EP1031533B1 - Liquid dispensing device and use for dispensing high purity liquid - Google Patents

Liquid dispensing device and use for dispensing high purity liquid Download PDF

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Publication number
EP1031533B1
EP1031533B1 EP19990403239 EP99403239A EP1031533B1 EP 1031533 B1 EP1031533 B1 EP 1031533B1 EP 19990403239 EP19990403239 EP 19990403239 EP 99403239 A EP99403239 A EP 99403239A EP 1031533 B1 EP1031533 B1 EP 1031533B1
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EP
European Patent Office
Prior art keywords
liquid
pressure
delivery system
delivery
distribution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP19990403239
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German (de)
French (fr)
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EP1031533A1 (en
Inventor
Georges Guarneri
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Liquide Electronics Systems SA
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Air Liquide Electronics Systems SA
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Publication date
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Publication of EP1031533A1 publication Critical patent/EP1031533A1/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B67—OPENING, CLOSING OR CLEANING BOTTLES, JARS OR SIMILAR CONTAINERS; LIQUID HANDLING
    • B67D—DISPENSING, DELIVERING OR TRANSFERRING LIQUIDS, NOT OTHERWISE PROVIDED FOR
    • B67D7/00—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes
    • B67D7/02—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring liquids other than fuel or lubricants
    • E—FIXED CONSTRUCTIONS
    • E03—WATER SUPPLY; SEWERAGE
    • E03C—DOMESTIC PLUMBING INSTALLATIONS FOR FRESH WATER OR WASTE WATER; SINKS
    • E03C1/00—Domestic plumbing installations for fresh water or waste water; Sinks
    • E03C1/12—Plumbing installations for waste water; Basins or fountains connected thereto; Sinks
    • E03C1/26—Object-catching inserts or similar devices for waste pipes or outlets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B67—OPENING, CLOSING OR CLEANING BOTTLES, JARS OR SIMILAR CONTAINERS; LIQUID HANDLING
    • B67D—DISPENSING, DELIVERING OR TRANSFERRING LIQUIDS, NOT OTHERWISE PROVIDED FOR
    • B67D7/00—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes
    • B67D7/02—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring liquids other than fuel or lubricants
    • B67D7/0238—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring liquids other than fuel or lubricants utilising compressed air or other gas acting directly or indirectly on liquids in storage containers
    • B67D7/0266—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring liquids other than fuel or lubricants utilising compressed air or other gas acting directly or indirectly on liquids in storage containers by gas acting directly on the liquid
    • B67D7/0272—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring liquids other than fuel or lubricants utilising compressed air or other gas acting directly or indirectly on liquids in storage containers by gas acting directly on the liquid specially adapted for transferring liquids of high purity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B67—OPENING, CLOSING OR CLEANING BOTTLES, JARS OR SIMILAR CONTAINERS; LIQUID HANDLING
    • B67D—DISPENSING, DELIVERING OR TRANSFERRING LIQUIDS, NOT OTHERWISE PROVIDED FOR
    • B67D7/00—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes
    • B67D7/02—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring liquids other than fuel or lubricants
    • B67D7/0277—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring liquids other than fuel or lubricants using negative pressure
    • B67D7/0283—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring liquids other than fuel or lubricants using negative pressure specially adapted for transferring liquids of high purity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B67—OPENING, CLOSING OR CLEANING BOTTLES, JARS OR SIMILAR CONTAINERS; LIQUID HANDLING
    • B67D—DISPENSING, DELIVERING OR TRANSFERRING LIQUIDS, NOT OTHERWISE PROVIDED FOR
    • B67D7/00—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes
    • B67D7/06—Details or accessories
    • B67D7/78—Arrangements of storage tanks, reservoirs or pipe-lines
    • E—FIXED CONSTRUCTIONS
    • E03—WATER SUPPLY; SEWERAGE
    • E03C—DOMESTIC PLUMBING INSTALLATIONS FOR FRESH WATER OR WASTE WATER; SINKS
    • E03C1/00—Domestic plumbing installations for fresh water or waste water; Sinks
    • E03C1/12—Plumbing installations for waste water; Basins or fountains connected thereto; Sinks
    • E03C1/14—Wash-basins connected to the waste-pipe
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/0318—Processes
    • Y10T137/0396—Involving pressure control
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/2931—Diverse fluid containing pressure systems
    • Y10T137/3115—Gas pressure storage over or displacement of liquid
    • Y10T137/3124—Plural units
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/2931—Diverse fluid containing pressure systems
    • Y10T137/3115—Gas pressure storage over or displacement of liquid
    • Y10T137/3127—With gas maintenance or application

Definitions

  • the present invention relates to a system for liquid distribution. It applies in particular to the distribution of ultra-pure chemicals, in particular for the microelectronics industry.
  • the pumped distribution generates bound particles to variations in pump pressure, and the pumps pose reliability issues.
  • tanks are at least 200 l. This leads to dimensions large cabinets, and the tanks must be able withstand the distribution pressure, of the order of 4 bars, or the vacuum.
  • the materials used include an inner shell in polyethylene (PE) plastic, perfluoroalkoxy (PFA) or polyvinylidene fluororide (PVDF), and an external reinforcement in fiberglass or stainless steel.
  • PE polyethylene
  • PFA perfluoroalkoxy
  • PVDF polyvinylidene fluororide
  • This design of the tanks can cause ionic contamination if the manufacturing is not perfectly under control, and security issues related to pressurization or vacuum for large volumes tanks.
  • the object of the invention is to provide a system for space-saving distribution, relatively easy to manufacture, minimizing the risk of contamination of the liquid and optimizing safety.
  • the invention also relates to the use of such a distribution system for the distribution of a ultra-pure liquid, in particular hydrogen peroxide, ammonia or hydrofluoric acid.
  • the distribution system shown in Figure 1 is intended to supply an ultra-pure liquid to a network user 100.
  • the system consists of an upstream part supply 1 and a downstream distribution part 2.
  • a sampling can 10 used to carry out analyzes of the conveyed liquid.
  • Line 14 is equipped with two filters 15A, 15B mounted in parallel, then a sampling container and 16, and it ends up at the user network 100.
  • Line 17 stuck on line 14 downstream filters 15A, 15B allows the recycling of liquid to the inlet of the tank 11, and another pipe 18 makes it possible to recycle excess liquid from user network 100 to the same location.
  • the installation also includes a number of known measurement and control devices per se and which have not been 'represented for the sake of clarity drawing.
  • the barrels 3A and 3B can have a volume of 100 to 20,000 liters, the tank 11, made of PE, PFA or PVDF slightly reinforced with fibers, a volume of 200 l to 5 m 3 , and the containers 12A and 12B have a much lower volume than the previous one, typically from 1 to 50 liters.
  • the filter 7 is a microfiltration member with membrane up to 0.2 ⁇ m
  • filter 8 provides filtration up to 0.1 ⁇ m
  • filters 15A and 15B filtration up to 0.05 ⁇ m.
  • each container 12A, 12B consists of a section of tube 23 made of PE, PFA or PVDF unreinforced, the thickness of which is adapted to withstand distribution pressure.
  • This tube is arranged vertically, its upper end is closed by a plug 24 connected to the associated nitrogen source 21A or 21B, and its lower end is closed by a second plug 25 to which is connected a connecting tee 26.
  • the two horizontal branches of this tee are connected respectively, upstream to a pipe 27 itself connected to the tube plunger 13, and downstream to a pipe 28 itself connected to line 14.
  • the size of the distribution part 2 is particularly reduced.
  • the gaseous sky of barrels 3A and 3B is maintained at slight overpressure, at a pressure less than 100 mbar by the device 4.
  • the pumped liquid by the pump 5 passes through the filters 7 and 8, and part of the liquid is eventually recycled via line 9.
  • the non-recycled liquid reaches the storage tank 11, via a second dip tube 29 which supplies it at source.
  • the gaseous sky of this tank is constantly maintained at a predetermined pressure P2, less than 500 mbar by source 20.
  • One of the two containers 12A, 12B is maintained at a positive pressure P4 or zero but less than pressure P2, by its source nitrogen 21B, and its outlet valve is closed while its inlet valve is open.
  • the other container 12A has its valve inlet valve closed, its outlet valve open, and it is maintained at a pressure P3 greater than P2 and equal to the distribution pressure by its nitrogen source 21A.
  • the container 12B is filled while the container 12A is used for distribution.
  • the pressures of the two containers are reversed, as well as the state of their inlet valves and outlet, so that container 12A fills while that the container 12B empties into the line of distribution 14.
  • the liquid thus distributed continuously undergoes the last filtration step in 15A and / or 15B, then is sent via line 14 to user network 100.
  • Ultrapure liquid can optionally be recycled in the tank 11, from the line 14 via the branch 17 and / or from network 100 via line 18.
  • a third dispensing container similar to containers 12A, 12B and mounted in parallel with them, as a container for help.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Public Health (AREA)
  • Water Supply & Treatment (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)
  • Pipeline Systems (AREA)
  • Loading And Unloading Of Fuel Tanks Or Ships (AREA)

Description

La présente invention est relative à un système de distribution de liquide. Elle s'applique en particulier à la distribution de produits chimiques ultra-purs, notamment destinés à l'industrie micro-électronique.The present invention relates to a system for liquid distribution. It applies in particular to the distribution of ultra-pure chemicals, in particular for the microelectronics industry.

Les pressions dont il est question ici sont des pressions relatives.The pressures discussed here are relative pressures.

L'évolution rapide de la micro-électronique vers une miniaturisation toujours plus poussée a des conséquences quant à la pureté des produits chimiques utilisés dans diverses phases de la fabrication des circuits intégrés. Il devient maintenant courant pour des produits chimiques comme le peroxyde d'hydrogène, l'ammoniaque, l'acide fluorhydrique de spécifier des teneurs en cations inférieures au ppb (partie par milliard), et des teneurs en particules inférieures à 500 particules de 0,2 micromètres par litre.The rapid evolution of microelectronics towards a ever-increasing miniaturization has consequences as to the purity of the chemicals used in various stages in the manufacture of integrated circuits. he is now becoming common for chemicals like hydrogen peroxide, ammonia, hydrofluoric acid to specify cation contents lower than ppb (part by billion), and particle contents less than 500 particles of 0.2 micrometers per liter.

Ces produits chimiques liquides dits ultra-purs, utilisés par exemple dans les procédés de nettoyage, sont distribués au-delà d'une certaine consommation par des systèmes de distribution centralisés. Ces systèmes comprennent les fonctions suivantes :

  • soutirage du produit à partir d'une source de produit fournisseur, ou réservoir d'alimentation, vers une cuve de stockage, à travers des étages de filtration pour améliorer les spécifications particulaires du produit, avec recirculation éventuelle à travers des étages de filtration pour améliorer les spécifications particulaires du produit tout en maintenant la qualité ionique,;
  • distribution du produit à partir de la cuve de stockage vers un réseau utilisateur via un étage de filtration pour améliorer les specifications particulaires du produit.
These so-called ultra-pure liquid chemicals, used for example in cleaning processes, are distributed beyond a certain consumption by centralized distribution systems. These systems include the following functions:
  • withdrawal of the product from a source of supplying product, or supply tank, to a storage tank, through filtration stages to improve the particulate specifications of the product, with possible recirculation through filtration stages to improve the particle specifications of the product while maintaining the ionic quality;
  • distribution of the product from the storage tank to a user network via a filtration stage to improve the specific product specifications.

Différents moyens sont connus pour véhiculer le produit à partir de la cuve de stockage. Ces moyens utilisent soit des pompes, soit la pression, soit le vide, ou encore des combinaisons de ces moyens (voir par exemple les brevets US-A-5 330 072, US-A- 5 417 346 et US-A- 5 772 447).Various means are known to convey the produced from the storage tank. These means use either pumps, pressure or vacuum, or combinations of these means (see for example licences US-A-5,330,072, US-A- 5,417,346 and US-A- 5,772,447).

Ces moyens présentent certains inconvénients : These means have certain drawbacks:

La distribution pompée génère des particules liées aux variations de pression des pompes, et les pompes posent des problèmes de fiabilité.The pumped distribution generates bound particles to variations in pump pressure, and the pumps pose reliability issues.

La distribution par pression et vide pose des problèmes de fiabilité liés à la non-compatibilité des vannes à membranes dans le système avec le vide, alors que ces vannes à membranes sont les seules compatibles avec les niveaux de pureté exigés.Pressure and vacuum distribution poses reliability problems linked to the non-compatibility of diaphragm valves in the system with vacuum, while these diaphragm valves are the only ones compatible with purity levels required.

Les systèmes de distribution classiques à pression utilisent au moins deux cuves de stockage d'un volume unitaire important, correspondant typiquement à la consommation journalière des équipements. Typiquement, les cuves sont au minimum de 200 l. Ceci entraíne des dimensions d'armoire importantes, et les cuves doivent pouvoir supporter la pression de distribution, de l'ordre de 4 bars, ou le vide. Pour cela, dans le cas des produits corrosifs, les matériaux utilisés comprennent une coquille intérieure en matière plastique du type polyéthylène (PE), perfluoroalkoxy (PFA) ou fluororure de polyvinylidène (PVDF), et un renforcement extérieur en fibre de verre ou en acier inoxydable. Cette conception des cuves peut entraíner des contaminations ioniques si les fabrications ne sont pas parfaitement maítrisées, et des problèmes de sécurité liés à la pressurisation ou au vide pour les cuves de gros volumes.Conventional pressure distribution systems use at least two volume storage tanks significant unit, typically corresponding to the daily consumption of equipment. Typically, tanks are at least 200 l. This leads to dimensions large cabinets, and the tanks must be able withstand the distribution pressure, of the order of 4 bars, or the vacuum. For this, in the case of corrosive products, the materials used include an inner shell in polyethylene (PE) plastic, perfluoroalkoxy (PFA) or polyvinylidene fluororide (PVDF), and an external reinforcement in fiberglass or stainless steel. This design of the tanks can cause ionic contamination if the manufacturing is not perfectly under control, and security issues related to pressurization or vacuum for large volumes tanks.

L'invention a pour but de fournir un système de distribution d'encombrement réduit, relativement facile à fabriquer, minimisant les risques de contamination du liquide et optimisant la sécurité.The object of the invention is to provide a system for space-saving distribution, relatively easy to manufacture, minimizing the risk of contamination of the liquid and optimizing safety.

A cet effet, l'invention a pour objet un système de distribution de liquide qui comprend :

  • - un réservoir d'alimentation contenant un liquide à distribuer, muni de moyens de maintien d'un ciel gazeux sous une surpression inférieure à une première pression prédéterminée P1;
  • une cuve intermédiaire de stockage munie de moyens de maintien d'un ciel gazeux sous une pression intermédiaire prédéterminée P2 > P1;
  • des moyens de transfert du liquide du réservoir d'alimentation à la cuve intermédiaire;
  • au moins deux récipients de distribution ayant un volume très inférieur à celui de la cuve intermédiaire, reliés, en parallèle, en amont à une sortie de liquide de cette dernière et en aval à une conduite de distribution du liquide à un réseau utilisateur; et
  • des moyens de commande pour appliquer individuellement à chaque récipient soit une pression de distribution P3 > P2, soit une pression de remplissage P4 < P2.
To this end, the invention relates to a liquid distribution system which comprises:
  • a supply tank containing a liquid to be dispensed, provided with means for maintaining a gaseous sky under an overpressure less than a first predetermined pressure P1;
  • an intermediate storage tank provided with means for maintaining a gaseous sky under a predetermined intermediate pressure P2>P1;
  • means for transferring the liquid from the supply tank to the intermediate tank;
  • at least two distribution containers having a volume much smaller than that of the intermediate tank, connected, in parallel, upstream to a liquid outlet from the latter and downstream to a pipe for distributing the liquid to a user network; and
  • control means for individually applying to each container either a dispensing pressure P3> P2, or a filling pressure P4 <P2.

Le système de distribution suivant l'invention peut comporter une ou plusieurs des caractéristiques suivantes, prises isolément ou suivant toutes leurs combinaisons techniquement possibles :

  • le système comprend trois récipients de distribution montés en parallèle;
  • les moyens de transfert et/ou la conduite de distribution sont équipés de moyens de filtration du liquide;
  • lesdits moyens de maintien et lesdits moyens de commande comprennent des sources de gaz d'inertage, notamment d'azote, équipées de moyens de régulation de pression;
  • le système de distribution comprend une conduite de recyclage de liquide de la conduite de distribution à l'entrée de la cuve de stockage;
  • le système de distribution comprend une conduite de recyclage de liquide du réseau utilisateur à l'entrée de la cuve de stockage;
  • chaque récipient de distribution est constitué par un tronçon de tube vertical obturé à son extrémité inférieure par un té d'alimentation et d'évacuation et à son extrémité supérieure par un bouchon équipé d'une entrée de gaz de pressurisation;
  • la pression P1 est égale à 100 mbars environ et/ou la pression P2 est comprise entre 100 et 500 mbars environ et/ou la pression P3 est comprise entre 500 mbars et 6 bars environ; et
  • les volumes de la cuve de stockage et de chaque récipient de distribution sont respectivement compris entre 200 1 et 5 m3 et entre 1 et 50 1.
The distribution system according to the invention may include one or more of the following characteristics, taken individually or according to all their technically possible combinations:
  • the system comprises three distribution containers mounted in parallel;
  • the transfer means and / or the distribution pipe are equipped with liquid filtration means;
  • said holding means and said control means comprise sources of inerting gas, in particular nitrogen, equipped with pressure regulation means;
  • the distribution system comprises a liquid recycling pipe from the distribution pipe to the inlet of the storage tank;
  • the distribution system comprises a pipe for recycling liquid from the user network to the inlet of the storage tank;
  • each distribution container is constituted by a section of vertical tube closed at its lower end by a supply and discharge tee and at its upper end by a plug fitted with a pressurizing gas inlet;
  • the pressure P1 is equal to approximately 100 mbar and / or the pressure P2 is between 100 and 500 mbar approximately and / or the pressure P3 is between 500 mbar and approximately 6 bar; and
  • the volumes of the storage tank and of each distribution container are respectively between 200 1 and 5 m 3 and between 1 and 50 1.

L'invention a également pour objet l'utilisation d'un tel système de distribution pour la distribution d'un liquide ultra-pur, notamment de peroxyde d'hydrogène, d'ammoniaque ou d'acide fluorhydrique.The invention also relates to the use of such a distribution system for the distribution of a ultra-pure liquid, in particular hydrogen peroxide, ammonia or hydrofluoric acid.

Un exemple de réalisation va maintenant être décrit en regard des dessins annexés, sur lesquels :

  • la Figure 1 représente schématiquement un système de distribution de liquide ultra-pur conforme à l'invention; et
  • la Figure 2 représente un mode de réalisation avantageux d'une partie du système de la Figure 1.
An exemplary embodiment will now be described with reference to the appended drawings, in which:
  • Figure 1 schematically shows an ultra-pure liquid distribution system according to the invention; and
  • Figure 2 shows an advantageous embodiment of part of the system of Figure 1.

Le système de distribution représenté sur la Figure 1 est destiné à fournir un liquide ultra-pur à un réseau utilisateur 100. Le système est constitué d'une partie amont d'alimentation 1 et d'une partie aval de distribution 2.The distribution system shown in Figure 1 is intended to supply an ultra-pure liquid to a network user 100. The system consists of an upstream part supply 1 and a downstream distribution part 2.

La partie amont comprend, d'amont en aval :

  • deux réservoirs ou fûts d'alimentation 3A, 3B, disposés en parallèle et utilisés successivement. Chacun de ces fûts contient le liquide à distribuer, mais n'ayant pas la très basse teneur en particules désirée;
  • un dispositif 4 de maintien dans les deux fûts d'une légère surpression gazeuse inférieure à une pression P1 prédéterminée. La pression P1 est typiquement comprise entre 50 et 100 mbar. Le dispositif 4 comprend une alimentation en azote 104, un évent 105 et un régulateur 106 adapté pour relier le ciel gazeux des fûts 3A et 3B soit à la source 104, soit à l'évent 105. Des dispositifs de ce type sont disponibles dans le commerce;
  • une pompe de circulation 5;
  • un pot dégazeur 6 adapté pour protéger contre l'assèchement les filtres disposés en aval;
  • un premier filtre 7;
  • un deuxième filtre 8;
  • entre les deux filtres 7 et 8, une conduite de piquage 9, équipée d'une vanne, pour le recyclage de liquide dans les fûts 3A et 3B.
The upstream part includes from upstream to downstream:
  • two supply tanks or drums 3A, 3B, arranged in parallel and used successively. Each of these drums contains the liquid to be dispensed, but not having the very low particle content desired;
  • a device 4 for maintaining in the two barrels a slight gas overpressure less than a predetermined pressure P1. The pressure P1 is typically between 50 and 100 mbar. The device 4 comprises a nitrogen supply 104, a vent 105 and a regulator 106 adapted to connect the gaseous headspace of the barrels 3A and 3B either to the source 104 or to the vent 105. Devices of this type are available in the trade;
  • a circulation pump 5;
  • a degasser pot 6 adapted to protect against drying the filters arranged downstream;
  • a first filter 7;
  • a second filter 8;
  • between the two filters 7 and 8, a tapping pipe 9, equipped with a valve, for recycling liquid in drums 3A and 3B.

On a également représenté, an aval du filtre 8, un bidon de prélèvement 10 servant à effectuer des analyses du liquide véhiculé.Also shown, downstream of the filter 8, a sampling can 10 used to carry out analyzes of the conveyed liquid.

La partie de distribution 2 est constituée, d'amont en aval :

  • d'une cuve de stockage 11;
  • de deux récipients de distribution 12A, 12B montés en parallèle. Ces récipients sont reliés, en amont, à un tube plongeur 13 de sortie de liquide de la cuve 11 et, en aval, à une conduite 14 de distribution du liquide.
The distribution part 2 consists, from upstream to downstream:
  • a storage tank 11;
  • two distribution containers 12A, 12B mounted in parallel. These containers are connected, upstream, to a dip tube 13 for leaving the liquid from the tank 11 and, downstream, to a pipe 14 for distributing the liquid.

La conduite 14 est équipée de deux filtres 15A, 15B montés en parallèle, puis d'un bidon de prélèvement et d'analyse 16, et elle aboutit au réseau utilisateur 100.Line 14 is equipped with two filters 15A, 15B mounted in parallel, then a sampling container and 16, and it ends up at the user network 100.

Une conduite 17 piquée sur la conduite 14 en aval des filtres 15A, 15B permet de recycler du liquide à l'entrée de la cuve 11, et une autre conduite 18 permet de recycler du liquide en excès du réseau utilisateur 100 vers le même emplacement.Line 17 stuck on line 14 downstream filters 15A, 15B allows the recycling of liquid to the inlet of the tank 11, and another pipe 18 makes it possible to recycle excess liquid from user network 100 to the same location.

On a également représenté sur la Figure 1 divers accessoires :

  • plusieurs sources 19 d'eau déionisée, servant au rinçage du système;
  • une source 20 d'alimentation régulée en azote du ciel gazeux de la cuve 11, et des sources 21A et 21B d'alimentation régulée en azote des récipients 12A et 12B respectivement;
  • un compteur de particules 22 branché sur la conduite 14 en aval du piquage 17; et
  • un certain nombre de vannes, qui permettent de mettre en oeuvre le fonctionnement qui sera décrit ci-dessous.
Various accessories have also been shown in Figure 1:
  • several sources 19 of deionized water, used for flushing the system;
  • a source 20 of regulated supply of nitrogen from the gas overhead of the tank 11, and sources 21A and 21B of regulated supply of nitrogen to the containers 12A and 12B respectively;
  • a particle counter 22 connected to the pipe 14 downstream of the tap 17; and
  • a certain number of valves, which make it possible to implement the operation which will be described below.

Bien entendu, l'installation comporte par ailleurs un certain nombre d'organes de mesure et de commande, connus en soi et qui n'ont pas été' représentés pour la clarté du dessin.Of course, the installation also includes a number of known measurement and control devices per se and which have not been 'represented for the sake of clarity drawing.

A titre d'exemple, les fûts 3A et 3B peuvent avoir un volume de 100 à 20 000 litres, la cuve 11, réalisée en PE, PFA ou PVDF légèrement renforcée de fibres, un volume de 200 l à 5 m3, et les récipients 12A et 12B un volume très inférieur eu précédent, typiquement de 1 à 50 litres.For example, the barrels 3A and 3B can have a volume of 100 to 20,000 liters, the tank 11, made of PE, PFA or PVDF slightly reinforced with fibers, a volume of 200 l to 5 m 3 , and the containers 12A and 12B have a much lower volume than the previous one, typically from 1 to 50 liters.

Le filtre 7 est un organe de microfiltration à membrane jusqu'à 0,2 µm, le filtre 8 assure une filtration jusqu'à 0,1 µm, et les filtres 15A et 15B une filtration jusqu'à 0,05 µm.The filter 7 is a microfiltration member with membrane up to 0.2 µm, filter 8 provides filtration up to 0.1 µm, and filters 15A and 15B filtration up to 0.05 µm.

Dans un mode de réalisation particulièrement avantageux représenté à la Figure 2, chaque récipient 12A, 12B est constitué d'un tronçon de tube 23 en PE, PFA ou PVDF non renforcé, dont l'épaisseur est adaptée pour résister à la pression de distribution. Ce tube est disposé verticalement, son extrémité supérieure est obturée par un bouchon 24 relié à la source d'azote associée 21A ou 21B, et son extrémité inférieure est obturée par un second bouchon 25 auquel est raccordé un té de raccordement 26. Les deux branches horizontales de ce té sont reliées respectivement, vers l'amont à une conduite 27 elle-même reliée au tube plongeur 13, et vers l'aval à une conduite 28 elle-même reliée à la conduite 14.In a particularly embodiment advantageous shown in FIG. 2, each container 12A, 12B consists of a section of tube 23 made of PE, PFA or PVDF unreinforced, the thickness of which is adapted to withstand distribution pressure. This tube is arranged vertically, its upper end is closed by a plug 24 connected to the associated nitrogen source 21A or 21B, and its lower end is closed by a second plug 25 to which is connected a connecting tee 26. The two horizontal branches of this tee are connected respectively, upstream to a pipe 27 itself connected to the tube plunger 13, and downstream to a pipe 28 itself connected to line 14.

Un tel mode de réalisation est peu coûteux et très fiable, et il en est de même de la cuve 11, qui ne doit supporter que la pression P2, inférieure à 500 mbar.Such an embodiment is inexpensive and very reliable, and the same is true of the tank 11, which must not bear that pressure P2, less than 500 mbar.

De plus, l'encombrement de la partie de distribution 2 est particulièrement réduit.In addition, the size of the distribution part 2 is particularly reduced.

En fonctionnement, le ciel gazeux des fûts 3A et 3B est maintenu en légère surpression, à une pression inférieure à 100 mbar, par le dispositif 4. Le liquide pompé par la pompe 5 traverse les filtres 7 et 8, et une partie du liquide est éventuellement recyclé via la conduite 9. Le liquide non recyclé parvient dans la cuve de stockage 11, via un second tube plongeur 29 qui l'alimente en source.In operation, the gaseous sky of barrels 3A and 3B is maintained at slight overpressure, at a pressure less than 100 mbar by the device 4. The pumped liquid by the pump 5 passes through the filters 7 and 8, and part of the liquid is eventually recycled via line 9. The non-recycled liquid reaches the storage tank 11, via a second dip tube 29 which supplies it at source.

Le ciel gazeux de cette cuve est constamment maintenu à une pression P2 prédéterminée, inférieure à 500 mbar, par la source 20.The gaseous sky of this tank is constantly maintained at a predetermined pressure P2, less than 500 mbar by source 20.

L'un des deux récipients 12A, 12B, par exemple le récipient 12B, est maintenu à une pression P4 positive ou nulle mais inférieure à la pression P2, par sa source d'azote 21B, et sa vanne de sortie est fermée tandis que sa vanne d'entrée est ouverte. L'autre récipient 12A a sa vanne d'entrée fermée, sa vanne de sortie ouverte, et il est maintenu à une pression P3 supérieure à P2 et égale à la pression de distribution par sa source d'azote 21A.One of the two containers 12A, 12B, for example the container 12B, is maintained at a positive pressure P4 or zero but less than pressure P2, by its source nitrogen 21B, and its outlet valve is closed while its inlet valve is open. The other container 12A has its valve inlet valve closed, its outlet valve open, and it is maintained at a pressure P3 greater than P2 and equal to the distribution pressure by its nitrogen source 21A.

Ainsi, le récipient 12B se remplit pendant que le récipient 12A est utilisé pour la distribution. Lorsque le niveau du liquide dans le récipient 12A est descendu jusqu'à un seuil prédéterminé, les pressions des deux récipients sont inversées, ainsi que l'état de leurs vannes d'entrée et de sortie, de sorte que le récipient 12A se remplit tandis que le récipient 12B se vide dans la conduite de distribution 14.Thus, the container 12B is filled while the container 12A is used for distribution. When the liquid level in container 12A has gone down to a predetermined threshold, the pressures of the two containers are reversed, as well as the state of their inlet valves and outlet, so that container 12A fills while that the container 12B empties into the line of distribution 14.

Le liquide ainsi distribué en continu subit la dernière étape de filtration en 15A et/ou 15B, puis est envoyé par la conduite 14 au réseau utilisateur 100.The liquid thus distributed continuously undergoes the last filtration step in 15A and / or 15B, then is sent via line 14 to user network 100.

Du liquide ultra-pur peut éventuellement être recyclé dans la cuve 11, à partir de la conduite 14 via le piquage 17 et/ou à partir du réseau 100 via la conduite 18.Ultrapure liquid can optionally be recycled in the tank 11, from the line 14 via the branch 17 and / or from network 100 via line 18.

En variante, il peut être prévu un troisième récipient de distribution, analogue aux récipients 12A, 12B et monté en parallèle avec eux, à titre de récipient de secours.Alternatively, there may be a third dispensing container, similar to containers 12A, 12B and mounted in parallel with them, as a container for help.

Claims (10)

  1. Liquid delivery system, characterized in that it comprises:
    a feed reservoir (3A, 3B) containing a liquid to be delivered, provided with means (4) for maintaining a gas headspace at an overpressure below a first predetermined pressure P1;
    an intermediate storage tank (11) provided with means (20) for maintaining a gas headspace at a predetermined intermediate pressure P2 > P1;
    means (5 to 8) for transferring the liquid from the feed reservoir to the intermediate tank;
    at least two delivery containers (12A, 12B) having a volume very much less than that of the intermediate tank, the said containers being connected, in parallel, upstream to a liquid outlet (13) of the latter and downstream to a line (14) for delivering the liquid to a user network (100); and
    control means (21A, 21B) for applying, to each delivery container individually, either a delivery pressure P3 > P2 or a fill pressure P4 < P2.
  2. Fluid delivery system according to Claim 1, characterized in that it comprises three delivery containers mounted in parallel.
  3. Fluid delivery system according to Claim 1 or 2, characterized in that the transfer means and/or the delivery line are equipped with liquid filtration means (7, 8, 15A, 15B).
  4. Fluid delivery system according to any one of Claims 1 to 3, characterized in that the said maintaining means (4, 20) and the said control means (21A, 21B) comprise sources of inerting gas, especially nitrogen, the said sources being equipped with pressure regulation means.
  5. Fluid delivery system according to any one of Claims 1 to 4, characterized in that it includes a line (17) for recycling liquid from the delivery line (14) to the inlet of the storage tank (11).
  6. Fluid delivery system according to any one of Claims 1 to 5, characterized in that it includes a line (18) for recycling liquid from the user network (100) to the inlet of the storage tank (11).
  7. Fluid delivery system according to any one of Claims 1 to 6, characterized in that each delivery container (12A, 12B) is formed by a vertical tube portion (23) closed off at its lower end by a feed/discharge tee (26) and at its upper end by a plug (24) equipped with a pressurizing gas inlet.
  8. Liquid delivery system according to any one of Claims 1 to 7, characterized in that the pressure P1 is equal to 100 mbar approximately and/or the pressure P2 is between 100 and 500 mbar approximately and/or the pressure P3 is between 500 mbar and 6 bar approximately.
  9. Liquid delivery system according to any one of Claims 1 to 8, characterized in that the volumes of the storage tank (11) and of each delivery container (12A, 12B) are between 200 l and 5 m3 and between 1 and 50 l, respectively.
  10. Use of a liquid delivery system according to any one of Claims 1 to 9 for the delivery of an ultrapure liquid, especially hydrogen peroxide, aqueous ammonia or hydrofluoric acid.
EP19990403239 1999-02-26 1999-12-21 Liquid dispensing device and use for dispensing high purity liquid Expired - Lifetime EP1031533B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9902467A FR2790253B1 (en) 1999-02-26 1999-02-26 LIQUID DISPENSING SYSTEM AND ITS USE FOR DISPENSING ULTRA-PUR LIQUID
FR9902467 1999-02-26

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EP1031533A1 EP1031533A1 (en) 2000-08-30
EP1031533B1 true EP1031533B1 (en) 2003-10-15

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US (1) US6267132B1 (en)
EP (1) EP1031533B1 (en)
JP (1) JP2000249299A (en)
KR (1) KR100668392B1 (en)
DE (1) DE69912089T2 (en)
FR (1) FR2790253B1 (en)
SG (1) SG76001A1 (en)
TW (1) TW418299B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100668392B1 (en) * 1999-02-26 2007-01-16 레르 리키드 쏘시에떼 아노님 뿌르 레드 에렉스뿔라따시옹 데 프로세데 조르즈 클로드 Liquid delivery system

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6299753B1 (en) * 1999-09-01 2001-10-09 Applied Materials, Inc. Double pressure vessel chemical dispenser unit
US6953047B2 (en) * 2002-01-14 2005-10-11 Air Products And Chemicals, Inc. Cabinet for chemical delivery with solvent purging
US20030185690A1 (en) * 2002-03-28 2003-10-02 Mindi Xu Systems and methods for transferring and delivering a liquid chemical from a source to an end use station
US6648034B1 (en) * 2002-05-23 2003-11-18 Air Products And Chemicals, Inc. Purgeable manifold for low vapor pressure chemicals containers
US7172096B2 (en) * 2004-11-15 2007-02-06 Advanced Technology Materials, Inc. Liquid dispensing system
FR2880011B1 (en) * 2004-12-23 2007-03-30 Air Liquide Electronics Sys SYSTEM FOR DISTRIBUTING CHEMICAL LIQUIDS
MY169584A (en) 2005-04-25 2019-04-22 Entegris Inc Liner-based liquid storage and dispensing system with empty detection capability
CN102101634B (en) * 2005-06-06 2014-12-17 高级技术材料公司 Fluid storage and dispensing systems and processes
US20070215639A1 (en) * 2006-02-15 2007-09-20 Roberts Benjamin R Method and Apparatus for Dispensing Liquid with Precise Control
JP4697882B2 (en) * 2006-05-19 2011-06-08 東京エレクトロン株式会社 Treatment liquid supply apparatus, treatment liquid supply method, and treatment liquid supply control program
US20090107562A1 (en) * 2007-10-29 2009-04-30 Ruibo Wang Pre-pressurized self-balanced negative-pressure-free water-supply apparatus
RU2497035C2 (en) * 2008-06-25 2013-10-27 Басф Се Method of preventing backflow in transfer of fluid
KR101657733B1 (en) 2009-07-09 2016-09-20 어드밴스드 테크놀러지 머티리얼즈, 인코포레이티드 Substantially rigid collapsible liner and flexible gusseted or non-gusseted liners and methods of manufacturing the same and methods for limiting choke-off in liners
WO2011085012A2 (en) 2010-01-06 2011-07-14 Advanced Technology Materials, Inc. Liquid dispensing systems with gas removal and sensing capabilities
WO2012071370A2 (en) 2010-11-23 2012-05-31 Advanced Technology Materials, Inc. Liner-based dispenser
FR2969994B1 (en) * 2011-01-05 2013-02-08 Hypred DEVICE FOR CONNECTING A STORAGE TANK TO A POWER SUPPLY AND METHOD FOR MANAGING SUCH CONNECTION
WO2012118527A1 (en) 2011-03-01 2012-09-07 Advanced Technology Materials, Inc. Nested blow molded liner and overpack and methods of making same
CN102563350B (en) * 2012-03-07 2013-11-27 北京航空航天大学 Large-sized double-heat-sink closed liquid nitrogen delivery system and working method thereof
US9605346B2 (en) * 2014-03-28 2017-03-28 Lam Research Corporation Systems and methods for pressure-based liquid flow control
CN104373817A (en) * 2014-11-05 2015-02-25 东晶锐康晶体（成都）有限公司 IPA supply and recovery device
US10363543B2 (en) * 2016-04-19 2019-07-30 General Electric Company Gas driven fluid transport
CN112368404A (en) 2018-06-29 2021-02-12 应用材料公司 Liquid lithium supply and conditioning
CN114394570B (en) * 2022-02-14 2023-05-26 连云港石化有限公司 Non-volatile chemical liquid conveying system and automatic control method

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5417346A (en) 1990-09-17 1995-05-23 Applied Chemical Solutions Process and apparatus for electronic control of the transfer and delivery of high purity chemicals
US5148945B1 (en) * 1990-09-17 1996-07-02 Applied Chemical Solutions Apparatus and method for the transfer and delivery of high purity chemicals
US5556002A (en) * 1995-02-03 1996-09-17 Abc Techcorp Measured liquid dispensing system
JP3533512B2 (en) * 1995-04-26 2004-05-31 株式会社荏原製作所 Liquefied gas supply system
US5772447A (en) 1996-02-26 1998-06-30 Koontat Development Co. Ltd. Pivoting electrical plug
US5832948A (en) * 1996-12-20 1998-11-10 Chemand Corp. Liquid transfer system
JP3546121B2 (en) * 1997-02-25 2004-07-21 三菱重工業株式会社 Fluid pressure control device in pipeline
FR2790253B1 (en) * 1999-02-26 2001-04-20 Air Liquide Electronics Sys LIQUID DISPENSING SYSTEM AND ITS USE FOR DISPENSING ULTRA-PUR LIQUID

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100668392B1 (en) * 1999-02-26 2007-01-16 레르 리키드 쏘시에떼 아노님 뿌르 레드 에렉스뿔라따시옹 데 프로세데 조르즈 클로드 Liquid delivery system

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Publication number Publication date
FR2790253B1 (en) 2001-04-20
FR2790253A1 (en) 2000-09-01
EP1031533A1 (en) 2000-08-30
KR100668392B1 (en) 2007-01-16
DE69912089T2 (en) 2004-07-22
DE69912089D1 (en) 2003-11-20
TW418299B (en) 2001-01-11
US6267132B1 (en) 2001-07-31
SG76001A1 (en) 2000-10-24
JP2000249299A (en) 2000-09-12
KR20000076712A (en) 2000-12-26

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