies of the fluorine gas storage unit can be suitably fixed together by a suitable frame. Specific frame geometries include triangles, squares, and rectangular geometries.

在根據本發明的氟氣體工廠中,該等氟氣體貯存裝置總體上能夠含有處於至少25磅/平方英寸(大約1.72表壓)的壓力的氟氣體。通常該壓力係等於或大於35磅/平方英寸(大約2.4表壓),較佳的是等於或大於40磅/平方英寸(大約2.8表壓)。在根據本發明的工廠中,該等氟氣體貯存裝置總體上能夠包含或包含處於至多400磅/平方英寸(大約27.6表壓)、較佳的是等於或小於75磅/平方英寸(大約5.2表壓)的壓力的氟氣體。通常該壓力係等於或低於65磅/平方英寸(大約4.5表壓),較佳的是等於或低於60磅/平方英寸(大約4.1表壓)。應理解到,氟氣體貯存單元的空心體總體上能夠包含或包含處於上述壓力的氟氣體。特別佳的是該等空心體含有處於上述壓力的氟氣體。In a fluorine gas plant according to the present invention, the fluorine gas storage devices can generally contain fluorine gas at a pressure of at least 25 psi (about 1.72 gauge). Typically, the pressure is equal to or greater than 35 psi (about 2.4 gauge), preferably equal to or greater than 40 psi (about 2.8 gauge). In a plant according to the invention, the fluorine gas storage means can generally comprise or comprise at most 400 psi (about 27.6 gauge), preferably equal to or less than 75 psi (about 5.2) Pressurize the pressure of the fluorine gas. Typically the pressure is equal to or lower than 65 psi (about 4.5 gauge), preferably equal to or lower than 60 psi (about 4.1 gauge). It should be understood that the hollow body of the fluorine gas storage unit can generally contain or contain fluorine gas at the above pressure. It is especially preferred that the hollow bodies contain fluorine gas at the above pressure.

在根據本發明的氟氣體工廠中,在氟貯存裝置中貯存的分子F2與氟氣體設備的每日的分子F2生產能力之比總體上是從0.1到1、較佳的是從0.1到0.25。In general the ratio of the fluorine gas plant of the present invention, stored in the storage means fluorine F 2 F in the molecule with molecular fluorine gas daily production capacity of the apparatus 2 is from 0.1 to 1, preferably from 0.1 to 0.25.

較佳的是,每個空心體可以從該工廠單獨關閉;這改進了安全性。氟離開滑動件4較佳的是通過雙壁管被運送到使用點處。氟氣體在內管中運送;外雙重壁封套包括氮氣。該等管系包括一壓力感測器來分析外雙重壁封套中的氮壓力。較佳的是,該等管的壁係比通常用於運送氣體的壁更厚的,即,較佳的是,它們更厚1 mm,較佳的是,更厚4 mm;等於或大於5 mm的壁厚係特別佳的;分類為“目錄表80”的管係非常適合的。它們用於改進安全性。具有放射線檢驗的焊接的管系係非常適合的。Preferably, each hollow body can be individually closed from the factory; this improves safety. The fluorine exiting slide 4 is preferably transported through a double walled tube to the point of use. The fluorine gas is carried in the inner tube; the outer double wall envelope comprises nitrogen. The piping systems include a pressure sensor to analyze the nitrogen pressure in the outer double wall envelope. Preferably, the walls of the tubes are thicker than the walls normally used to carry the gas, i.e., they are preferably 1 mm thicker, preferably 4 mm thicker; equal to or greater than 5 The wall thickness of mm is particularly good; the pipe system classified as "Table of Contents 80" is very suitable. They are used to improve security. A welded tube system with radiation inspection is very suitable.

這個或該等貯存容器可以安裝在輪上或是藉由一升降叉車可運輸的。This or such storage containers can be mounted on wheels or transported by a forklift.

滑動件4的環境空氣係與一滌氣器通氣的,特別是以下描述的ERS滌氣器(出於安全原因)。The ambient air of the slide 4 is vented with a scrubber, in particular the ERS scrubber described below (for safety reasons).

在根據本發明的氟氣體工廠中,使用點可以是與一另外的製作工廠相連的,例如一化學工廠或具體一使用氟氣體用於表面處理的工廠。使用位點通常是與一半導體製造工廠相連的,較佳的是光電裝置或平板顯示器的製造。In the fluorine gas plant according to the present invention, the point of use may be connected to an additional manufacturing plant, such as a chemical plant or a specific plant that uses fluorine gas for surface treatment. The site of use is typically associated with a semiconductor manufacturing facility, preferably a photovoltaic device or flat panel display.

在根據本發明的氟氣體工廠的一較佳的實施方式中,包括氟氣體貯存單元的滑動件4係一封閉的空間。該封閉的空間總體上包括能夠觸發封閉的空間與滑動件6的連接的一氟感測器。適當地,該封閉的空間係藉由一連接到一風扇上的抽吸管線來連接到滑動件6上的,該風扇係可操作的從而將氣體從滑動件4的封閉的空間運送到滑動件6。In a preferred embodiment of the fluorine gas plant according to the present invention, the slider 4 including the fluorine gas storage unit is a closed space. The enclosed space generally includes a fluorine sensor capable of triggering the connection of the enclosed space to the slider 6. Suitably, the enclosed space is connected to the slider 6 by a suction line connected to a fan that is operable to transport gas from the enclosed space of the slider 4 to the slider 6.

在另一的實施方式中,根據本發明的氟氣體工廠進一步包括一混合器、較佳的是一靜態混合器,所述混合器較佳的是能夠接受來自滑動件4的氟並且接受來自一惰性氣體供應管線的惰性氣體,如較佳的是氬和/或氮。In another embodiment, the fluorine gas plant according to the present invention further comprises a mixer, preferably a static mixer, which is preferably capable of accepting fluorine from the slider 4 and accepting from a The inert gas of the inert gas supply line is preferably argon and/or nitrogen.

在一可隨意的實施方式中,一壓力控制迴路調節了、總體上將供應到使用點處的氟氣體的壓力降低到所希望的值。In a discretionary embodiment, a pressure control loop regulates, generally reduces, the pressure of the fluorine gas supplied to the point of use to a desired value.

滑動件5提供了藉由冷卻水冷卻或加熱工廠的零件。它較佳的是位於電解的滑動件2或子滑動件2A和2B或任何另外的子滑動件2X附近,更佳的是,它係位於該等滑動件上面。滑動件5包括至少一個用於當反應開始時加熱電解池以熔化電解質鹽並且當反應運行時冷卻該等電解池的迴路。該迴路填充了冷卻水,這種水可以是自來水或蒸餾水。該迴路包括一緩衝罐、一泵(較佳的是多餘的)、以及一具有風扇(具有可變的速率驅動)的乾燥冷卻器。在操作過程中,冷卻水較佳的是保持在75℃至95℃以避免電解池中的電解質的凝固。The slider 5 provides parts for cooling or heating the plant by cooling water. It is preferably located adjacent to the electrolyzed slider 2 or sub-sliders 2A and 2B or any other sub-slider 2X, and more preferably it is located above the sliders. The slider 5 includes at least one circuit for heating the electrolytic cell at the beginning of the reaction to melt the electrolyte salt and cooling the electrolytic cells while the reaction is running. The circuit is filled with cooling water, which may be tap water or distilled water. The circuit includes a buffer tank, a pump (preferably redundant), and a dry cooler having a fan (with variable rate drive). During operation, the cooling water is preferably maintained at 75 ° C to 95 ° C to avoid solidification of the electrolyte in the electrolytic cell.

在滑動件5中包括的另一迴路用於冷卻該裝置的其他熱交換器。它含有一冷卻液,較佳的是水與乙二醇的一混合物,更佳的是,包括按重量計40%的乙二醇的水。同樣該迴路包括一緩衝液、一泵(較佳的是多餘的)、以及一乾燥冷卻器。該冷卻迴路包括用於測量冷卻水的溫度的多個檢測器、用於加熱冷卻水的裝置(例如電加熱)、用於冷卻此類循環液體的熱交換器。可隨意地,該工廠包括一蒸汽發生器以便提供蒸汽或者熱的清洗水。該蒸汽發生器可以是便攜的一種。熱蒸氣可以例如用於提供熱水,在該熱水中電解質鹽可以是溶解的,如果希望的話。結果係,滑動件5較佳的是包含至少兩個冷卻水迴路。Another circuit included in the slider 5 is used to cool other heat exchangers of the device. It contains a cooling liquid, preferably a mixture of water and ethylene glycol, more preferably 40% by weight of ethylene glycol. Also the circuit includes a buffer, a pump (preferably redundant), and a dry cooler. The cooling circuit includes a plurality of detectors for measuring the temperature of the cooling water, means for heating the cooling water (for example, electric heating), and a heat exchanger for cooling such circulating liquid. Optionally, the plant includes a steam generator to provide steam or hot wash water. The steam generator can be a portable one. The hot vapor can, for example, be used to provide hot water, in which the electrolyte salt can be dissolved, if desired. As a result, the slider 5 preferably comprises at least two cooling water circuits.

滑動件6包括至少一個滌氣器,每一個用於F2和H2。較佳的是,該等滌氣器泵係多餘的。該工廠的滑動件(特別是滑動件1、2、3、4和7)包括一通風系統以使滑動件外殼的環境空氣藉由滑動件6中的滌氣器永久性通氣。The slider 6 includes at least one scrubber, one for each of F 2 and H 2 . Preferably, the scrubber pumps are redundant. The slides of the plant (especially the slides 1, 2, 3, 4 and 7) include a ventilation system to permanently vent the ambient air of the slider housing by the scrubber in the slide 6.

較佳的是,滑動件6包括一F2滌氣器用於為了安全原因或維修操作而銷毀任何的F2或放空HF。來自該等滑動件的通風的空氣的F2和HF在一滌氣器中被處理用於應急回應(ERS)。該等滌氣器較佳的是噴射洗滌器並且提供了抽吸。該等滌氣器可以安裝在子滑動件上,例如一子滑動件6A,它包括至少一個用於緊急情況回應(ERS)的滌氣器,一滑動件6B,它用於洗滌產生的H2,目的係去除其中夾帶的HF,以及一滌氣器以去除源自滑動件的環境空氣的通氣的廢氣中的HF和/或F2(如以上所解釋)。Preferably, the slider 6 includes an F 2 scrubber for destroying any F 2 or venting HF for safety reasons or maintenance operations. The F 2 and HF of vented air from the sliders are processed in an scrubber for emergency response (ERS). Preferably, the scrubbers are jet scrubbers and provide suction. Such scrubber H can be mounted on the sub-sliding member, such as a sub-sliding member. 6A, which comprises a scrubber at least one emergency response (ERS), and a slide member 6B, which is used to produce a washed 2 The purpose is to remove the HF entrained therein, and a scrubber to remove HF and/or F 2 in the vented exhaust gas from the ambient air of the slider (as explained above).

規則的F2滌氣器(可隨意地安裝在子滑動件6B中)至少對應在規則操作過程中有待去除的預期量的F2。藉由與一減輕溶液進行接觸來去除F2。該滌氣器較佳的是包括一噴射洗滌器以及一填充柱以提供減輕溶液與F2之間的高接觸面積。較佳的是,離開規則的F2滌氣器的氣體穿過ERS滌氣器的支持滌氣器。A regular F 2 scrubber (optionally mounted in sub-slider 6B) corresponds at least to the desired amount of F 2 to be removed during regular operation. F 2 is removed by contact with a mitigating solution. The scrubber preferably includes a jet scrubber, and a packed column to provide a solution to alleviate the F 2 between high contact area. Preferably, the gas exiting the regular F 2 scrubber passes through the support scrubber of the ERS scrubber.

該等ERS滌氣器用作規則的F2滌氣器的支持滌氣器,它用於從所通氣的空氣去除F2或HF並且用於含有HF和/或F2的所通氣的氣體在洩漏之後的緊急處理。ERS滌氣器(可隨意地安裝在子滑動件6A中)的容量較佳的是至少對應於在對於緊急事件情況下有待去除的氟和HF的量,例如,在非常未必發生的管破裂的情況下,關於含有氟的一管或一HF的貯存罐的事故中。所建議的是根據最壞的情形選擇ERS滌氣器的容量;例如如果存在具有2 m3容量的HF罐以及具有8 kg F2容量的F2貯存管,該ERS應該能夠減少對應的HF以及F2的量以及工廠滯留量。較佳的是,該ERS滌氣器包括用於洗滌的2個單元以實現高的銷毀以及去除效率;藉由正常以及緊急情況供電來向多餘的泵送料。它較佳的是包括一噴射洗滌器以及一填充柱以實現有待處理的氣體與減輕溶液之間的良好接觸。用於緊急情況處理的其他單元可以包括一填充柱,但是較佳的是,它包括兩個串聯的噴射洗滌器。可以用已知的用於去除F2的試劑來進行F2去除。較佳的是,一KOH溶液或NaOH(可隨意地包括一鹼金屬硫代硫酸鹽,例如硫代硫酸鈉或硫代硫酸鉀)被用作減輕溶液並且通過這個滌氣器或該等滌氣器以及該柱(如果存在的話)來泵送,作為對於F2的分解劑。可以預知一冷卻器用於冷卻KOH溶液。當然,這係一緊急情況滌氣器用於處理HF和F2的構思的一優點。The ERS scrubbers are used as a support scrubber for a regular F 2 scrubber for removing F 2 or HF from vented air and for venting gases containing HF and/or F 2 to leak After the emergency treatment. The capacity of the ERS scrubber (optionally mounted in the subslider 6A) preferably corresponds at least to the amount of fluorine and HF to be removed in the event of an emergency, for example, in the event of a tube crack that does not necessarily occur. In the case of an accident involving a tube containing fluorine or a storage tank of HF. It is recommended to select the capacity of the ERS scrubber according to the worst case; for example, if there is an HF tank with a capacity of 2 m 3 and an F 2 storage tube with a capacity of 8 kg F 2 , the ERS should be able to reduce the corresponding HF and The amount of F 2 and the amount of plant retention. Preferably, the ERS scrubber includes two units for washing to achieve high destruction and removal efficiency; the excess pump is fed by normal and emergency power. It preferably includes a jet scrubber and a packed column to achieve good contact between the gas to be treated and the mitigation solution. Other units for emergency handling may include a packed column, but preferably it includes two jet scrubbers in series. F 2 removal can be carried out using known reagents for removing F 2 . Preferably, a KOH solution or NaOH (optionally including an alkali metal thiosulfate such as sodium thiosulfate or potassium thiosulfate) is used as a lightening solution and through the scrubber or the scrubber and the column is (if present) is pumped, as a decomposing agent for the F 2. It is foreseen that a cooler is used to cool the KOH solution. Of course, this advantage of a system emergency scrubber for processing concepts HF and F 2.

用於H2氣流的HF減少的滑動件6的滌氣器可以安裝在子滑動件6B中。子滑動件6B較佳的是包括一用水性HF溶液操作的噴射洗滌器以降低H2中的HF含量。HF的濃度可以是在按重量計1%與10%之間的範圍內。該滌氣器進一步包括一填充柱,其中在柱的頂部給予新鮮的水以降低HF含量。滑動件6B還包括一管線,它允許藉由氮(它被用作滑動件3中的冷卻介質)來稀釋H2A scrubber for the HF reduction of the H 2 gas stream can be installed in the subslider 6B. 6B the sub-sliding member preferably includes a jet scrubber aqueous HF solution to reduce the HF content of the operation in H 2. The concentration of HF may be in the range between 1% and 10% by weight. The scrubber further includes a packed column wherein fresh water is applied to the top of the column to reduce the HF content. The slider 6B also includes a line that allows dilution of H 2 by nitrogen, which is used as a cooling medium in the slider 3.

滑動件6中、或對應的滑動件6A和6B中的滌氣器的可靠性係非常重要的。因此,用於使減輕溶液循環通過該等滌氣器的基本部件如風扇或泵可以是多餘的。不時地,向循環減輕溶液中加入新鮮的緩和劑,例如KOH溶液,和/或硫代硫酸鹽或其溶液,例如由一卡車提供。The reliability of the scrubber in the slider 6, or in the corresponding sliders 6A and 6B, is very important. Therefore, the basic components, such as fans or pumps, used to circulate the mitigation solution through the scrubbers may be redundant. From time to time, fresh moderators, such as KOH solutions, and/or thiosulfate or solutions thereof, such as provided by a truck, are added to the recycle reducing solution.

滑動件6較佳的是還包括用於在事故性洩漏的情況下的液體的一或多個截留凹陷。The slider 6 preferably further includes one or more trapped depressions for the liquid in the event of an accidental leak.

滑動件7涉及用於分析產生的F2的裝置。它較佳的是安裝在滑動件2A和2B附近;非常佳的是,它位於滑動件2A和2B上面。滑動件7例如是一分析器屏障。它周圍的環境大氣較佳的是通風到ERS的。該分析器包含適合用於確定所產生的F2的主要雜質的含量的分析裝置。The slider 7 relates to a device for analyzing the generated F 2 . It is preferably mounted near the sliders 2A and 2B; very preferably, it is located above the sliders 2A and 2B. The slider 7 is, for example, an analyzer barrier. The ambient atmosphere around it is preferably ventilated to the ERS. The analysis apparatus comprising an analyzer for determining the appropriate content of the main impurities of the generated F 2 a.

在一實施方式中,一紫外光譜儀(它分析紫外光譜)以及多輸入、多池FT-IR光譜儀(傅裡葉變換紅外光譜)分析器係非常適合的。較佳的是,取自電解池的粗F2以及純化的F2兩者可以被送到單槽FT-IR或者多槽FT-IR中。在多槽FT-IR中,在一給定的時間對一通道進行分析。HF、CF4、C2F6以及COF2的量例如可以藉由FT-IR來測量,而F2的含量藉由UV來分析。已經發現,紫外光譜法可以用作氟的一直接測量工具,當陽極燃燒發生時它顯示出了氟濃度的劇烈降低;在FT-IR中的相同時間觀察到CF4的巨大增加。因此,這種燃燒很容易藉由燃燒過程中F2濃度的急劇降低進行檢測,在這個過程中形成了雜質(主要是CF4和C2F6)。這種燃燒的結果(所生產的F2包含比規則工作時更多的CF4、C2F6、COF2、HF)不僅是雜質含量的改變而且還有藉由檢測器(尤其在本發明中是藉由UV光譜學)所監測的氟含量的急劇降低。在使用UV光譜學的測量過程中,可以使用整個UV光譜。較佳的是,不是將整個光譜而僅僅將這個特定波長處的吸收(具體是在200和400 nm之間、更佳的是250至330 nm、最佳的是270至290 nm之間、甚至在約280 nm處的UV光譜)用於測量,因為它差不多是F2的UV吸收的最大值。FTIR和UV測量同樣用於控制純化的F2的純度。因此,該分析用於藉由用UV測量粗F2並且用FT-IR測量CF4來檢測陽極燃燒並且用於證明並且控制純化的F2的純度。In one embodiment, an ultraviolet spectrometer (which analyzes the ultraviolet spectrum) and a multi-input, multi-cell FT-IR spectrometer (Fourier transform infrared spectroscopy) analyzer are well suited. Preferably, both the crude F 2 taken from the electrolytic cell and the purified F 2 can be sent to a single tank FT-IR or a multi tank FT-IR. In a multi-slot FT-IR, a channel is analyzed at a given time. The amounts of HF, CF 4 , C 2 F 6 and COF 2 can be measured, for example, by FT-IR, and the content of F 2 can be analyzed by UV. It has been found, UV spectroscopy may be used as a direct measurement tool fluorine, anode burn occurs when it shows a drastic reduction of the fluorine concentration; CF 4 dramatically increase observed at the same time in the FT-IR. Therefore, this combustion is easily detected by a sharp drop in the concentration of F 2 during combustion, in which impurities (mainly CF 4 and C 2 F 6 ) are formed. The result of this combustion (the F 2 produced contains more CF 4 , C 2 F 6 , COF 2 , HF than during regular operation) is not only a change in the impurity content but also by the detector (especially in the present invention) The middle is a sharp decrease in the fluorine content monitored by UV spectroscopy. The entire UV spectrum can be used during measurements using UV spectroscopy. Preferably, instead of the entire spectrum, only the absorption at this particular wavelength (specifically between 200 and 400 nm, more preferably between 250 and 330 nm, optimally between 270 and 290 nm, or even at about 280 UV spectrum nm at) for measuring, as it is almost the maximum F UV 2 absorption. FTIR and UV measurement is also used to control the purity of the purified F 2. Therefore, this analysis was used to detect anode combustion by measuring crude F 2 with UV and CF 4 by FT-IR and used to demonstrate and control the purity of purified F 2 .

所有電解池的粗F2以及純化的F2被連續取樣並分析。目前的FT-IR可以接受高達9個樣品。因此,純化的F2以及高達8個電解池的粗F2可以用電流產生裝置的多池FTIR進行分析。All of the electrolytic cell and the crude purified F 2 F 2 are continuously sampled and analyzed. The current FT-IR can accept up to 9 samples. Thus, purified F 2 and crude F 2 of up to 8 electrolytic cells can be analyzed using a multi-cell FTIR of a current generating device.

根據另一實施方式,所生產的氟的分析係僅僅通過單槽FT-IR進行的;沒有應用一紫外光譜儀。該單槽FT-IR被用於對純化的F2進行分析(最終分析)。According to another embodiment, the analysis of the produced fluorine is carried out only by single-slot FT-IR; no UV spectrometer is applied. This single-well FT-IR was used to analyze the purified F 2 (final analysis).

滑動件8包含多個整流器、BPCS(基本程序控制系統)、ESD(應急關閉系統)、F&G(火災和氣體系統)嵌板(對齊了火警警報和氣體警報)、小電動機起動器、光強度分佈以及其他裝置以提供電力並且控制工廠的電力裝置。滑動件8安裝在滑動件2A和2B附近;較佳的是,它位於它們上面。每個電解池,如以上所述,通常具有至少一個但是經常多個陽極,例如26個。術語“多個陽極”可以是指任何等於或大於2的數位。陽極的數目係僅受實際的考慮限制的,例如池或者池單元(由幾個池構成)不應該是不合理的大的。經常,陽極的數目係等於或低於80的,較佳的是等於或低於70。一整流器可以向一個、兩個或者更多個陽極提供電流。較佳的是,每個陽極係由一整流器供應的。整流器係市場上可獲得的,該整流器可以分開地向幾個陽極提供電流。例如,如果26個陽極存在于一池中的話,較佳的是提供26個整流器或者13個雙整流器(它們分開地向2個陽極提供電流)。該等整流器較佳的是在裝在空氣調節的外殼中的整流器盒中組裝的。Slide 8 contains multiple rectifiers, BPCS (Basic Program Control System), ESD (Emergency Shutdown System), F&G (Fire and Gas System) panels (aligned with fire alarms and gas alarms), small motor starters, light intensity distribution And other devices to provide power and control the power plant of the plant. The slider 8 is mounted near the sliders 2A and 2B; preferably, it is located above them. Each electrolytic cell, as described above, typically has at least one but often multiple anodes, for example, 26. The term "plurality of anodes" may refer to any digit equal to or greater than two. The number of anodes is only limited by practical considerations, such as pools or pool units (consisting of several pools) should not be unreasonably large. Often, the number of anodes is equal to or lower than 80, preferably equal to or lower than 70. A rectifier can supply current to one, two or more anodes. Preferably, each anode is supplied by a rectifier. Rectifiers are commercially available that can separately supply current to several anodes. For example, if 26 anodes are present in a cell, it is preferred to provide 26 rectifiers or 13 dual rectifiers (which separately supply current to the 2 anodes). The rectifiers are preferably assembled in a rectifier box housed in an air-conditioned housing.

較佳的是在這個滑動件8中提供輕微超壓以保護免於氣體進入。所有線纜和陰極匯流線應該被小心地密封。It is preferred to provide a slight overpressure in this slider 8 to protect against gas ingress. All cables and cathode bus lines should be carefully sealed.

較佳的是整流器盒係在一固定的框架上用螺栓固定的用於地震保護。Preferably, the rectifier box is bolted to a fixed frame for seismic protection.

滑動件8包括多個壁以及一頂蓋。它較佳的是還包括一火災檢測系統,特別是一VESDA(非常早期煙霧檢測裝置)以及一熄火系統,該系統例如用HFC-227ea或用(惰性氣體的混合物(氮、氬以及二氧化碳)來操作。The slider 8 includes a plurality of walls and a top cover. It preferably further comprises a fire detection system, in particular a VESDA (very early smoke detection device) and a flameout system, for example using HFC-227ea or (A mixture of inert gases (nitrogen, argon, and carbon dioxide) is operated.

滑動件9較佳的是一預製室,該室具有混凝土壁或類似於一從金屬防護物製成的容器。它包含用於連接到電流的並且將它從中電壓轉化成低電壓的裝置。較佳的是,它含有“子發電站”子滑動件9A和9B。滑動件9A較佳的是含有MV(中電壓)池用於引入的和輸出的電流和旁路電流以及變壓器用於將中電壓電流轉化成低電壓電流。它對於局部網是可操作的;例如,該等變壓器係被選擇為它們適合局部電壓,該電壓可以是例如380 V或400 V(50 Hz)或440 V(60 Hz)。滑動件9較佳的是還包括一火災檢測系統,特別是一VESDA(非常早期煙霧檢測裝置)以及一熄火系統,該系統例如用HFC-227ea或用(惰性氣體的混合物(氮、氬以及二氧化碳)來操作。The slider 9 is preferably a prefabricated chamber having a concrete wall or a container similar to that made of metal shield. It contains means for connecting to a current and converting it from a medium voltage to a low voltage. Preferably, it contains "sub-power station" sub-sliders 9A and 9B. The slider 9A is preferably a current and bypass current containing an MV (medium voltage) cell for introduction and output and a transformer for converting the medium voltage current into a low voltage current. It is operable for the local network; for example, the transformers are selected such that they are suitable for local voltages, which may be, for example, 380 V or 400 V (50 Hz) or 440 V (60 Hz). The slider 9 preferably further comprises a fire detection system, in particular a VESDA (very early smoke detection device) and a flameout system, for example using HFC-227ea or (A mixture of inert gases (nitrogen, argon, and carbon dioxide) is operated.

滑動件9B同樣較佳的是一預製的具有多個壁和一頂蓋的混凝土室。該子站容納了低壓開關裝置(LVCS)和一柴油發電機。它係通過線纜互聯到需要低電壓供電的滑動件上的,例如通過一線纜槽。它較佳的是還包括一火災檢測系統,特別是一VESDA(非常早期煙霧檢測裝置)以及一熄火系統,該系統例如用HFC-227ea或用(惰性氣體的混合物(氮、氬以及二氧化碳)來操作。The slider 9B is also preferably a prefabricated concrete chamber having a plurality of walls and a top cover. The substation houses a low voltage switchgear (LVCS) and a diesel generator. It is interconnected by wires to a slider that requires low voltage power, for example through a cable trough. It preferably further comprises a fire detection system, in particular a VESDA (very early smoke detection device) and a flameout system, for example using HFC-227ea or (A mixture of inert gases (nitrogen, argon, and carbon dioxide) is operated.

滑動件9B較佳的是還包括一對於一升降叉車的蓄電池充電站。The slider 9B preferably further includes a battery charging station for a forklift.

滑動件9B必須是互聯到過程滑動件上的,特別是滑動件8中的帶有幾個整流器的。The slider 9B must be interconnected to the process slide, in particular with several rectifiers in the slider 8.

滑動件10包括用於個人的實用設施,例如,一控制室、一實驗室和一休息室。較佳的是,它被劃分成子滑動件10A和子滑動件10B。子滑動件10A包含控制室和實驗室。可能是小的實驗室包括一具有良好的通風的通風櫥,例如高達500 m3/h並且甚至更大,該櫥較佳的是由耐酸材料製成的並且可以用於分析滴定法,一安全櫥用於試劑和樣品,一洗手盆和一化學品池,其中可以收集化學品廢品,較佳的是在一由耐酸材料製成的筒中。該實驗室較佳的是具有一氣體檢測器,該氣體檢測器安裝在新鮮空氣進口處,以及一關閉機構,該機構在氣體警報的情況下關閉氣體進口。子滑動件10A較佳的是保持在輕微超壓下以防止空氣進入。滑動件10A較佳的是包括空氣調節。The slider 10 includes practical facilities for an individual, such as a control room, a laboratory, and a lounge. Preferably, it is divided into a sub-slider 10A and a sub-slider 10B. The subslider 10A includes a control room and a laboratory. It may be that the small laboratory includes a fume hood with good ventilation, for example up to 500 m 3 /h and even larger, the cupboard is preferably made of acid-resistant material and can be used for analytical titration, a safety The cabinet is used for reagents and samples, a wash basin and a chemical tank in which chemical waste can be collected, preferably in a cylinder made of an acid resistant material. Preferably, the laboratory has a gas detector mounted at the fresh air inlet and a closing mechanism that closes the gas inlet in the event of a gas alarm. The subslider 10A is preferably kept under slight overpressure to prevent air from entering. The slider 10A preferably includes air conditioning.

該控制室的控制板較佳的是線上連接到一遙控板上,該遙控板可以位於另一設施上。這允許了從一單個的控制室遠端操作若干氟氣體生產工廠。The control panel of the control room is preferably connected in-line to a remote control panel, which may be located at another facility. This allows a number of fluorine gas production plants to be operated remotely from a single control room.

子滑動件10B包含休息室。它含有對於控制室個人有用的設備。它較佳的是包括多個抽屜、一更衣室、一廁所、一淋浴器、以及用於化學品罩衣(手套、披肩等)的櫥櫃。該工廠安全淋浴器包括眼淋浴系統並且較佳的是位於子滑動件10B的外部附近,因為它必須被供應熱的可引用水。滑動件10較佳的是包括通風和加熱。The subslider 10B includes a lounge. It contains equipment that is useful to the control room. It preferably includes a plurality of drawers, a dressing room, a toilet, a shower, and a cabinet for chemical gowns (gloves, shawls, etc.). The factory safety shower includes an eye shower system and is preferably located adjacent the exterior of the subslider 10B as it must be supplied with hot water. Slide 10 preferably includes ventilation and heating.

該工廠將包括另外的對操作它有用的設備。The plant will include additional equipment useful for operating it.

壓縮機係需要的以便提供加壓的氟氣體。它們必須是耐氟氣體的。用於在核工業中氟氣體處理的壓縮機係非常適合的。它們較佳的是膜片式壓縮機。此類壓縮機市場上是可獲得的。該等膜片係由耐F2的材料(尤其用蒙乃爾合金金屬、不銹鋼、銅、或者鎳)製成的。該等隔膜係3-層的薄膜,這樣在一隔膜破裂的情況下,該破裂將會由壓力測量裝置來檢測到,並且沒有F2將會離開該壓縮機隔膜到該外部區域中。A compressor is required to provide pressurized fluorine gas. They must be resistant to fluorine. Compressors for fluorine gas treatment in the nuclear industry are very suitable. They are preferably diaphragm compressors. Such compressors are available on the market. The diaphragms are made of F 2 resistant materials (especially with Monel metal, stainless steel, copper, or nickel). Such membrane-based 3-ply film, so that in case of a rupture of the diaphragm, the measuring device will be broken by the pressure to be detected, and F 2 will not leave the compressor to the external region of the membrane.

該工廠還將需要用於操作的儀器以及閥門。The plant will also require instruments and valves for operation.

例如,如果一混合器係存在的以便提供F2和惰性氣體或者其他氣體的混合物,則混合該等氣體的過程步驟包括用於F2以及有待與它混合的一或多種氣體的質量流量計、所安裝的控制閥門與專用的程式控制迴路以及互鎖裝置,以便確保將該等氣體(例如一惰性氣體或者多種惰性氣體)與F2進行一適當且安全的混合。For example, if a mixer is present to provide a mixture of F 2 and an inert gas or other gas, the process steps of mixing the gases include mass flow meters for F 2 and one or more gases to be mixed with, a control valve installed to the dedicated program control circuit and an interlocking means to ensure that the gases and the like (e.g., an inert gas or more inert gases) F 2 with an appropriate and safe for mixing.

該工廠,如以上說明的,具有用於其操作的對某些參數(例如氟氣體或惰性氣體的質量流量控制)進行分析的裝置。為此目的,質量流控制器係較佳的是使用的。藉由此類質量流控制器,氟氣體的量可以被控制,它穿過攜帶它的管線,例如到該等FTIR和UV分析器。該等質量流控制器應該是“低ΔP類型”的控制器,僅引起了一低的壓力下降。用於將氣體輸送到該等分析器(它們必須適合用於氟氣體的運輸)上的此類流量計,連同管道、管、以及裝配件在市場上也是可獲得的。閥門應該是膜盒密封的重載(heavy duty)閥門。一PLC(可程式設計邏輯控制器)管理了該等FTIR反射鏡的移動、收集了故障警報並且將結果傳送到BPRS(基本程序控制系統)。為了分析純的F2,較佳的是應用的是用AgCl製成的視窗,為了分析粗F2,例如來自該等電解池的採樣管線的粗F2,可以應用Al2O3視窗。The plant, as explained above, has means for analyzing certain parameters, such as mass flow control of fluorine gas or inert gas, for its operation. For this purpose, a mass flow controller is preferably used. With such a mass flow controller, the amount of fluorine gas can be controlled, passing through the pipeline carrying it, for example to the FTIR and UV analyzers. These mass flow controllers should be "low ΔP type" controllers, causing only a low pressure drop. Such flow meters for delivering gas to such analyzers, which must be suitable for the transport of fluorine gas, are also commercially available along with pipes, tubes, and fittings. The valve should be a heavy duty duty valve seal. A PLC (programmable logic controller) manages the movement of the FTIR mirrors, collects fault alarms and transmits the results to the BPRS (Basic Program Control System). For the analysis of pure F 2 , it is preferred to use a window made of AgCl. For the analysis of the crude F 2 , such as the crude F 2 of the sampling line from the electrolytic cells, an Al 2 O 3 window can be applied.

根據以上說明,變得清楚的是可以應用幾個關於F2分析的替代方案。According to the above description, it becomes clear that several alternatives may be applied on F 2 analysis.

根據一第一替代方案,單槽FT-IR位於滑動件4中。它用於對該F2進行最終分析。According to a first alternative, the single-slot FT-IR is located in the slider 4. It is used for the final analysis of this F 2 .

根據一第二替代方案,多槽FT-IR以及可隨意地一紫外分析器位於滑動件7中。According to a second alternative, the multi-slot FT-IR and optionally an ultraviolet analyzer are located in the slider 7.

根據一第三替代方案,單槽FT-IR位於滑動件4中,並且多槽FT-IR以及可隨意地一紫外分析器位於滑動件7中。According to a third alternative, the single-slot FT-IR is located in the slider 4, and the multi-slot FT-IR and optionally an ultraviolet analyzer are located in the slider 7.

該第一替代方案係最便宜的解決方案。該第二替代方案係比第一替代方案更昂貴;但它允許一快速反應,如果在一或多個池中的F2生產被干擾的話。它還允許識別池的不規則操作。該第三替代方案係最昂貴的一個;它允許同時一快速反應並且識別有故障的池,並且它允許檢查最終F2的純度。This first alternative is the cheapest solution. The second alternative system is more expensive than a first alternative; it allows a rapid response, F or if a plurality of pools of 2, then the production is disturbed. It also allows for the identification of irregular operations of the pool. The third most expensive alternative a system; it allows a quick response and simultaneously identify a faulty cell, and it allows to check the final purity F 2.

對該等替代方案的選擇取決於消費者的預期或需求、個人的經驗、工廠運行到有故障的條件的傾向,等等。往往還有可能的是在滑動件4和7中提供多個分析器以便對它們的一者或者兩者不連續地或者間歇地進行操作。The choice of such alternatives depends on the consumer's expectations or needs, the individual's experience, the propensity of the plant to operate to faulty conditions, and the like. It is often also possible to provide a plurality of analyzers in the sliders 4 and 7 to operate discontinuously or intermittently on one or both of them.

安全設備:眾所周知的是尤其是F2和HF是需要謹慎處理的化合物。H2當然是可燃的。因此,該設備包括安全裝置。例如,該工廠包括一帶有多個轉換開關的用於一應急關閉(ESD)、用於警報、以及用於最優先自動處理的安全嵌板。Safety equipment: It is well known that especially F 2 and HF are compounds that require careful handling. H 2 is of course flammable. Therefore, the device includes a security device. For example, the plant includes a safety panel with multiple transfer switches for an emergency shutdown (ESD), for alarms, and for the highest priority automatic handling.

F2、HF、如果適當的話、H2的檢測器係安裝在例如一至ERS滌氣器的通風管中並且位於發射點處的。為了安全的作用,氣體報警信號被發送到ESD。該工廠包括多個報警信號燈,它們係被開啟的,即,如果氣體報警信號發送到該ESD的話。該等警報還必須是在滑動件10的控制室中可檢測的。氣體測量必須在控制室中例如以ppm來給出。如果工廠包括在滑動件10的控制室中的一火災和氣體嵌板以便顯示所有的火災和氣體警報、以及通風故障則係非常有利的。F 2 , HF, if appropriate, the detector of H 2 is installed, for example, in a venting tube to the ERS scrubber and at the point of emission. For safety reasons, a gas alarm signal is sent to the ESD. The plant includes a plurality of alarm lights that are turned on, that is, if a gas alarm signal is sent to the ESD. The alarms must also be detectable in the control room of the slider 10. The gas measurement must be given in the control chamber, for example in ppm. It would be advantageous if the factory included a fire and gas panel in the control room of the slider 10 to display all fire and gas alarms, as well as ventilation failures.

如以上提及的,該工廠包括多個煙霧探測儀以及VESDA檢測器。尤其是該等過程滑動件,例如滑動件1、2、3、4以及7包括使F2生產手動停止的裝置(例如,緊急按鈕)和/或啟動消滅火災的裝置的裝置。可以使用CC TV(閉路電視)來監控該工廠。它可以被用於監測到該工廠的通路、材料的卸載(例如便攜的HF罐的或者KOH溶液的)。As mentioned above, the plant includes a plurality of smoke detectors and a VESDA detector. Such slider particular process, e.g., 3, 4 and 7 the slider comprises means (e.g., emergency button) F 2 produced manually stopping means elimination of fire and / or start. The CC TV (Closed Circuit Television) can be used to monitor the plant. It can be used to monitor access to the plant, unloading of materials (such as portable HF tanks or KOH solutions).

安全儀器系統(SIS)(包括感測器、ESD系統以及安全致動器)被包括在這個工廠中。該SIS被設計為實現一安全完整性等級“2”。具體地說,在需要電動機或者電力負荷以便被包括作為一安全插裝的功能元件的一零件的地方,考慮了將該等電動機/負荷進行斷開的交替的或和獨立的裝置,例如藉由斷開該上游斷路器如果專用於該電動機/電負荷的接觸器或者斷路器沒有打開的話。Safety Instrumented Systems (SIS), including sensors, ESD systems, and safety actuators, are included in this facility. The SIS is designed to achieve a safety integrity level of "2". In particular, where a motor or electrical load is required to be included as a component of a securely inserted functional component, alternate or separate devices that disconnect the motor/load are contemplated, such as By disconnecting the upstream circuit breaker, if the contactor or circuit breaker dedicated to the motor/electrical load is not open.

一緊急發電機,較佳的是一供應100kVA的柴油發電機較佳的是被包含在該工廠中,如果一外部電力供應的被中斷了話。An emergency generator, preferably a 100 kVA diesel generator, is preferably included in the plant if an external power supply is interrupted.

如果該控制室包括對於單獨工作的操作員的一“失動”檢測(“dead man”detection)的話,它也是較佳的。It is also preferred if the control room includes a "dead man" detection for an operator working alone.

此外,較佳的是該控制室提供了關於風的方向以及風的速度的資料。Furthermore, it is preferred that the control room provides information about the direction of the wind and the speed of the wind.

用於一工廠(其容量為150噸/年)的該等被組裝的過程滑動件的占地面積係30 m‧9.2 m。其中用於實施項、用於維護和修理的人員面積以及入口間隙的滑動件,其整個尺寸係約39 m‧23 m。該等滑動件的高度可以是比標準(標準高度係64英寸)更高的。包括應急滌氣器的滑塊6A經常具有的不是標準的占地面積但是與對應的工廠的特定要求相適配。The assembled process slides for a factory (with a capacity of 150 tons/year) have an footprint of 30 m‧9.2 m. The slides used for the implementation, the area for maintenance and repair, and the entrance clearance are approximately 39 m‧23 m. The height of the sliders can be higher than the standard (standard height of 64 inches). The slider 6A, including the emergency scrubber, often has a standard footprint but is adapted to the specific requirements of the corresponding plant.

經常,該滑動件結構係一塗漆的鋼架,在該鋼架上所有的設備都固定了;它們被設計為用於戶外安裝。嵌板、門、以及屋頂,如果安裝在滑動件的外部結構的話,暗示了該等外部滑動件尺寸超過了該等標準海運集裝箱的尺寸。如果需要的話,該等滑動件係預製的,並且嵌板、門、以及屋頂在現場被對應地組裝到該等滑動件上。該等滑動件係錨接在一現有的混凝土厚片上的或者通過或在一特定的底架上。Often, the slider structure is a painted steel frame on which all of the equipment is secured; they are designed for outdoor installation. Panels, doors, and roofs, if mounted on the exterior structure of the slider, imply that the dimensions of the outer slides exceed the dimensions of the standard shipping containers. If desired, the sliders are prefabricated and the panels, doors, and roof are correspondingly assembled to the sliders in the field. The sliders are anchored to an existing concrete slab or passed through or on a particular chassis.

該等滑動件的優點係例如在車間試驗之前將它們製造、布管、佈線並且組裝在一起。如果將它們構造為使得該等滑動件之間的介面被最小化並且在對應滑動件中的所有部件對於維護、檢查或修理係盡可能容易地進入的,則是較佳的。The advantages of such sliders are, for example, they are manufactured, piped, routed and assembled together prior to workshop testing. It is preferred if they are constructed such that the interface between the sliders is minimized and all of the components in the corresponding slider are as easily accessible as possible for maintenance, inspection or repair.

該等滑動件的優點係安全方面,每週7天每天24小時高純度F2的可靠的F2生產。The advantages of these slides are the safety aspects of reliable F 2 production of high purity F 2 24 hours a day, 7 days a week.

以下,對由多個滑動件構成的一工廠的組裝和操作進行說明。Hereinafter, the assembly and operation of a factory composed of a plurality of sliders will be described.

如上述的該等滑動件係在一車間中進行組裝的;在一實施方式中,滑動件2的電解池係早已提供的、填充有電解質鹽的。這改進了安全性。該等滑動件在該車間中進行預試驗並且然後被運輸到需要藉由它們生產F2的設施中。在該設施中,較佳的是如果一混凝土厚片已經預先充分建立了,在其上就可以建築該F2生產工廠。The sliders as described above are assembled in a workshop; in one embodiment, the electrolytic cell of the slider 2 is already provided with an electrolyte salt. This improves security. Such pre-test slider in the workshop and then transported by them to the needs of production facilities in the F 2. In the facility, it is preferred that if a concrete slab has been sufficiently established in advance, the F 2 production plant can be constructed thereon.

該等滑動件係組裝的並且連接的。滑動件2包括形成單元室的6個電解池。在這種情況下,每個電解池包括26個陽極;其他多個例如多達80個陽極或者甚至更多,將是有可能的,如果希望的話。在連接之前或者之後,它們被砌在該地面上作為地震或者天氣預防措施測量。The sliders are assembled and connected. The slider 2 includes six electrolytic cells forming a unit cell. In this case, each electrolytic cell comprises 26 anodes; other multiples such as up to 80 anodes or even more, would be possible, if desired. They are built on the ground before or after the connection as an earthquake or weather prevention measure.

滑動件13用於所需要的化學品(例如,硫代硫酸鹽、氫氧化物和/或電解質鹽)的儲存室。The slider 13 is used in a storage chamber for a desired chemical (e.g., thiosulfate, hydroxide, and/or electrolyte salt).

該等內置的部件的可操作性較佳的是然後進行測試。The operability of these built-in components is preferably tested.

現在詳細地對該工廠的操作進行說明。The operation of the plant will now be described in detail.

提供了帶有6個池的工廠。這個工廠的標稱容量,如果運行每週7天每天24小時是約100噸/年的純的F2(12 kg/h,峰值20 kg/h)。該容量可以藉由加入兩個另外的電解池以及整流器或者整流器架來擴展。藉由加入另外的滑動件(另外的池空間以及整流器、另外的冷卻滑動件、另外的分析器)將容量擴展到300噸/年將是有可能的。罐(較佳的是其內部體積為1至20 m3,最佳的是其尺寸為1至3 m3並且填充有HF)在滑動件1中組裝並且連接到該等電解池上。在該工廠的最終組裝之前,粗的組合物KF‧2HF的電解質鹽已經填充到該等池中了。該等電解池的內含物被加熱到約80℃-120℃以便在其中熔化。來自滑動件1的蒸發器的HF被送料進入到該電解池中。中電壓從滑動件9A被供應到滑動件9B、被轉換成低電壓直電流,其電壓的範圍為8至12 V,並且電流穿過HF和熔融電解質鹽的熔融組合物,該熔融組合物被保持在80℃與120℃之間的範圍內的一溫度。一整流器可以被分配到每個池;較佳的是,一整流器被分配到每一陽極。尤其佳的是應用雙整流器;這種雙整流器可以用作兩個陽極。如果于每個池中存在26個陽極的話,那麼可以應用13個雙整流器就以便向該等陽極提供電流。以高於環境壓力的一壓力(例如,以7至10 m表壓)來操作該等池。在滑動件2的對應的電極隔室中形成了元素氟(F2)以及元素氫(H2)。A factory with 6 pools is available. The nominal capacity of this plant is approximately 100 tons/year of pure F 2 (12 kg/h, peak 20 kg/h) if operated 24 hours a day, 7 days a week. This capacity can be expanded by adding two additional electrolytic cells and a rectifier or rectifier frame. It would be possible to expand the capacity to 300 tons/year by adding additional slides (additional pool spaces and rectifiers, additional cooling slides, additional analyzers). The cans (preferably having an internal volume of 1 to 20 m 3 , preferably having a size of 1 to 3 m 3 and filled with HF) are assembled in the slider 1 and connected to the electrolytic cells. Prior to the final assembly of the plant, the electrolyte salt of the crude composition KF‧2HF has been filled into the cells. The contents of the electrolytic cells are heated to about 80 ° C - 120 ° C to melt therein. The HF from the evaporator of the slider 1 is fed into the electrolytic cell. The medium voltage is supplied from the slider 9A to the slider 9B, converted into a low voltage direct current, the voltage thereof is in the range of 8 to 12 V, and the current is passed through the molten composition of the HF and the molten electrolyte salt, and the molten composition is A temperature in the range between 80 ° C and 120 ° C is maintained. A rectifier can be distributed to each cell; preferably, a rectifier is assigned to each anode. It is especially preferred to use a dual rectifier; this double rectifier can be used as two anodes. If there are 26 anodes in each cell, then 13 dual rectifiers can be applied to supply current to the anodes. The cells are operated at a pressure above ambient pressure (e.g., at a gauge pressure of 7 to 10 m). Elemental fluorine (F 2 ) and elemental hydrogen (H 2 ) are formed in the corresponding electrode compartments of the slider 2 .

HF係有利地來提供的這樣使得在對應的池中的電解質鹽和HF的水平不會超過特定的上下水平。較佳的是,包含一或多個電解池的滑動件還包括確定池中的溫度、這個或該等池中的液體水平、壓力或壓差、陽極電流以及電壓和氣體溫度的感測器。該等池用具有約75℃至95℃、較佳的是75℃至85℃溫度的冷卻水進行冷卻。The HF system is advantageously provided such that the levels of electrolyte salts and HF in the corresponding pool do not exceed a particular upper and lower level. Preferably, the slider comprising one or more electrolytic cells further includes a sensor that determines the temperature in the cell, the level of liquid in the cell or the cells, pressure or differential pressure, anode current, and voltage and gas temperature. The cells are cooled with cooling water having a temperature of from about 75 ° C to 95 ° C, preferably from 75 ° C to 85 ° C.

將所形成的H2送到滑動件6B並且與一噴射洗滌器(帶有一水溶液,該水溶液包括按重量計0至約5%的水中的HF)接觸。將離開該滌氣器的氣體送到一填充柱的底部並且在其中與噴灑在該柱頂部的淡水接觸。離開該填充柱的氣體用氮氣稀釋了並且傳送進入到大氣中。The formed H 2 is sent to the slider 6B and brought into contact with a jet washer (with an aqueous solution comprising 0 to about 5% by weight of HF in water). The gas leaving the scrubber is sent to the bottom of a packed column where it is contacted with fresh water sprayed on top of the column. The gas leaving the packed column was diluted with nitrogen and passed to the atmosphere.

該工廠產生了約415 kg/天的F2The plant produced an F 2 of approximately 415 kg/day.

該等池中生產的F2首先藉由去除顆粒(主要是,夾帶的再固化的電解質鹽)來進行預純化。然後將粗F2流冷卻,由此一部分夾帶的HF濃縮並且可以被去除。然後,將粗F2藉由一膜片壓縮機進行壓縮至約3.5表壓的一壓力。將多餘對的NaF塔安裝在滑車上以便使它們係可移動的,尤其是針對以下的情況,該等NaF球粒需要完全交換(當進一步的再產生係不再可能的時候)。然後使被壓縮的F2穿過一阱並且藉由蒸發的液體N2以及氣態N2在其中冷卻至約-70℃。剩餘的HF在這個阱中藉由濃縮來去除。然後藉由使穿過包含NaF球粒的兩個吸收塔中的兩根管線中的一根管線而將任何殘餘的痕量的HF去除;該等線由於有時是多餘的,將該等NaF塔加熱至約350℃到400℃,並且使N2穿過它們而將吸收的HF去除並且使該等對應的塔再生。該等NaF塔中處於吸收模式的壓力係約3.5表壓。將離開這兩個NaF塔的F2氣流穿過兩個過濾器以便將任何固體(尤其是NaF)去除,該等過濾器較佳的是用蒙乃爾合金金屬製成的,並且該第二過濾器具有3 nm的孔直徑。第一塔的溫度係約100℃,第二塔的溫度係約30℃-40℃。對純化的F2連續採樣。Such a pool of F 2 is first produced by removing particles (mostly entrained resolidified electrolyte salt) pre-purification is performed. The crude F 2 stream is cooled, whereby a portion of the entrained concentrated HF and may be removed. Then, the crude F 2 by a diaphragm compressor a compressed to a pressure of about 3.5 psig. The excess pairs of NaF towers are mounted on the trolley to make them movable, especially for the case where the NaF pellets need to be completely exchanged (when further regeneration is no longer possible). The compressed F 2 is then passed through a trap and cooled by evaporation of liquid N 2 and gaseous N 2 to about -70 ° C. The remaining HF is removed by concentration in this trap. Any residual traces of HF are then removed by passing one of the two lines in the two absorption columns containing the NaF pellets; the lines are sometimes superfluous, The NaF column is heated to about 350 ° C to 400 ° C and N 2 is passed through them to remove the absorbed HF and regenerate the corresponding columns. The pressure in the absorption mode in the NaF columns is about 3.5 gauge. The F 2 gas stream leaving the two NaF columns is passed through two filters to remove any solids, especially NaF, which are preferably made of Monel metal and the second filter The device has a hole diameter of 3 nm. The temperature of the first column is about 100 ° C and the temperature of the second column is about 30 ° C to 40 ° C. The purified F 2 was continuously sampled.

根據一實施方式,將多個樣品送入到多槽FT-IR並且到一UV分析器中,如以上說明的。根據另一實施方式,應用單槽FT-IR用於選擇性地分析所純化的F2。分析資料可以線上發送到滑動件10A的控制室中的控制板中。According to one embodiment, multiple samples are fed into a multi-slot FT-IR and into a UV analyzer as explained above. According to another embodiment, application of single-slot for selectively FT-IR analysis The purified F 2. The analytical data can be sent online to the control panel in the control room of the slider 10A.

如果該等樣品的分析顯示,該等電解池中的一或多個產生了太不純的F2而不能用於半導體製造的目的,例如,包含了多得很的CF4或者更高的同系物(表明電解池故障),那麼這個或該等對應的樣品以及由電解池產生的F2穿過滑動件5中的F2滌氣器以及用於藉由包含硫代硫酸鈉的KOH溶液來銷毀的應急滌氣器。可替代地,可以將不純的F2收集用於純度是足夠的目的。如果該等樣品顯示所生產的F2與所希望的純度相對應,那麼就將該等樣品返回到F2生產線上。然後將該F2傳送到一儲存裝置中,該儲存裝置包括6個相同形狀的容器,它們各自具有一個1.3 m3的內部容積。該等圓柱體的任何一個可以是開放的並且由關閉閥門單獨地關閉。可替代地,通過一壓力控制迴路來將所生產的F2的壓力降低至約1.5表壓並且然後將其送至使用點,使用F2用於腔室清潔的平板顯示器製造工廠。使用一雙壁圍繞的管,其中在該內外管之間的空間包含著氮氣,並且使該F2穿過其內管。If the analysis of these samples shows that one or more of the electrolytic cells produce too impure F 2 and cannot be used for semiconductor manufacturing purposes, for example, contains much more CF 4 or higher homologues. (indicating that the cell is faulty), then this or the corresponding sample and the F 2 produced by the cell pass through the F 2 scrubber in the slide 5 and are used to destroy by the KOH solution containing sodium thiosulfate Emergency scrubber. Alternatively, impure F 2 collection can be used for the purpose that purity is sufficient. If such sample exhibits produced and F 2 corresponding to the desired degree of purity, then we will return to these samples F 2 line. The F is then transferred to a storage device 2, the storage device comprises a container 6 of the same shape, each having an internal volume of 1.3 m 3. Any of the cylinders may be open and individually closed by a closing valve. Alternatively, a pressure control loop via the F 2 produced pressure is reduced to about 1.5 psig and then sent to a point of use, the use of F 2 for chamber cleaning flat panel display manufacturing facility. Use of a double-walled tube surrounding in which the space between the inner and outer tubes contains a nitrogen, the F 2 and the inner tube therethrough.

在正常的操作中,該等關閉閥門係開放的並且在F2儲存單元與使用點之間的壓力差提供了一緩衝,該緩衝允許對遞送的氟氣體流的一平滑的控制,甚至用於使用點處的或者在F2產生單元的生產的中斷過程中可以獲得的不同消耗樣式。In normal operation, these lines open and close the valve to provide a pressure difference between F 2 and the point of the storage unit a buffer, the buffer allows a smooth control of the delivery of a fluorine gas flow, even for Different consumption patterns available at the point or during the interruption of the production of the F 2 generating unit.

若任何藉由引用結合在此的專利案、專利申請案以及公開物中的揭露內容與本申請案的說明相衝突的程度至它可能使一術語不清楚,則本說明應該優先。In the event that any disclosure of patents, patent applications, and publications incorporated herein by reference is inconsistent with the description of the present application to the extent that it may make the term unclear, this description should be preferred.

P...工廠P. . . factory

1...滑動件1. . . Slide

2...滑動件2. . . Slide

2A...子滑動件2A. . . Subslider

2B...子滑動件2B. . . Subslider

3...滑動件3. . . Slide

4...滑動件4. . . Slide

5...滑動件5. . . Slide

6...滑動件6. . . Slide

6A...子滑動件6A. . . Subslider

6B...子滑動件6B. . . Subslider

7...滑動件7. . . Slide

8...滑動件8. . . Slide

9...滑動件9. . . Slide

9A...子滑動件9A. . . Subslider

9B...子滑動件9B. . . Subslider

10...滑動件10. . . Slide

10A...子滑動件10A. . . Subslider

10B...子滑動件10B. . . Subslider

11...滑動件11. . . Slide

11a...自動扶梯和平臺11a. . . Escalators and platforms

11b...自動扶梯和平臺11b. . . Escalators and platforms

12...叉式起重機12. . . Forklift

13...貯料場13. . . Storage yard

14...緊急淋浴器14. . . Emergency shower

圖1示出了根據本發明的工廠的一實施方式,該設備具有一個有用的滑動件的安排。Figure 1 shows an embodiment of a factory according to the invention having a useful arrangement of sliders.

P...工廠P. . . factory

1...滑動件1. . . Slide

2...滑動件2. . . Slide

3...滑動件3. . . Slide

4...滑動件4. . . Slide

5...滑動件5. . . Slide

6A...子滑動件6A. . . Subslider

6B...子滑動件6B. . . Subslider

7...滑動件7. . . Slide

8...滑動件8. . . Slide

9A...子滑動件9A. . . Subslider

9B...子滑動件9B. . . Subslider

10A...子滑動件10A. . . Subslider

10B...子滑動件10B. . . Subslider

11a...自動扶梯和平臺11a. . . Escalators and platforms

11b...自動扶梯和平臺11b. . . Escalators and platforms

12...叉式起重機12. . . Forklift

13...貯料場13. . . Storage yard

14...緊急淋浴器14. . . Emergency shower

Claims (17)

一個氟氣體之製造工廠,其包括:-包括至少一個HF儲存槽的滑動安裝模組,表示為滑動件1,-包括至少一個產生F2的電解池之滑動安裝模組,表示為滑動件2,-表示為滑動件3之滑動安裝模組,其包括用於預冷卻粗質F2流的冷卻器,其中該冷卻器係連接至壓縮機,且該壓縮機連接至在低溫下操作的HF冷凝器,其中該HF冷凝器包含冷卻介質,其中該冷卻介質係為藉由混合液態N2和氣態N2所得的N2氣體,及-包括緩衝罐和遞送到使用點的供應管線之滑動安裝模組,表示為滑動件4。 Manufacturing plant of a fluorine gas, comprising: - at least one module is slidably mounted HF storage tank, expressed as a sliding member 1, - comprising at least one sliding mounting of the cell module F 2, showing the sliding member 2, - a sliding mounting module, shown as slide 3, comprising a cooler for pre-cooling the coarse F 2 stream, wherein the cooler is connected to a compressor and the compressor is connected to an HF condensation operating at low temperatures Wherein the HF condenser comprises a cooling medium, wherein the cooling medium is N 2 gas obtained by mixing liquid N 2 and gaseous N 2 , and - including a buffer tank and a sliding mounting mold for a supply line delivered to the point of use Group, denoted as slider 4. 如申請專利範圍第1項之工廠,其進一步包括:-滑動件模組9,其係將中電壓轉變至低電壓之變電站,和/或-滑動件模組10,其容納公用設施和便利設施。 The factory of claim 1, further comprising: a slider module 9, which is a substation that converts a medium voltage to a low voltage, and/or a slider module 10 that accommodates utilities and amenities . 如申請專利範圍第1項之工廠,其中該滑動件1中的HF儲存槽具有1至2m3的內部容積。 A factory according to claim 1, wherein the HF storage tank in the slider 1 has an internal volume of 1 to 2 m 3 . 如申請專利範圍第1項之工廠,其中滑動件2包括至少4個電解池,該電解池分別被分配到至少一個分開的整流器上。 A plant according to claim 1, wherein the sliding member 2 comprises at least four electrolytic cells, each of which is distributed to at least one of the separate rectifiers. 如申請專利範圍第1項之工廠,其中滑動件3包括用於使粗質F2氣體與液體HF接觸的HF洗滌器、從F2中去除 HF的冷凝器、以及至少一個從F2中吸收HF的吸收劑管柱。 A plant according to claim 1, wherein the sliding member 3 comprises an HF scrubber for contacting the crude F 2 gas with the liquid HF, a condenser for removing HF from the F 2 , and at least one absorption from the F 2 Absorbent column for HF. 如申請專利範圍第1項之工廠,其中滑動件4包括用於氟氣體儲存的多個空心體。 A factory according to claim 1, wherein the slider 4 comprises a plurality of hollow bodies for storage of fluorine gas. 如申請專利範圍第6項之工廠,其中每個空心體可以分開地從該工廠關閉。 A factory as claimed in claim 6, wherein each hollow body can be separately closed from the factory. 如申請專利範圍第1項之工廠,其另外包括冷卻水迴路的滑動安裝模組,表示為滑動件5,其中滑動件5包括至少2個冷卻水迴路以及該冷卻水的加熱和冷卻裝置。 A factory according to claim 1 further comprising a sliding mounting module of the cooling water circuit, designated as a sliding member 5, wherein the sliding member 5 comprises at least two cooling water circuits and heating and cooling means for the cooling water. 如申請專利範圍第1項之工廠,其另外包括處理廢氣的裝置之滑動安裝模組,表示為滑動件6,其中滑動件6包括包含緊急滌氣器的子滑動件6A,以及包含用於F2和H2的滌氣器的子滑動件6B。 A factory according to claim 1, further comprising a sliding mounting module for treating the exhaust gas, represented as a sliding member 6, wherein the sliding member 6 comprises a subslider 6A comprising an emergency scrubber, and comprising F for 2 and sub-slider 6B of the scrubber of H 2 . 如申請專利範圍第1項之工廠,其另外包括用於分析F2的裝置之滑動安裝模組,表示為滑動件7,其中滑動件7包括多槽FT-IR光譜儀以及隨意地紫外光譜儀,和/或其中滑動件4包括用於該氟的最終分析之單槽FT-IR。 The factory of claim 1, further comprising a sliding mounting module for analyzing the F 2 device, represented as a slider 7, wherein the slider 7 comprises a multi-slot FT-IR spectrometer and optionally an ultraviolet spectrometer, and / or wherein the slider 4 comprises a single slot FT-IR for the final analysis of the fluorine. 如申請專利範圍第1項之工廠,其另外包括操作該電解池的裝置之滑動安裝模組,表示為滑動件8,其中滑動件8包括多個整流器,其中整流器的數量與陽極的數量相對應;或者其中滑動件8包括多個雙整流器,其中該雙整流器分別提供電流至2個陽極。 A factory according to claim 1, further comprising a sliding mounting module for operating the electrolytic cell, represented as a sliding member 8, wherein the sliding member 8 comprises a plurality of rectifiers, wherein the number of rectifiers corresponds to the number of anodes Or wherein the slider 8 comprises a plurality of dual rectifiers, wherein the dual rectifiers respectively supply current to the two anodes. 如申請專利範圍第2項之工廠,其中滑動件9包括容納來電流、去電流以及旁路電流的中電壓電池之子滑動 件9A,以及容納低電壓的開關設備、緊急發電機、蓄電池充電站之滑動件9B。 A factory according to claim 2, wherein the slider 9 includes a sub-sliding of a medium voltage battery that accommodates current, current, and bypass current Piece 9A, and a sliding device 9B for accommodating a low voltage switching device, an emergency generator, and a battery charging station. 如申請專利範圍第2項之工廠,其中滑動件10包括容納包括實驗室的控制室之子滑動件10A,以及容納休息室的子滑動件10B。 A factory according to claim 2, wherein the slider 10 includes a sub-slider 10A that houses a control room including a laboratory, and a sub-slider 10B that houses the restroom. 如申請專利範圍第1項之工廠,其中在每個滑動件存在有至少一個緊急按鈕。 A factory as claimed in claim 1, wherein there is at least one emergency button in each of the sliders. 如申請專利範圍第1項之工廠,其包括地震檢波器。 For example, the factory of claim 1 includes a geophone. 如申請專利範圍第15項之工廠,其中該地震檢波器係強地動地震檢波器。 For example, the factory of claim 15 of the patent scope, wherein the geophone is a strong geophone. 如申請專利範圍第15或16項之工廠,其中該地震檢波器係連接到控制板並且觸發該工廠的關閉。 A plant of claim 15 or 16, wherein the geophone is coupled to the control panel and triggers shutdown of the plant.
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