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WO1999041591A1 - Regulation de la teneur en eau d'un procede de reformage catalytique servant a produire des composants de melange d'essence, au moyen d'une spectroscopie dans l'infrarouge proche - Google Patents

Regulation de la teneur en eau d'un procede de reformage catalytique servant a produire des composants de melange d'essence, au moyen d'une spectroscopie dans l'infrarouge proche Download PDF

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Publication number
WO1999041591A1
WO1999041591A1 PCT/GB1999/000367 GB9900367W WO9941591A1 WO 1999041591 A1 WO1999041591 A1 WO 1999041591A1 GB 9900367 W GB9900367 W GB 9900367W WO 9941591 A1 WO9941591 A1 WO 9941591A1
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WO
WIPO (PCT)
Prior art keywords
water
reactor
absorbance
stream
chloride
Prior art date
Application number
PCT/GB1999/000367
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English (en)
Inventor
Henryk Herman
Maurice John Roebuck
Original Assignee
Bp Oil International Limited
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Bp Oil International Limited filed Critical Bp Oil International Limited
Priority to AU24349/99A priority Critical patent/AU2434999A/en
Publication of WO1999041591A1 publication Critical patent/WO1999041591A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G35/00—Reforming naphtha
    • C10G35/04—Catalytic reforming
    • C10G35/06—Catalytic reforming characterised by the catalyst used
    • C10G35/085—Catalytic reforming characterised by the catalyst used containing platinum group metals or compounds thereof
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3554—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for determining moisture content
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; Viscous liquids; Paints; Inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G01N33/2829—Mixtures of fuels
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N2021/8411—Application to online plant, process monitoring
    • G01N2021/8416—Application to online plant, process monitoring and process controlling, not otherwise provided for
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids

Definitions

  • the present invention relates to a method for controlling the water content of a reaction susceptible to water, in particular the catalytic reforming of hydrocarbons to produce a gasoline blending component.
  • the catalytic reforming of hydrocarbon feedstocks is effected by contacting 5 the feedstock with hydrogen at elevated temperature in the presence of a catalyst.
  • the catalyst may comprise a Group Vffi metal component, for example platinum, preferably with one or more promoters, for example, rhenium and/or tin, germanium or indium.
  • the catalyst is usually supported, for example, on an inorganic oxide such as alumina or on a zeolite.
  • the base supports chloride ions to
  • the reforming operation produces under pressure a reactor product which is cooled to give a liquid and a gas which are separated, the gas being usually recycled to the reformer and the excess exported for use elsewhere in the refinery; the pressure in the liquid is then reduced giving a second liquid (reformate gasoline) and some gas which can be used elsewhere in the
  • the reactor product comprises predominately C5+ hydrocarbons together with smaller quantities of Hydrogen and C1-C4 hydrocarbons, which are especially in the two gas streams.
  • Water is often present in the reactant stream e.g. a naptha feed contains typically l-3ppm by volume of water.
  • the catalyst must have some acidic character to promote isomerisation of reactant molecules which is required along with dehydrogenation for successful reforming reactions to occur. However, if the system contains too much water initially the catalyst is activated to such a degree that it possesses too much acidic character which leads to hydrocracking of the
  • coke In a reforming process coke accumulates on the catalyst thereby deactivating it, reducing its lifetime and decreasing the reformate yield.
  • the extent of coke accumulation can be reduced by maintaining a constant water/chloride ratio of the catalyst. If this ratio increases above that of a desired level the extent of coke accumulation on the catalyst will increase.
  • a known method of maintaining the water/chloride balance involves the determination of the water content in the catalytic reforming unit (CRU). If the water/chloride ratio is below that desired, water is added to the CRU. Alternatively if the water/chloride ratio is above that desired it may be reduced by drying the feedstock or removing excess moisture from the recycle gas and/or adding chloride at a higher than normal level to the reaction system until the water content returns to the desired level.
  • the water content of a CRU can be determined using a moisture meter usually fitted on line.
  • impedance water meters are unreliable as they cannot cope with the wide variation of moisture levels seen in reformer operations, impedance devices take a significant time eg 16 hr to respond to changes (during which time the catalyst is being deactivated) and there is an inherent unreliability that leads to mistrust of readings.
  • frequent calibration is required for accurate measurements and they are delicate instruments. Therefore there remains the need for an improved method of monitoring and subsequently controlling the water content in a catalytic reforming process as well as many other processes in particular catalytic processes susceptible to water.
  • NIR Near-Infrared
  • the present invention provides a method for monitoring, and preferably controlling the amount of water in a reactor of a reaction susceptible to the presence of water, which process comprises passing at least one feedstream into said reactor, effecting reaction in said reactor to produce at least one product and withdrawing at least one product stream from said reactor, with analysis of at least one of a feedstream, reactor contents and product stream or a fraction thereof, in particular of a gas stream , by visible and/or near infra red spectroscopy in the wavelength range 800-2650nm to determine an absorbance for water or correlatable to water, and then preferably comparing said absorbance or a function thereof or the amount of water corresponding to said absorbance with a desired value, and so adjusting the process based in said comparison to minimise the difference from said desired value.
  • the particular absorbance(s) in the NIR may be in the region of the 2000-
  • absorbances are especially preferred in the 1800- 1900nm region. Only one absorbance in the NIR region may be used, but advantageously the absorbances at at least 2 wavelengths, are chosen, e.g. 2-4 such as 2 or 3 especially within 300 nm of each other.
  • the absorbances may be chosen because of known absorption of water at that wavelength or may be chosen statistically by regression analysis e.g. partial least squares (PLS) or multi linear regression MLR because of the correlation there with the water amount. Examples of suitable wavelengths are at 2592 - 2597 e.g.
  • 1845 - 1850 e.g. 1847 or 1848nm are preferred.
  • direct correlation was found at 2595 and 1847nm between water contents measured by other devices and the amount of absorbance seen at each wavelength at moisture levels ranging from 1000-1200 ppm (vol).
  • the absorbances may be measured on samples of the appropriate stream, these samples being taken from the stream manually for analysis in a separate cell, or preferably through a pipe acting as a spectroscopy analysis cell e.g. containing an NIR probe. Especially, the absorbance may be measured directly on the appropriate stream e.g. via a probe inserted directly into the stream, in which case the absorbance is measured effectively on line and in real time.
  • the cell path lengths vary according to the wavelength of the absorbance, being e.g. OJ-lm for wavelength of 1600-2650 nm and, 1-lOm for wavelengths of 800-1500 nm.
  • the NIR radiation source and detector in the NIR spectrophotometer may be close to the cell, but are preferably spaced therefrom e.g. by l-lOOOm in particular 5-100m, the radiation passing to and from the cell by way of an optical waveguide e.g. one or more optical fibres.
  • the optical fibres transmit the NIR radiation of the chosen wavelength and may consist of zirconium fluoride for wavelengths of 2000-2650 nm, and silica or glass for lower wavelengths.
  • the absolute size of the absorption is reduced as the wavelength chosen becomes smaller.
  • the 1600-1900 nm region is chosen with optical fibres e.g. of silica , quartz or glass leading to a spectrophotometer 5- 100m away from the cell.
  • the NIR spectrophotometer is preferably able to scan with a resolution of less than 10cm "1 e.g. less than 4 cm "1 .
  • the radiation from source to cell to detector may pass to only one cell or may, via a multiplexer, be passed in parallel to a series of cells with parallel return to the detector.
  • the absorbance signal may be converted to a figure for the water content either directly by the Beer Lambert Law of absorbance proportional to concentration of absorbent, if at that wavelength, the simple linear relationship applies. Otherwise the relationship may be determined by calibration with if required statistical analysis of the data on the reaction with a variety of water contents (measured independently by standard means) and hence a variety of absorptions; the statistical methods may be by multilinear regression (MLR) or partial least squares (PLS) or other regression techniques. Statistical analysis may also be used to determine the optimum wavelength(s) to choose correlatable to the water content.
  • MLR multilinear regression
  • PLS partial least squares
  • the absorbance data may be mathematically processed; functions of the absorbances such as derivatives e.g. first, second or third derivatives may be used in the statistical analysis.
  • the relationship between absorbance (or function thereof e.g. derivative) and water content is thus found and may involve more than one wavelength, with a regression equation having linear terms, quadratic terms and/or reciprocal terms.
  • An example of such an equation is
  • [Water content] A, + ⁇ Ai ⁇ i where A > is a constant and A_ is multiplier constant for the absorbance (or derivative) ⁇ i at wavelength 1 (or wavenumber 1).
  • reaction conditions e.g. temperature, pressure, feed rate(s), ratios of feeds, space time yield, and analysis of catalyst are kept constant, while the water content is systematically varied.
  • the calibrations may then if desired be repeated with variations in the conditions.
  • the method of the invention may be applied to a reaction under the same conditions, to obtain the absolute water content of the analysed stream. If the obtained value deviates from the desired value then the rate of water addition is adjusted to minimise the difference from that desired value. Deviations are kept usually below 10% from the desired value, in particular below 5% from that value. If desired, the absolute water content need not be determined, so long as a function related thereto is obtained and the process controlled to minimise deviations in the value of that function, e.g. with the size of deviations as shown above. The deviations may be determined by computer and the adjustments to control the process and minimise it may also be made by computer. Examples of such reactions are naphtha dehydrogenation, paraffin isomerisation and also dehydrocyclisation reactions.
  • the method is particularly applicable to catalysed reforming reactions in which an organic hydrocarbon feedstock e.g. naphtha or a mixture of 6-12 alkanes is passed in the vapour phase over a solid catalyst activated by chloride ion, and in the presence of hydrogen.
  • an organic hydrocarbon feedstock e.g. naphtha or a mixture of 6-12 alkanes is passed in the vapour phase over a solid catalyst activated by chloride ion, and in the presence of hydrogen.
  • the catalyst may be activated by addition of chloride ion e.g. as metal chloride in the catalyst production or hydrogen chloride addition to the feedstream or as a separate feedstream. Once the catalyst is activated, the chloride addition may be stopped or may be periodic or continuous at a lower level to maintain the activity.
  • the water/chloride ratio of the catalyst is a very important parameter as it correlates with the tendency of the catalyst to coke and corresponding C5+ and hydrogen yield loss, and therefore relates to its total and single cycle lifetime.
  • the catalyst activity is reduced due to coking.
  • the catalysed reforming may involve operation with a swing, semi regeneration or continuous catalyst regeneration system.
  • the catalytic reforming is performed in at least one reactor e.g. 1-10 reactors especially 2-4 reactors.
  • the analyses may be performed in gas streams passing between the reactors, but preferably are on gas products separated from the overall reaction product.
  • the water content of the gas stream(s) is preferably controlled to 1-50 ppm in particular 5-20 ppm.
  • the method of the invention may be used to determine water content of the desired stream, especially a gaseous product stream, for subsequent or simultaneous use in control purposes whether manually or automatically via a computer control of the process.
  • the method may also be applied directly to measure the chloride level of a product stream (in particular the same one), again by calibration, based on NIR absorbance at the appropriate wavelength, examples of which are 1785.15 and 1737.9nm for hydrogen chloride.
  • the water/chloride ratio in the product stream can be determined and from deviations from the desired value, adjustments made to the level of water and/or chloride addition to minimise those deviations and control the process; if the level of water in the reactor and product stream is too high then the water content of a feedstream may be reduced e.g.
  • the chloride level in the gaseous stream for use in the calibration is usually and preferably measured using conventional methods such as Draeger tubes. If desired the water level may be found by NIR and the chloride by conventional means to obtain a value for the water/chloride ratio.
  • the water/chloride ratio is found from its known correlation with the ratios in the product of two hydrocarbons (gaseous at 25°C and 1 atmosphere) preferably differing by 1, 2 or 3 carbons, especially the pair of 3 and 1 carbon content hydrocarbons, or the total of 3+4 to 1+2 carbons; the ratio of 2 to 1 hydrocarbons may be used.
  • the ratio of C 3 to Ci hydrocarbons is preferred.
  • This correlation is described widely in reference literature and is known to the expert in the reforming art.
  • the correlation equations are determined for one or more conditions of operation e.g. temperature, pressure, nature of feed stock and catalyst.
  • the method of the invention may be applied to the reaction by NIR analysis of the product stream to determine the water content (the absolute level of water) and also by NIR analysis for said gaseous hydrocarbons especially for propane and methane, preferably in the same region e.g. within 300 nm of the wavelength used for the water determination.
  • absorbances for propane are found between 1670 and 1850 nm, and for methane between 1620 and 1820 nm especially 1620- 1660 nm.
  • the measurements of the NIR absorptions of the water, propane and methane are usually done simultaneously and the absolute level of water and the relative levels of propane to methane are found and, from the ratio of the latter, the water/chloride level in the product (and hence in the reactor).
  • the present invention provides a method of determining, and preferably controlling, the water level in a reactor of a catalytic reforming reaction over a catalyst comprising chloride, which process comprises passing at least one hydrocarbon feedstream into said reactor, effecting reaction in said reactor to produce at least one product, usually a gasoline blending component and at least one gas stream, and withdrawing at least one product stream from said reactor, with analysis of at least one product stream or fraction thereof by near infra red spectroscopy in the wavelength range 1600-1900nm with passage of transmission and absorbance radiation through the stream (or fraction) with the NIR source and detector spaced from the said stream by at least one optical fibre to determine an absorbance for water or correlatable to water, and then preferably comparing said absorbance (or a function thereof) or the amount of water corresponding to said absorbance with a desired value, and adjusting the process based on said comparison to minimise the difference from said desired value.
  • the NIR analysis also involves measuring the absorbance for propane and methane or an absorbance correlatable therewith (or a function thereof) to obtain a ratio of propane to methane and hence the water/chloride ratio in the reactor and then adjusting addition of water and/or chloride to bring the water/chloride ratio in the reactor to the desired level.
  • the products of the reaction comprise a gasoline blending component and lower hydrocarbons which are gaseous at 25°C and 1 atmosphere pressure, such as ones of 1-4 carbons.
  • the product stream may be separated in one or more stages e.g. by cooling and/or depressurisation at least partly to give one or more liquid streams comprising the gasoline blending component fractions and one or more gaseous streams comprising said hydrocarbons.
  • At least a portion of one of said gaseous streams may be recycled to the reactor, e.g. the first gas stream separated from the product stream e.g. after cooling (e.g. in a high pressure separator) and/or the second gas stream separated from the product stream e.g. after pressure reduction e.g.
  • the first gas stream is partly recycled to the reactor (or reactors) and partly passes out of the reforming plant as plant exit gas (excess gas recycle stream).
  • the gas from the pressure reduction is not recycled to the reactor but passes out of the plant as stabilizer exit gas (or stripped gas stream).
  • These streams may thus be a gas recycle stream, excess gas recycle stream or stripped gas stream. Analysis for propane/methane may be performed on one or more of these streams.
  • the method of control is usually operated by adjustment to the process because of deviations from the above values.
  • a signal related to that absolute level may be used and comparisons made between that and a desired level for that signal.
  • a ratio of absorbance signals or derivative signals may be used instead of the absolute values for the water and/or gaseous hydrocarbons themselves. In this way the reaction may be more easily be computer controlled.
  • the method of the present invention can give a rapid accurate measurement of water content (or a parameter related thereto), usually in real time eg less than 5 minutes, and provides the facility for rapid response to changes (especially large changes) in water content to control the process faster than is possible with water meters and/or gas chromatography.
  • the level of water detectable may vary from 1 to 30,000ppm, usually 10 to 1500 ppm, especially 60-500 ppm or 2-100 ppm.
  • tehre is provided the use of visible and/or near infra red spectroscopy in the wavelength range 800-2650nm in a method for monitoring the amount of water in a reforming reaction in which an organic feedstock is passed in the vapour phase and in the presence of hydrogen, over a solid catalyst activated by chloride ion.
  • the invention is illustrated in the following examples.
  • Hydrotreated naptha (liquid feed) containing primarily Cs-C ⁇ hydrocarbons was fed into a reforming reactor in conjunction with hydrogen.
  • the reactor was at a pressure of 20 atm and temperatures of between the 500-510°C.
  • the reactor H 2 hydrocarbon mole ratio was 6: 1.
  • the catalyst was Pt on alumina promoted by Re.
  • the reaction product leaving the reactor was cooled to give a liquid product and a gaseous one (PEG, exit recycle gas), which was recycled to the front end of the reactor.
  • the liquid product was depressurized to give a second gas stream (SEG stabilized exit as stream) which was also recycled to the reactor and a stabilized product (reformate).
  • a 100mm path cell was set up in the sample compartment of a B omen MB 120 NIR spectrometer.
  • a background transmittance spectrum was obtained of ambient air containing 3000ppm water (as determined by impedance water meter) over the range 3700 to 8000cm "1 [1250-2702nm] resolution of 4cm "1 .
  • a 150mm path cell was set up in the sample compartment of the spectrometer and fitted to the PEG and SEG gas flows. The spectra were obtained over the range 3800 to 6300cm "1 (2631-1587 nm).
  • the regression equation for methane was as follows.
  • the % concentration of methane 5.58 ⁇ (O n -A,), where otn is the MLR coefficient (Multiplier constant) associated with wavenumber n, and A, is the actual absorbance of the sample, measured at wavenumber n.

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Abstract

La présente invention concerne un procédé de régulation de la quantité d'eau présente dans un réacteur, dans une réaction sensible à la présence d'eau, ce procédé comprenant les étapes consistant: a) à faire passer au moins un courant d'alimentation dans ce réacteur, b) à faire se produire la réaction, dans le réacteur, afin d'obtenir au moins un produit, et c) à retirer au moins un courant de produit à partir de ce réacteur, en analysant au moins un des courants d'alimentation, le contenu du réacteur ou le courant de produit ou une fraction de ceux-ci, au moyen d'une spectroscopie dans l'infrarouge proche, dans une gamme de longueurs d'onde comprise entre 800 et 2650 nm, afin de déterminer l'absorbance du rayonnement par l'eau ou l'absorbance en rapport avec l'eau.
PCT/GB1999/000367 1998-02-10 1999-02-04 Regulation de la teneur en eau d'un procede de reformage catalytique servant a produire des composants de melange d'essence, au moyen d'une spectroscopie dans l'infrarouge proche WO1999041591A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU24349/99A AU2434999A (en) 1998-02-10 1999-02-04 Controlling water content of a catalytic reforming process for producing gasoline blending components using near infrared spectroscopy

Applications Claiming Priority (2)

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GB9802695.8 1998-02-10
GBGB9802695.8A GB9802695D0 (en) 1998-02-10 1998-02-10 Process control

Publications (1)

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WO1999041591A1 true WO1999041591A1 (fr) 1999-08-19

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