FR2936038A1 - MINIATURIZED INSTALLATION FOR MANUFACTURING SPECIAL GAS MIXTURES. - Google Patents

Abstract

Application relating to the filling plant for gas cylinders with pure gases and / or pure gas mixtures comprising: - a gas selection and / or gas mixture manufacturing equipment intended to be introduced into a gas cylinder - Apparatus for analyzing the composition of said mixtures or said pure gases; characterized in that said installation is integrally contained in a transportable container whose floor area is less than 45m2, preferably the floor area is between 34 m2 and 40 m2.

Description

The present invention relates to a miniaturized bottle filling plant with pure industrial gases and / or mixtures and a miniaturized plant for manufacturing special gas mixtures. Said filling bottles with pure industrial gases and / or mixtures uses gases such as: - those extracted from air (N2, Ar, 02), helium, hydrogen, and mixtures thereof percent concentrations with other gases, when the bottles are filled batchwise (several bottles at a time). - carbon dioxide or nitrogen hemioxide whose bottles are filled by weighing, one bottle at a time. Special gas mixtures are mixtures of compressed or liquefied gases in gas cylinders, with characteristics such as, for example: - a high concentration accuracy of the constituents; a large number of constituents, sometimes several tens, such as, for example, hydrocarbon mixtures used in refineries and petrochemicals; a difficult maintenance of the stability of the concentration of the constituents when they are reactive with respect to the walls of the bottle and this especially as their concentration is low. These are very precise mixtures of composition and / or containing very low levels of components up to the level of parts per million or ppm. These characteristics require complex manufacturing equipment for, in particular: cleaning and passivating the interior of the bottles to be filled so as to obtain stable concentrations over time of the reactive constituents vis-à-vis the bottle walls; - manufacture the mixtures with a high concentration accuracy of the constituents; - control the composition of the mixtures.

The integration of this equipment in a manufacturing facility requires specialist studies and appropriate buildings (eg temperature controlled). The study period and the cost of appropriate buildings are great. In particular, the cost is too high if the market is too small or sometimes difficult to justify because of a risky economic environment and a little-known market or an unstable environment. The sophistication of factories is changing rapidly. The industrial world is moving more and more from heavy manufacturing to production units of capital goods and consumer goods. This leads, on the one hand, to a change of size of the factories and, on the other hand, to resort to more and more sophisticated production machines, very different, and from many countries. Whether large or small, simple or complex, the approach to building a factory has remained classically the same. It operates very frequently by supply "turnkey". This has the advantage for the manufacturer of compelling the supplier (s) to respect a technical and financial goal determined in advance and thus guarantee the industrial (end user customer) results. Consequently, the "turnkey" realization of a factory is organized as follows: First, production machines are built in various existing factories, for example in already developed countries. These various machines are shipped to the final site by land or sea. These machines are set up in a traditional or prefabricated building previously built on the final site. We assemble and connect the machines (fluids, electricity, pipes, ...) inside the building on the final site. The machines are tested on the final site before starting up.

This conventional method of turnkey realization of distant industrial units, for example in developing countries, presents many hazards. It is enough that the ordered material arrives while the construction of the building on the final site is delayed, and this material risks remaining several months, even several years, in cases. This results in machine corrosion and the need for costly repackaging. Problems also occur frequently if not all machines are delivered within the agreed time. A missing element in the middle of the chain can block the start-up of a factory or a factory slice. According to this traditional scheme, several partners take part in the project at various stages and in very distant places. The manufacturing plant delegates personnel specialized in equipment for supervision of assembly, commissioning and final acceptance. Engineering design and implementation, delegates specialized personnel, engineers for detailed design, assembly plans and tests. This results in many communication problems. This is particularly the case when the manufacturer or a local company takes charge of the construction of the building and the installation of the equipment. By transferring the factories it is possible to reduce production costs and to amortize investments for new industrial plants more efficiently. However, the present situation is limited essentially to providing the possibility of transporting the different machines, respective inner receptacles of the type generally used for moving goods by sea or by road (with trucks). This does not reduce the time and costs below certain limits, because the machines have to be loaded into the containers, removed from the containers and then reassembled the production line. A technical problem underlying the present invention is therefore to provide a plant for the industrial manufacture of special gas mixtures, which can be dismantled, transported and collected simply and quickly. On the other hand, when it comes to carry out tests before a possible industrialization, it is better to realize them on a miniature scale at first. Patent applications EP 0 366 559 and WO 2006/123373 describe containers transportable by sea or by land containing machines intended to be used in the factory; said containers, once combined with each other according to a provision to be defined, form a real factory. However, in the field of special gases, on the one hand this experience has not been attempted, on the other hand, the state of the art does not describe a miniaturized plant that would facilitate the resolution of the technical problems described above . The containers described in application EP 0366559 have one or more completely free lateral faces. Today, with the world economy moving faster and faster, countries that are growing rapidly right now are in need of industrial quantities of filled gas cylinders on the ground. An object of the present invention is to overcome all or part of the disadvantages of the prior art noted above. For this purpose, the subject of the invention is an installation for filling gas cylinders with pure gases and / or mixtures of pure gases comprising: gas selection and / or gas mixture manufacturing equipment intended to be introduced into a gas cylinder; apparatus for analyzing the composition of said mixtures or said pure gases; Characterized in that said installation is integrally contained in a transportable container whose floor area is less than 45 m 2, preferably the floor area is between 34 m 2 and 40 m 2. The invention also relates to an installation for filling gas cylinders with pure gases and / or special gas mixtures comprising two parts, a first part comprising: - equipment for manufacturing special gas mixtures intended to be introduced into a gas cylinder; apparatus for analyzing the composition of said special gas mixtures or said pure gases, the other part comprising: at least one means of emptying the residual gases contained in the bottles to be filled, at least one means for cleaning and / or passivating the bottles to be filled, at least one means for homogenizing the manufactured mixtures, characterized in that said installation is entirely contained in a transportable container whose floor area is less than at 45m2, preferably the floor area is between 34 m2 and 40 m2.

Furthermore, embodiments of the invention may include one or more of the following features: Installation as defined above, characterized in that the two parts are separated from each other by a movable wall .

Installation as defined above, characterized in that said first part further comprises a means for controlling the internal temperature. Said means for controlling the internal temperature allows the manufacture of precise mixtures by a barometric process. Installation as defined above, characterized in that the equipment for manufacturing mixtures comprises at least one mixer associated with at least one analyzer. Installation as defined above, characterized in that the equipment for manufacturing mixtures comprises: - a weighing apparatus and / or a manometric apparatus capable of accurately measuring the quantities of gas to be introduced into said bottle, - a means connection between the bottle to fill and gas sources located, for example, outside the container. Installation as defined above, characterized in that the equipment for manufacturing mixtures comprises at least one ramp capable of manufacturing any type of compressed or liquid gas mixtures. Installation as defined above, characterized in that the weighing apparatus in the container is disposed on a support independent of the container, whose base is located below the floor level of the container. Installation as defined above, characterized in that it comprises at least one mixture composition analysis apparatus chosen from: at least one gas chromatograph for separating the various constituents in a mixture; at least one thermal conductivity detector (TCD) or flame ionization detector (FID); at least one oxygen analyzer; at least one moisture analyzer; at least one infrared spectrometer for determining the concentration of certain compounds in a mixture.

The invention also relates to the use of the installation as defined above for the filling of gas cylinders with pure gases and / or special gas mixtures. The invention also relates to a process for preparing a mixture of special bottled gases using an installation as defined above connected to at least two sources of special gases external to the installation. A process as defined above, characterized in that the bottle to be filled is connected to a single source of gas at a time.

A method as defined above comprising the steps of: a) preparing the bottle to be filled; b) filling said bottle, by connection to a gas source, using a weighing apparatus and / or a manometric apparatus capable of accurately measuring the quantities of gas to be introduced into said bottle; c) analysis of the composition of the contents of the bottle thus filled. The invention relates to a facility for manufacturing special gas mixtures comprising the best manufacturing techniques and miniaturized to be placed, for example, in an ISO-container transportable for example by land and sea. In this way it is possible to standardize the manufacturing of the complete plant in a factory to optimize manufacturing costs, remove it if necessary and transport it to a more suitable location to recover the investment. Unlike the documents of the state of the art cited above, the equipment contained in said container is fixed on the walls of the container. Indeed, the components such as for example the manufacturing equipment or the analysis apparatus are fixed on the walls of the container containing the installation according to the invention. Therefore, said walls are not completely free. The advantage of these fasteners is that such an arrangement allows the users to access this equipment from inside the container and makes it possible to connect these equipments with each other on the one hand, and on the other hand, with sources of gases located outside the container, using pipes fixed on the walls of the container. This provides, among other things, a saving of space and thus a better miniaturization of the installation, as well as a better stability for the measurements due to the fixing of the apparatus.

The installation can be placed inside an ISO-container of 12 meters length, 3 meters width and height or two ISO-containers of 6 meters length placed end to end. Reasons why this type of installation did not exist for the filling of gas cylinders are: - for the filling of pure gases: the quantity of gas to be filled is such that sufficient raw materials are required which require example of the sources of liquefied gases (liquid nitrogen, liquid argon, liquid oxygen, carbon dioxide, etc.) requiring an investment such as a large building housing the filling plant has always been considered. - for the filling of special gas mixtures the factories were most frequently built using the raw material resources of a pure gas cylinder filling plant. On the other hand, this type of installation did not exist before because the packaging machines were larger and could not have gone into an ISO-container. For example, analytical devices were larger as well as weighing devices. Other features and advantages will appear on reading the description below, with reference to the figures in which: - Figure 1 shows a diagram of an example of organization of an installation according to the invention; FIG. 2 represents a diagram of equipment for manufacturing special gas mixtures included in an installation according to the invention. In Figure 1, there is shown a plant 1 according to the invention for manufacturing special gas mixtures comprising two parts 2 and 3. The two parts are separated by a movable wall 20. For example, the movable wall 20 is a sliding door. The two parts can also be two iso containers connected to each other. The first part 2 has an indoor temperature controlled by a temperature control means. For example, such a means is a heater or an air conditioning system. Said part 2 houses the equipment 4 for manufacturing the mixtures and the apparatus for analyzing the composition of the mixtures here located in zone 5.

An example of equipment 4 for manufacturing said mixtures is shown in FIG. 2. The precise measurement, for example by manometry, of the quantities of gas to be mixed is preferably carried out using equipment and bottles to be filled in a container. space at controlled temperature. This being an essential characteristic to obtain an accuracy of appreciable reliability on an industrial scale. Temperature control is necessary for the manufacture of precise mixtures by a barometric process. Part 3 comprises at least one emptying means 6 of the residual gases contained in the bottles to be filled, at least one means for cleaning and / or passivation 8 of the bottles to be filled, at least one means 9 for homogenizing the manufactured mixtures. The installation 1 is entirely contained in a transportable container 10 whose floor area is less than 45 m 2, preferably the floor area is between 34 m 2 and 40 m 2. The height of the container 10 is for example between 2.5 meters and 3.5 meters, preferably the height is 3 meters. In practice, the personnel enters the container through a door 11 and proceeds to fill the bottles 7 located in the first part, in part 3 intended for the preparation (cleaning, passivation, emptying) of the bottles 7. Said filling of the mixtures is performed in Part 2, whose temperature is controlled, using the equipment 4 for manufacturing the mixtures. The bottle 7 intended to be filled with a mixture of special gases is, in a first step, prepared, if necessary, for example by cleaning with the cleaning and / or passivation means 8, and / or by emptying residual gas from the bottle if it has already been used with the aid of a draining means 6. If this is the case, said bottle will indeed probably be polluted by residual gases. The passivation means 8 is for example an oven into which the bottle 7 is introduced for a few hours. Once the bottle 7 ready, the user takes it then rolled or the door into the part 2 of the installation whose temperature is controlled. The user can then proceed to fill the special gas mixture in the bottle 7 thus prepared. When several bottles are ready, the user can carry several at a time to optimize his working time and productivity and store said bottles in a dedicated location 11. The equipment 4 manufacturing the mixture is shown schematically in Figure 2 The bottles to be filled are each connected to the same filling ramp 12 by connecting means 14. This filling ramp 12 is connected to a control panel 13, for example a PLC. This filling ramp 12 is connected to automatic valves 22 which are connected to measuring instruments, for example to the measurement of weight developed by the weighing system 17 so that when the weight of gas to be introduced into the bottle is reached, the valve closes automatically. The filling ramp 12 is also connected to a network 15 of special gas sources disposed outside the container 10 in which the installation according to the invention is arranged, as represented in FIG. 1.

An essential feature of the invention, especially in terms of safety, is the fact that when a bottle is being filled, it is connected to only one source of gas at a time. Indeed, it is preferable, in order to avoid an explosion, not to connect at the same time, a source of flammable gas and a source of oxidizing gas, to said bottle being filled. The fact that the filling ramp 12 is able to fill the bottles with any family of mixtures may require cleaning of said ramp 12, including cleaning the connection volume. Such a ramp 12 may be unique according to one embodiment of the invention. The same ramp 12 is able to fill the bottles with mixtures such as for example flammable gas / inert gas mixtures, oxidizing gases / inert gases, oxidant / fuel. A safety system (not shown) to prevent the manufacture of incompatible gas mixtures in the equipment can also be added in the container 10. The quantities of special gases composing the mixture are measured and controlled using measuring means. and control such as a manometer 16 and a weighing system 17. Depending on the degree of precision desired for the manufacture of the desired mixture, the equipment 4 comprises either a manometer 16 and a weighing system 17, or only one of the two . Said mixing equipment 4 is located in the part 2 of the container 10 whose temperature is controlled, and the stable temperature allows a reliable measurement of the pressure. In order to avoid a disturbance of the measurements due for example to the vibrations on the floor of the container 10, the weighing system 17 is placed on a support 18 independent of the said container 10. The base of the support 18 is situated below the ground level of the container 10. For example, this base of the support 18 of the system 17 is based on a frame welded to the container 10 independently of the frame of the floor of the container 10, so as to minimize vibration during eg moving people or bottles. Once the mixture is made, it is analyzed using the analysis apparatus located in the zone 5 of the container 10. The analysis devices are for example: gas chromatographs intended to separate the various constituents in a mixture. The concentration of the constituents in the mixtures is measured by means of detectors varying according to the type of constituent and its concentration. The most commonly used detectors are thermal conductivity (TCD) or flame ionization (FID) detectors for hydrocarbon compounds; - oxygen analyzers; - moisture analyzers; infrared spectrometers for determining the concentration of certain compounds in a mixture. It should be noted that the arrangement of the components of the installation according to the invention is such that the user makes a minimum of displacements. The bottles are not moved much. On the other hand, the space between the manufacturing equipment 4 and the analysis equipment is sufficient for the user to move but low enough so that the installation is miniaturized to the maximum and thus limit the movements of bottles .

Moreover, such an installation requires the presence of only a few people to operate it. Compared to existing real size factories today, the number of people working on the plant 1 according to the invention is very small and the distance due to the transport of the bottles during the process of filling the mixtures is reduced to a minimum. When the analyzes are completed, the bottles filled with special gas mixtures are transported in the part 3 of the container 10 to a means 9 called homogenization. Said means 9 is for example a roll of bottles. It is possible that a gas mixture at the end of filling of a bottle does not have a homogeneous composition in the bottle when for example it is filled vertically and that the component introduced last has a lower density than the precedents. One way to homogenize the mixture is to put the bottle in a horizontal position and to turn it on its axis at a speed of several revolutions per minute for about ten minutes minimum. The means 6, 8 and 9 are automated.

When this operation is completed, the user leaves the container 10 the bottle filled with the desired gas mixture and has it in a storage location 19 from which a batch of bottles will be transported to the customer. The storage place 19 is for example located outside the container 10. An embodiment of the installation 1 according to the invention may be limited to the manufacture of a few bottles of mixtures per day, for example 8 bottles per day of eight hours. or the equivalent of 2000 bottles per year, considering mixtures containing on average 3 compounds. This type of installation is therefore capable of providing a market corresponding to the need of several refineries and / or petrochemical industries and / or automotive industries. The raw materials of manufacture of these mixtures, which may be flammable and / or toxic gases, are disposed in sources connected to the equipment 4, 13, 12 of the plant 1 from the outside. This saves space in the ISO-container 10 and more easily manage the risk of ignition and explosion in case of flammable gas leak in the bottles. This facility 1 is able to manufacture special gas mixtures requested by the main users: refineries, petrochemical plants, automotive industry and research laboratories for example.

Said plant according to the invention can also be used advantageously as an installation for testing limited quantities of bottles and if these tests are conclusive, it may be decided to implant a larger plant to increase production.

By way of example, here are non-exhaustive lists of special gas mixtures that can be manufactured by the installation according to the invention.

Examples of mixtures for analysis apparatus: 5% or 10% CH4 in Argon 2% or 5% H2 in Argon 40% H2 in Helium 10% 002 in Argon 5% 002 in Oxygen 5% of 002/5% or 10% of H2 in Nitrogen 10% of 002/10% of H2 in Nitrogen 40% or 45% of H2 in Nitrogen Examples of mixtures for the measurement of pollution in the atmosphere: Composition Concentration NH3 in N2 15 ppm HCl in N2 10 to 45 ppm CO in N2 45 to 9000 ppm H2S in N2 5 at 1000 ppm NO in N2 8 at 1800 ppm C3H8 in Air 3 at 3000 ppm CO in Air 9 to 15 ppm NO2 in Air 9 at 450 ppm SO2 in Air 28 to 500 ppm NO / NOX in N2 40 to 1000 ppm Examples of hydrocarbon mixtures used in refineries and petrochemical plants: Hydrocarbon mixtures gaseous (2 to 10 components) Liquid hydrocarbon mixtures (2 to 10 components) 5

Claims (13)

REVENDICATIONS1. Installation (1) for filling gas cylinders (7) with pure gases and / or pure gas mixtures comprising: - a gas selection and / or manufacturing equipment (4) for gas mixtures intended to be introduced into a bottle (7) of gas, - apparatus for analyzing the composition of said mixtures or said pure gases; Characterized in that said installation is integrally contained in a transportable container (10) whose floor area is less than 45 m 2, preferably the floor area is between 34 m 2 and 40 m 2. 2. Installation (1) according to claim 1, for filling cylinders (7) of gas with pure gases and / or special gas mixtures comprising two parts, a first part (2) comprising: - equipment (4) ) for the manufacture of special gas mixtures for introduction into a gas cylinder (7), apparatus for analyzing the composition of said special gas mixtures or pure gases, the other part (3) comprising: at least one means for emptying (6) the residual gases contained in the bottles (7) to be filled, at least one means for cleaning and / or passivating (8) the bottles (7) to be filled, at least means for homogenizing (9) the manufactured mixtures, characterized in that said installation (1) is entirely contained in a transportable container (10) whose floor area is less than 45m2, preferably the floor area is included between 34 m2 and 40 m2. 3. Installation (1) according to claim 2 characterized in that the two parts (2, 3) are separated from one another by a movable wall (20). 4. Installation according to any one of claims 2 or 3, characterized in that said first portion (2) further comprises a means for controlling the internal temperature. 5. Installation according to any one of claims 1 to 4, characterized in that the equipment for manufacturing mixtures comprises at least one mixer associated with at least one analyzer. 6. Installation according to any one of claims 1 to 5, characterized in that the equipment for manufacturing mixtures comprises: - a weighing apparatus (17) and / or a manometric apparatus (16) capable of accurately measuring the quantities gas to be introduced into said bottle, - a connection means between the bottle to be filled and gas sources located, for example, outside the container. 7. Installation according to claim 6, characterized in that the equipment for manufacturing mixtures comprises at least one ramp (12) suitable for manufacturing any type of compressed or liquid gas mixtures. 8. Installation according to any one of claims 6 or 7, characterized in that the weighing apparatus (17) located in the container (10) is disposed on a support independent of the container, the base is located below the ground level of the container. 9. Installation according to any one of claims 1 to 8, characterized in that it comprises at least one mixture composition analysis apparatus selected from: - at least one gas chromatograph intended to separate the various constituents in a mix ; at least one thermal conductivity detector (TCD) or flame ionization detector (FID); at least one oxygen analyzer; at least one moisture analyzer at least one infrared spectrometer for determining the concentration of certain compounds in a mixture. 10. Use of the plant as defined in one of claims 1 to 9 for filling gas cylinders with pure gases and / or special gas mixtures. 11. A method for preparing a mixture of bottled special gases implementing an installation as defined in one of claims 2 to 9 connected to at least two special sources of gas external to the installation. 12. The method of claim 11, characterized in that the bottle to be filled is connected to a single source of gas at a time. 13. Method according to any one of claims 11 or 12 comprising the steps: d) preparation of the bottle to be filled; e) filling of said bottle, by connection to a gas source, using a weighing apparatus and / or a manometric apparatus capable of accurately measuring the quantities of gas to be introduced into said bottle; f) analysis of the composition of the content of the bottle thus filled.