• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a flexible process for the purification of a solvent inhibiting the formation of hydrates during the treatment of gases, in particular monoethylene glycol (MEG), said solvent having a boiling point higher than that of the water and being, at least at a time, mixed with water and salts, the process operating differently with the same plant according to the salt content of the MEG to be treated. The process operates according to a so-called reclaiming phase (separation of the salts under vacuum followed by distillation under vacuum) when the salt content exceeds the precipitation threshold and otherwise the process operates in the regeneration phase (absence of salt separation and no operation under vacuum). Advantageously, the tilting takes place under control of a salt dosing means.
    公开号:FR3013710A1
    申请号:FR1361500
    申请日:2013-11-22
    公开日:2015-05-29
    发明作者:Jeremie Esquier；Bernard Chambon；Christian Streicher
    申请人:Prosernat；
    IPC主号:
    专利说明:

    [0001] FLEXIBLE PROCESS FOR TREATING SOLVENT, SUCH AS MONOETHYLENE GLYCOL, USED IN THE EXTRACTION OF NATURAL GAS The invention relates to a process for the purification of a solvent, in particular monoethylene glycol, which is used on natural gas fields to avoid the formation of hydrates. Said solvent has a boiling point higher than that of water, and is, at least at least one time, mixed with water and salts.
    [0002] These hydrates are formed in the presence of water, natural gas and under the conditions favoring their stability. Their presence can become extremely harmful for the operation since plugs can form in the extraction tubes or in the transport pipes, which can lead to a stop of the production. The problem arises with particular acuity for offshore platforms where the gas is extracted in a relatively cold environment favorable to the formation of hydrates and where, moreover, the gas treatments are carried over to earth, and therefore the gas such as that extract is sent to the facility on land and at temperatures where the hydrates are stable.
    [0003] To avoid these disadvantages, it is known to use inhibitors of hydrate formation such as monoethylene glycol (MEG). This solution remains expensive, given the necessary amounts of inhibitor. So we had to find a way to recycle the inhibitor.
    [0004] It is known, for example by the patents of CCR Technologies, a process for purifying the MEG and recycling it. Thus EP-1261410 discloses an installation and a method for purifying hydrate formation inhibitor such as MEG. The MEG to be treated is sent into a flash flask or a column operating under vacuum so as to separate a liquid stream at the bottom of the flask (or column) comprising MEG and the salts, and at the top of the flask (or column) a stream essentially gaseous including water and MEG. The flow of MEG and salts is partly heated to be recycled to the flask (or column), the other part is purged, the purged amount depending on the salt concentration. The overhead stream is vacuum distilled to separate the water and gases (at the top) and recover the purified MEG (bottom) that is recycled to the natural gas field. This process works in so-called reclaiming mode. Another so-called regeneration mode is known for purifying the MEG. In this mode, the MEG to be treated is distilled at atmospheric pressure in order to separate the water at the top of the column, the flow of MEG and the salts leaving at the bottom of the column are treated so as to separate the salts, for example by means of a balloon or vacuum column.
    [0005] The applicant has found that the reclaiming phase is energy intensive because it is necessary to circulate and heat large quantities of solvent (eg MEG). Moreover, the field work shows that the solvent (eg MEG) may at certain times not contain formation water (water loaded salts of the formation traversed) just as at other times it may contain large quantities, it depends on the formations crossed. This phenomenon is random and until now difficult to predict. An object of the invention is to reduce the energy costs of the process while maintaining a good level of purification.
    [0006] More specifically, the invention relates to a method for purifying a solvent that inhibits hydrate formation, said solvent having a boiling point greater than that of water and being, at least at least one time, in a mixture with water and salts, which process comprises: - optionally, a pretreatment of said solvent to be treated, said pretreatment separating at least part of the hydrocarbons, the condensates and the gases, and said pretreatment optionally comprising chemical agent addition of neutralization, - a reclaiming phase implemented when the salt content of said solvent to be treated, optionally pretreated, reaches the precipitation threshold in the treated mixture - said phase comprising a flash under vacuum, operating at a pressure below the pressure atmospheric and preferentially between 0.2 and 0.5 bar absolute and at a temperature below the degradation temperature of the solvent, by the whereby a solvent stream containing the salts and a vaporized stream of solvent and water is obtained, said stream of solvent and water is distilled under vacuum at a pressure substantially equal to that prevailing in said vacuum flash for separating the water and recovering a stream of purified solvent, the salts are separated from said stream of solvent containing the salts, and the solvent obtained is flash recycled, when said salt content in the treated mixture is below the precipitation threshold, the reclaiming phase is stopped and a so-called regeneration phase is implemented, - said regeneration phase comprising the vacuum suppression, the solvent to be treated, optionally pretreated, undergoing a flash step, operating under a pressure equal to or greater than atmospheric pressure and preferably between 1 and 2 bar absolute and at a temperature below the degradation temperature of the solvent, by which it is obtained a first stream of purified solvent and a stream of solvent and water, said stream of solvent and water is distilled under a pressure substantially equal to that prevailing in said flash, the water is separated and a second stream of solvent purified is obtained, said second stream being mixed with said first stream, and / or recycled to said flash. The process is particularly applicable to monoethylene glycol. The solvent to be treated (in particular MEG) is an inhibitor of hydrate formation during gas treatment. The solvent to be treated (in particular MEG) is not treated to separate the divalent salts. The divalent salts remain in the solvent entering the flash. The level of purification of the solvent (in particular MEG) desired and obtained is greater than 60% by weight and preferably greater than 80% by weight. The water resulting from the process generally contains less than 1% by weight of solvent (MEG in particular) and preferably less than 0.1% by weight; it can be reused. The invention also relates to a plant for purifying a hydrate-inhibiting solvent, said solvent having a boiling point higher than that of water and being, at least at least one time, in admixture with water and salts, said installation comprising: - a flash balloon 7 provided with a pipe 6 for introducing the solvent to be treated, a pipe 8 for the outlet of a mixture of solvent and water, a line 9 for discharging a mixture of solvent and salts, - a means 10 for separating the salts provided with a pipe 9bis for introducing the mixture of solvent and salts, said pipe 9a comprising a valve 16, the means 10 also being provided with an outlet pipe 11 for separating the separated salts and a pipe 12 for dispensing the solvent separated from the salts, said pipe 12 being connected to the flash tank 7 and provided with a valve 26; a distillation column 13 which can operate under vacuum, provided with a pipe 6 for introducing 8 said mixture of solvent and water, an outlet pipe 15 of the purified solvent located at the bottom of the column, an outlet pipe 14 of water and gas, located at the top of a column, - a pipe 17 provided with a valve 18 connecting said pipe 9 to the outlet pipe 15 for the purified solvent - a vacuum system 20 capable of delivering a reduced pressure in the distillation column and the flash balloon a bypass pipe 19 of said system and valves 24 and 25 respectively at said system and the bypass line, a pipe 29 provided with a valve 28, connecting the pipe 15 to the flash balloon 7, and said plant operating in two phases according to the content of salts of the solvent delivered by the metering means: in one of the phases, the valves 18, 25 and 28 are closed, the valves 26, 16 and 24 are open , and said vacuum system provides a reduced pressure -in the other phase, the valves 16,26 and 24 are closed, the valves 18, 25 and 28 are open and said vacuum system is stopped. Preferably, the installation comprises upstream of the flash balloon pretreatment comprising a means 4 for separating the hydrocarbons, condensates and gases and the pipe 6 for recovering the pretreated solvent. Preferably, the installation further comprises a pipe 5 connected to the pipe 6 for the introduction of a chemical agent. Advantageously, the installation comprises a pipe 14 for introducing water and gas into a means 22 for separating the gases from said water, said means comprising a water outlet pipe 23 and an outlet pipe 21. gas, said pipe 21 being connected to the vacuum system 20 (compressor for example). The installation is particularly applicable when the solvent is monoethylene glycol.
    [0007] The invention will be described from the diagram in FIG. the solvent is MEG but the figure may be described with any other solvent as defined in the invention; "MEG" can be replaced by "solvent". Upstream of the actual process, it is advantageous to perform a pretreatment.
    [0008] The MEG to be treated (brought by the pipe 1) is generally separated from the gases (exiting through the pipe 2) and condensates and hydrocarbons (exiting through the pipe 3) into a balloon 4. There may remain traces or small amounts of gas. hydrocarbons, condensates or gases depending on the level of separation. The MEG obtained contains water and salts. It is optionally neutralized, for example by sodium hydroxide (supplied via line 5). Preferably, the MEG is separated from the gases, condensates and hydrocarbons, and is neutralized. MEG is also preheated. The MEG to be treated contains a high proportion of water (generally from 10 to 95 wt.%), A quantity of salts that can be high (from Og / l to 90 g / l, for example, or more), the remainder being essentially MEG.
    [0009] It will be noted that the MEG to be treated does not undergo separation of the divalent salts. The divalent salts remain present in the MEG entering the flash balloon described below. The operator has a means of determining the amount of salts in the MEG to be treated.
    [0010] It can be a manual (sample out at a tapping and dosing) or automated (measurement in line or from a sample followed by dosing and servoing). This means is located at the level of the MEG to be treated, or the MEG obtained after separation of the gases and condensates, or the neutralized MEG, and preferably at the level of the neutralized MEG. When the salt content is greater than the threshold of precipitation of said salts in the incoming mixture (to be treated or pretreated), the process operates in the reclaiming phase, which is described below.
    [0011] The MEG to be treated containing water and salts, and preferably derived from the pretreatment, preferably including the neutralization, is sent through line 6 into a separation flask 7. In the bottom of the flask, a mixture of MEG is released. and salts. It comes out at the top of the balloon (line 8) a mixture of MEG and water.
    [0012] This separation of salts is the first step in the so-called reclaiming phase. The separation is carried out at a pressure below atmospheric pressure and preferably between 0.2 and 0.5 bar absolute and at a temperature substantially equal to the boiling point of monethylene glycol (or more generally the solvent). To reach the desired temperature, heat exchangers can be arranged and a reboiler system 27 on the balloon (conventional). This system consumes a lot of energy since large quantities of MEG and water are heated and vaporized. In the bottom of the flask, the MEG mixture and salts are withdrawn (via line 9), and the salts are separated using the appropriate means (means for separating the salts). For example, a sedimentation flask associated with a centrifuge may be used, any means known to those skilled in the art is suitable. The salts are removed from the process (via line 11) and the MEG obtained (usually free of salts) is flash recycled (via line 12), after possible warming.35 MEG mixed with water (from the pipeline 8) is distilled in a vacuum distillation column 13. The water is separated at the top (exiting via the pipe 14) and the purified MEG is recovered at the bottom of the column (via the pipe 15). It can then be recycled for field production.
    [0013] This distillation corresponds to the second stage of the reclaiming. The vacuum is obtained by means of a vacuum system 20 (such as a compressor) located on the pipe 21 for drawing off the gases resulting from the vacuum distillation, said gases having been separated from the water (exiting through the pipe 23) by a separation means 22 located on the pipe 14 for discharging the overhead of the distillation column 13 which operates under vacuum. According to the invention, when the salt content of the MEG to be treated (or pretreated) is below the threshold of precipitation of said salts, the same installation is carried out differently.
    [0014] The reclaiming phase is stopped and a so-called regeneration phase is implemented. For this transition from the reclaiming phase to the regeneration phase, there is provided on the installation a valve 16 on the pipe 9 and which closes the access to the salt separation means, a pipe 17 which connects the bottom of the balloon 7 to the line 15 for withdrawing the purified MEG, said line 17 is provided with a valve 18. The installation is also provided with a pipe 19 making it possible to bypass the vacuum system 20. The method operates more under vacuum, the vacuum system being bypassed (valve 24 closed). The pressure is established at a pressure equal to or greater than atmospheric pressure and preferably between 1 and 2 bar absolute.
    [0015] The MEG entering the flash balloon is separated at a temperature below the degradation temperature of the MEG (or more generally of the solvent) into a first stream of purified monoethylene glycol and a stream of monoethylene glycol and water. Said first stream exits at the bottom of the balloon, and, the valve 16 being closed, the valve 18 being open, it is transferred via the pipe 17 to the pipe 15. Said flow of monoethylene glycol and water is distilled to separate the water and the remaining gases (leaving the line 14) and recover a second stream of purified monoethylene glycol exiting through the pipe 15. In one case, said first and second streams are mixed and discharged for reuse as a solvent. The proportion of flows will depend on the operating conditions, the quality of flash separation and the desired level of purification.
    [0016] In another case, said second stream is optionally recycled to the flash step (balloon 7) via the pipe 29. The valve 28 allows or not this recycling. This valve is closed in the reclaiming phase. Preferably, a portion of said second stream is mixed with said first stream. The mixture is reused as a solvent. The other part of said second stream is recycled to the flash stage (balloon 7). The level of purification of the MEG desired and obtained is greater than 60% by weight and preferably greater than 80% by weight.
    [0017] The water resulting from the process generally contains less than 1% by weight of MEG and preferentially less than 0.1% by weight; it can be reused. It is clear that this method allows significant energy savings (gain in the reboiler system 27 of the separation tank 7 and the vacuum system 20 (such as a compressor) and allows great flexibility in The advantage of operating from one phase to the other is very simple, the advantage being that it can be operated manually or automatically, with appropriate servo-control of the valves according to the salt assays. recovery of the solvent (in particular MEG) which is more than 99.5%, the MEG losses are therefore very minimized, for example, in the case where the MEG to be treated contains 70% by weight of MEG and 30% wt of water, the purified MEG containing 80 wt% of MEG and 20 wt% of water The process in the regeneration phase consumes 30% of the energy consumed by the process in reclaiming phase which provides a gain in energy The process and installation described for the MEG are suitable for other solvents used in the treatment of gases such as alkanolamines, and for example monoethanolamine (MEA), diethanolamine (DEA), methyldiethanolamine (MDEA), etc..30
    权利要求:
    Claims (9)
    [0001]
    REVENDICATIONS1. A process for purifying a hydrate-inhibiting solvent, said solvent having a boiling point higher than that of water and being, at least at least one time, in admixture with water and salts, process which comprises: - optionally, a pretreatment of said solvent to be treated, said pretreatment at least partly separating the hydrocarbons, the condensates and the gases, and said pretreatment optionally comprising the addition of chemical neutralization agent, - a reclaiming phase implementation when the salt content of said solvent to be treated, optionally pretreated, reaches the precipitation threshold in the treated mixture - said phase comprising a flash under vacuum, operating at a pressure below atmospheric pressure and preferably between 0.2 and 0.5 absolute bar and at a temperature below the degradation temperature of the solvent, whereby a flow of solvent containing t salts and a vaporized stream of solvent and water, said stream of solvent and water is distilled under vacuum at a pressure substantially equal to that prevailing in said vacuum flash to separate the water and recover a stream of purified solvent, the salts are separated from said stream of solvent containing the salts, then the solvent obtained is flash recycled, - when said salt content in the treated mixture is below the precipitation threshold, the reclaiming phase is stopped and a so-called regeneration phase is implemented, - said regeneration phase comprising the removal of vacuum, the solvent to be treated, optionally pretreated, undergoing a flash step, operating at a pressure equal to or greater than atmospheric pressure and preferably between 1 and 2 bar absolute and at a temperature below the degradation temperature of the solvent, whereby a first stream of purified solvent is obtained. t a stream of solvent and water, said stream of solvent and water is distilled under a pressure substantially equal to that prevailing in said flash, the water is separated and a second stream of purified solvent is obtained, said second stream being mixed with said first stream, and / or recycled to said flash.
    [0002]
    2. The process of claim 1 wherein the solvent is monoethylene glycol.
    [0003]
    The process of claim 1 wherein the solvent is an alkanolamine.
    [0004]
    4. The method of claim 3 wherein the solvent is selected from the group consisting of monoethanolamine (MEA), diethanolamine (DEA), methyldiethanolamine (MDEA).
    [0005]
    5. Method according to one of the preceding claims wherein the solvent to be treated does not undergo treatment to separate the divalent salts.
    [0006]
    6. A purification plant for a hydrate-inhibiting solvent, said solvent having a boiling point higher than that of water and being, at least at least one time, in a mixture with water and salts, said installation comprising: - a flash balloon 7 provided with a pipe 6 for introducing the solvent to be treated, a pipe 8 for the exit of a mixture of solvent and water, a pipe 9 of leaving a mixture of solvent and salts, - a means 10 for separating salts provided with a pipe 9bis for introducing the mixture of solvent and salts, said pipe 9bis comprising a valve 16, the means 10 being also provided an outlet pipe 11 for separating the separated salts and a pipe 12 for discharging the solvent separated from the salts, said pipe 12 being connected to the flash tank 7 and provided with a valve 26, a distillation column 13 capable of operating under vacuum, provided with a pipe 6 of introduction 8 of said mel solvent and water angel, an outlet pipe 15 of the purified solvent located at the bottom of the column, an outlet pipe 14 of water and gas, located at the head of the column, - a pipe 17 provided with a valve 18 connecting said pipe 9 to the outlet pipe 15 of the purified solvent - a vacuum system 20 which can deliver a reduced pressure in the distillation column and the flash balloon, a pipe 19 by-pass of said system and valves 24 and 25 respectively at said system and the bypass pipe, -a pipe 29 provided with a valve 28, connecting the pipe 15 to the flash tank 7, and said installation operating in two phases according to the content of salts of the solvent delivered by the metering means: in one of the phases, the valves 18, 25 and 28 are closed, the valves 26, 16 and 24 are open, and the said vacuum system provides a reduced pressure - in the other phase, the valves 16, 26 and 24 are closed, the valves 18, 25 and 28 are open and said vacuum system is stopped.
    [0007]
    7. Installation according to claim 6, comprising upstream of the flash balloon, a means 4 for separating hydrocarbons, condensates and gases.
    [0008]
    8. Installation according to claim 6 or 7, comprising a pipe 5 for the introduction of a chemical neutralization agent.
    [0009]
    9. Installation according to one of claims 6 to 8, comprising a pipe 14 for introducing water and gas into a means 22 for separating the gases from said water, said means comprising an outlet pipe 23 of the water and a pipe 21 of gas outlet, said pipe 21 being connected to the vacuum system 20.
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    法律状态:
    2015-11-05| PLFP| Fee payment|Year of fee payment: 3 |
    2016-11-21| PLFP| Fee payment|Year of fee payment: 4 |
    2017-11-28| PLFP| Fee payment|Year of fee payment: 5 |
    2019-11-28| PLFP| Fee payment|Year of fee payment: 7 |
    2020-10-02| TP| Transmission of property|Owner name: AXENS, FR Effective date: 20200826 |
    2021-08-06| ST| Notification of lapse|Effective date: 20210705 |
    优先权:
    申请号 | 申请日 | 专利标题
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