Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation 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
  • B01D53/22—Separation 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 by diffusion
  • B01D53/225—Multiple stage diffusion
  • B01D53/226—Multiple stage diffusion in serial connexion
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation 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
  • B01D53/22—Separation 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 by diffusion
  • B01D53/225—Multiple stage diffusion
  • B01D53/227—Multiple stage diffusion in parallel connexion
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B23/00—Noble gases; Compounds thereof
  • C01B23/001—Purification or separation processes of noble gases
  • C01B23/0036—Physical processing only
  • C01B23/0042—Physical processing only by making use of membranes
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
  • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
  • C01B3/501—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
  • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
  • C01B3/501—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
  • C01B3/503—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion characterised by the membrane
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2317/00—Membrane module arrangements within a plant or an apparatus
  • B01D2317/02—Elements in series
  • B01D2317/022—Reject series
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2317/00—Membrane module arrangements within a plant or an apparatus
  • B01D2317/02—Elements in series
  • B01D2317/025—Permeate series
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
  • C01B2203/0405—Purification by membrane separation
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
  • C01B2203/0465—Composition of the impurity
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
  • C01B2203/0465—Composition of the impurity
  • C01B2203/047—Composition of the impurity the impurity being carbon monoxide
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
  • C01B2203/0465—Composition of the impurity
  • C01B2203/048—Composition of the impurity the impurity being an organic compound
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2210/00—Purification or separation of specific gases
  • C01B2210/0029—Obtaining noble gases
  • C01B2210/0031—Helium
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2210/00—Purification or separation of specific gases
  • C01B2210/0043—Impurity removed
  • C01B2210/005—Carbon monoxide
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2210/00—Purification or separation of specific gases
  • C01B2210/0043—Impurity removed
  • C01B2210/0051—Carbon dioxide
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2210/00—Purification or separation of specific gases
  • C01B2210/0043—Impurity removed
  • C01B2210/0068—Organic compounds
  • C01B2210/007—Hydrocarbons
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2210/00—Purification or separation of specific gases
  • C01B2210/0043—Impurity removed
  • C01B2210/0078—Noble gases
  • C01B2210/0084—Krypton
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2210/00—Purification or separation of specific gases
  • C01B2210/0043—Impurity removed
  • C01B2210/0078—Noble gases
  • C01B2210/0085—Xenon

Definitions

• the present invention relates to an installation and a system for treating a gas mixture by permeation.
• Membrane gas separation is a technique widely used by the chemical industry, which has been particularly developed over the last 25 years. Depending on the nature and structure of the membrane used (polymer, ceramic, dense or porous), different mechanisms of transport and separation are involved.
• Molecular sieving is a technique that consists of separating gases present in mixture, using a difference in kinetic radius of the molecules to be separated.
• a microporous membrane is used which, under the effect of a difference in concentration or of partial pressure on either side of the membrane, allows the molecules with the smallest kinetic radius to diffuse preferentially and retains more the molecules of higher size.
• the membrane is used as molecular sieve, implementing a steric exclusion process ("pore size exclusion"), which inhibits or delays the diffusion of large molecules, thus promoting the diffusion of size the weakest.
• pore size exclusion a steric exclusion process
• adsorption phenomena on the surface of the membrane and / or in its pores
• Selective permeation gas mixture separation plants comprise separation modules each comprising a permselective membrane separating a non-permeate zone or a retentate zone and a permeate zone.
• a separation module generally includes several membranes. It will be noted that the geometry of the membranes can also vary. There are essentially two types of membranes: flat membranes and tubular membranes. The tubular membranes may be single-channel or multichannel (made for example in the form of a monolith).
• the separation module has a feed inlet, a retentate outlet and a permeate outlet.
• the separation module In order to separate a gaseous mixture, the separation module is charged with a stream of the mixture at a pressure P1 by means of a feed. There is then a pressure difference between the two sides of the membrane.
• the permeate is enriched by constituting the most permeable while the - constituent is essentially on the non-permeate side.
• a retentate is recovered at a pressure P1 and at the outlet of permeate a permeate at a pressure P2 less than P1.
• transmembrane gas separation technique is very advantageous, especially insofar as it is modular and can be used in a continuous mode.
• it is a non-polluting technology and allows the construction of compact units.
• it constitutes a very interesting alternative to other separation processes, such as cryogenic or adsorption processes, with respect to which it proves to be simpler to implement and less expensive.
• this technique has, in practice, many fields of application.
• it is used for the separation of O 2 and N 2 from air, for the extraction of H 2 and N 2 in NH 3 production gases, or of H 2 in effluents with hydrocarbon base such as those resulting from refining processes, or else to remove CO 2 or NOx in various gaseous effluents.
• FIG. 1 shows an installation for treating a gas mixture by permeation 1 comprising:
• the retentate output of each module is connected to the permeate input of the next module.
• the common collector pipe 6 groups all the flows of permeate passing to the user. The more permeable compounds are recovered mainly in the permeate and the less permeable ones are recovered in the retentate.
• the enrichment portion 12 comprises three separation modules 15 to 17 and three compressors 18 to 20.
• the extraction portion 13 comprises three separation modules 21 to 23.
• the permeate at the outlet of each separation module is compressed and used to feed the next separation module. This compression is an essential step in order to be able to inject the permeate into the inlet of the next separation module since the permeate at the permeate outlet is at a pressure lower than its inlet pressure.
• the retentate output of each separation module directly feeds the next separation module.
• the number of stages (here three) in the enrichment part as in the extraction part depends on the desired purity. However, the implementation of the installation 1 1 according to the article
• the disadvantage of this configuration is a relatively low production of pure product. Indeed, there is a large production of side products that are not used (L 1 to L 3 for the enrichment part and L'-i to U 3 for the extraction part). Thus the final product obtained, P for the enrichment part 12 and R for the extraction part 13, represents only a small fraction of the feed F.
• the installation 100 comprises: an input separation module 102 with a main supply input F,
• the retentate output of the separation module 102 is connected to the supply input of the separation module 103.
• the permeate output of the separation module 102 is connected to the supply inlet of the separation module 101 via the compressor 104.
• the retentate output of the separation module 103 is connected to the main supply input F via the compressor 105.
• the feed F is divided into only two final products, the permeate P (corresponding to the permeate output of the separation module 103) and the retentate R (corresponding to the retentate output of the separation module 101).
• This installation makes it possible to increase the production of pure product compared to a cascade configuration without recycling.
• the present invention aims at providing an installation for treating a gas mixture by permeation making it possible to obtain products of high purity while avoiding losses related to side products, said installation also having a relatively low cost. not very high and offering the possibility of treating gas flows with low concentrations of impurities.
• the invention proposes an installation for treating a gaseous mixture by permeation comprising m * n separation modules P, j5 m and n being natural numbers greater than or equal to 2, i being a variant integer from 1 to m and j being a natural integer varying from 1 to n, each of the separation modules P 1J comprising:
• the permeate outlet Sp 1J is connected to the permeate inlet Ep l + 1J of the separation module P I + 1J ; the retentate outlet Sr 1J is connected to the permeate inlet Ep IJ + 1 of the module of P u + 1 separation, said installation not having intermediate recycling.
• the gaseous mixture treatment plant can be represented as a matrix having m lines of separation modules (corresponding to m enrichment stages constituting the most permeable, passing successively from a permeate outlet to the next permeate inlet) and n columns of separation modules (corresponding to m enrichment stages constituting less permeable passing successively from a retentate outlet to the next permeate inlet).
• each separation module can be either a unitary module (ie with a single permeate inlet, a single retentate outlet and a single permeate outlet) as described above or a combination of modules. units mounted in parallel (ie a power supply which separates to feed each of the inputs of the unit modules and the outputs of unit modules connected to each other).
• the flow of permeate leaving a separation module is reused as part of the supply of the separation module of the next step.
• This allows to continue to separate the compounds in successive steps without using compressors.
• the installation according to the invention does not require intermediate recycling with compressors between each permeation step: this absence of compressors of course leads to a significant economic advantage.
• it is desired to purify a gas i.e. separate the gas from less permeable impurities and present in said gas
• it is desirable that the membrane has a good permselectivity with respect to the gas to be purified in order to concentrate the impurities.
• the number of steps is a function of the desired concentration of impurities: thus, the greater the number of steps, the lower the concentration of impurities in the permeate.
• the number of steps and stages is a function of the desired purity (for both retentate and permeate) and the amount of product to be recovered.
• the number m of steps may be different from the number n of stages.
• the subject of the present invention is also a system for treating a gaseous mixture by permeation comprising at least one installation according to the invention, the system being represented by a matrix structure Mij with p rows and q columns comprising p * q elements Mij, i being a natural integer varying from 1 to p and j being a natural integer varying from 1 to q, Mij being either a separation module Pij or an empty element, each of said separation modules P 1J comprising:
• the element M 11 is a non-empty element corresponding to the separation module P 11 belonging to said at least one device, the permeate inlet Ep 11 of the separation module P 11 corresponding to the feed inlet gas mixture in the system.
• the system according to the invention may also have one or more of the following characteristics, considered individually or in any technically possible combination:
• the different permeate flows obtained at the outlet of the system are grouped together on the same permeate output line and / or the different retentate streams obtained at the output of the system are grouped together on the same retentate output line.
• the system includes a compressor at the feed inlet of the gas mixture in the system.
• the separation modules comprise tubular or multichannel membranes.
• the tubular membranes comprise a microporous layer based on silica doped with boron.
• each separation module is adapted so as to obtain similar concentrations between the retentate flow and the permeate flow which feed the same following separation module.
• the subject of the present invention is also a use of a system according to the invention for the separation of helium or hydrogen in gaseous mixtures comprising them and a nuclear installation comprising a helium heat transport circuit equipped with a system of treatment according to the invention.
• FIG. 1 is a simplified schematic representation of a first installation for treating a gaseous mixture by permeation according to the prior art
• FIG. 2 is a simplified schematic representation of a second installation for treating a gas mixture by permeation according to the prior art
• FIG. 3 is a simplified schematic representation of a third installation for treating a gas mixture by permeation according to the prior art
• FIG. 4 is a simplified schematic representation of an installation for treating a gas mixture according to the invention.
• FIG. 5 is a simplified schematic representation of a system for treating a gas mixture according to the invention.
• FIG. 6 is a simplified schematic representation of a separation module comprising several unit modules mounted in parallel.
• FIG. 4 is a simplified schematic representation of an installation I for treating a gas mixture according to the invention.
• the installation I comprises:
• the separation module P 12 comprises a permeate inlet Ep 12 , a permeate outlet Sp 12 and a retentate outlet Sr 12 .
• the feed inlet F of the gaseous mixture corresponds to the permeate inlet Ep 11 of the separation module P 11 .
• the permeate outlet Sp 1J is connected to the permeate inlet Ep l + 1J of the separation module P I + 1J : this connection corresponds to the transition from a step i (line i of the separation module matrix) to a step i + 1 (line i + 1 of the separation module matrix).
• the retentate outlet Sr 4 is connected to the permeate inlet Ep u + 1 of the separation module P ij + 1: This connection corresponds to the transition from one floor j (column j of the matrix separation modules) in a stage j + 1 (column j + 1 of the separation module matrix).
• the separa- tion module is charged with 11 P a stream of the mixture at a pressure P1 by the feed F. It then occurs a pressure difference between both sides of the membrane.
• the permeate is enriched by constituting the most permeable while the Another constituent remains essentially on the non-permeate side.
• a retentate is recovered at a pressure P1 and at the outlet of permeate a permeate at a pressure P2 less than P1.
• the plant I according to the invention comprises 3 lines of separation modules (corresponding to 3 enrichment stages by constituting the most permeable passing successively from a permeate outlet to the next permeate inlet) and 3 columns. separation modules (corresponding to 3 enrichment stages by constituting less permeable passing successively from a retentate outlet to the next permeate inlet). According to a particular embodiment, the different permeate flows
• FIG. 5 represents a system S for treating a gas mixture according to the invention.
• the system S comprises an installation I similar to that described with reference to FIG. 4 (the only difference lies in the fact that the installation I of FIG. 5 comprises 2 lines of separation modules and not 3 as it is the case. on the installation of Figure 4).
• System S is in the form of a matrix structure
• M 1J at 4 lines (L1 to L4) and 6 columns (C1 to C6) having 24 elements M 1J , i being a natural integer varying from 1 to 4 and j being a natural integer varying from 1 to 6.
• An element M 1J is either a separation module P 1 (such as those described with reference to FIG. 4) or an empty element.
• M 32 is a separation module P 32 while M 31 is an empty element.
• each of the elements M u is a separation module (no empty element).
• the system S has 15 separation modules (instead of the 24 possible ones):
• the permeate outlet of the separation module P n is connected to the permeate inlet of the separation module P I + 1J when the latter exists.
• the retentate output of the separation module P 1 is connected to the permeate inlet of the separation module P u + 1 when the latter exists.
• the permeate outlet Sp 22 of the separation module P 22 is connected to the permeate inlet Ep 32 of the separation module P 32 .
• the retentate output Sr 22 of the separation module P 22 is connected to the permeate inlet of the separation module P 23 .
• the permeate outlet Sp 3 2 of the separation module P32 is not connected to any separation module (M 42 is an empty element).
• the retentate outlet 24 P 24 Sr separation module is connected to any separation module (M 25 is an empty element).
• the various permeate streams (here Sp 2 -I, Sp 32 , Sp 43 , Sp 44 , Sp 45 , and Sp 46 ) obtained at the output of the system S are grouped on the same permeate output line Lp; the same is true of the different retentate streams (here Sr 13 , Sr 24 , Sr 35 and Sr 46 ) obtained at the output of the system S which are grouped together on the same retentive output line Lr.
• the operating conditions pressure, temperature, flow and composition of the feed
• the membrane surface of each separation module can be chosen so as to obtain similar concentrations between the retentate flow and the flow. permeate feeds the same separation module (see for example concentrations of streams F1 and F2 as shown in Figures 4 and 5).
• the installation I and the system S according to the invention find, in particular, a very advantageous application in the treatment of heat-transfer helium currents used in particular in the primary circuit of the new-generation high-temperature nuclear reactors, called HTR ( "High Temperature Reactor".
• HTR High Temperature Reactor
• impurities such as CO, CO 2 or CH 4 , as well as fission products of the Xe or Kr type, which are present in the helium must be removed, insofar as they are a source of corrosion.
• the installation and the system according to the invention have applications in many fields of use, given their multiple advantages.
• the plant and the system according to the invention can be used to extract hydrogen H 2 from gaseous mixtures containing it, such as effluents from petrochemical refineries, or to eliminate gaseous pollutants present in a feed stream.
• hydrogen for example prior to its introduction into a synthesis reactor, or even into fuel cells (in particular PEM-type "Proton Ex- Change Membrane "in English) where they allow, among other things, to eliminate CO type gases that can poison catalysts.
• separation modules comprising one or more tubular membranes such as those described in the article "Development of new microporous silica membranes for gas separation" (Barboiu et al World Hydrogen Energy Conference - June 13-16, 2006 - Lyon). These membranes comprise a microporous layer based on silica doped with boron.
• the supply pressure P1 is of the order of 70 bar: this pressure is therefore high enough to allow the operation of the installation I without compressor input; the total output permeate flow will then be reintroduced into the reactor (a compressor being necessary to allow recirculation of the permeate to the reactor).
• cascade systems with recycling are normally developed for rather high gaseous concentrations of impurities (> 5%).
• the cascade systems are not suitable for treating very dilute impurities.
• the impurities are very dilute, of the order of vpm (volume per million).
• the amount of helium to be recovered must be as high as possible (> 99%).
• the plant and the system according to the invention are particularly suitable for this type of application insofar as the number of stages and stages can be adapted so as to recover a large amount of helium passing through the membrane surface towards permeate and allow efficient filtration despite very dilute impurities.
• the separation modules can be eliminated because there is a gradual decrease in the flow as the number of stages and / or steps is increased.
• the separation modules can be eliminated because it is not desired to increase the concentration of the compounds too much (in the case of HTR application, ie impurities) in the retentate or an excessive increase of the compounds in the mixture. (In the case of the HTR application, the concentration of helium is too high compared to the recirculation requirements to the reactor and the concentration of impurities in the recirculating helium is too low).
• each of the unitary modules P, j as shown in FIGS. 4 and 5 may also be a separation module comprising a plurality of unit modules connected in parallel; such an example of separation module P is shown in FIG. 6.
• This separation module comprises three unitary separation modules M 1 to M 3 .
• the retentate outputs of the modules M 1 to M 3 are interconnected so as to form an overall retentate output.
• the permeate outlets of the modules M 1 to M 3 are connected together so as to form a global permeate outlet.
• the number of stages and stages of the installation shown in FIG. 4 are identical but they can of course be different.
• we have described for illustrative a tubular type membrane but the invention applies to any type of membrane (flat membranes or tubular membranes, single channel or multichannel) and any type of separation module. It is the same for the material used for the membrane which can be polymer, mineral and / or composite.

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