DE1623002A1 - Device for determining the flash point of a liquid and method for controlling a process with the aid of the device - Google Patents

Description

1.ING. F. WUBSTHOFF 8 MÜNCfiBN 9

DIP] J. ING. G. PITIiS SCHWEIOEHSTRASSE 2 DR.B.T.PKOHMANN til »ox SSOOSl I PBOTBOTPATBKT HÜHOBBU

1A-30 216

Boson friction to the patent application

SHELL INTERNATIONAL RESEAROH MAATSOHAPPIJ S.V.,

Hague, Netherlands

concerning

device to beat the flashpointa of a liquid and Procedure for rules a proceaaea with the help of the device .

The invention relates to a device for determining the flash point of a liquid, and it relates in particular to a device for determining and possibly for registering the flash point of a continuous stream of liquid which is passed through the device. *. Furthermore, the invention provides a method for a process, e.g. a distillation process, a dewaxing process, an extraction or asphalt removal process, based on the flash point of a product of the process in question.

It is well known that the flash point of a liquid hydrocarbon, in particular a petroleum product to be tested with the aid of an apparatus which in combination comprises an ignition chamber, furthermore arranged outside this chamber Means for heating a stream of the liquid to be tested as well as for heating an oxygen-containing gas, e.g.

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Air, means for introducing the heated liquid and gas into the chamber, means for maintaining a puddle formed by the liquid in the chamber at a constant or substantially constant level, means for an ignition spark in the ignition chamber above the puddle and in the presence of the gas mentioned, i.d_tfcel to determine the temperature of the liquid puddle in the chamber, as well as means to automatically detect the occurrence of a flame or a light phenomenon in the chamber. The temperature of the liquid can be measured ψ automatically at the moment in which a Lichterscheii-uri ^ occurs in the fighting compartment of the Entflananunjskanuner.

If it is ensured that the heating means for the liquid gradually increase the temperature of the liquid supplied to the jintflammunskimr.er, and if one provides means to control the heating means with the help of the means for lighting the lights that the lenperatur the liquid at least substantially at the value _ö e is old, in which takes place the Jüntflammung the liquid, P can be a Flüssi-- the flash point _temperature: keitsstroms repeated continuously, and measure \ in relatively short time intervals.

The device described above is used to determine the flash point of light petroleum products, e.g. of gasoline and To measure kerosene, with flash points up to about 85 ° 0; however, it has been shown that this is known The device is not suitable for testing liquids with a flash point higher than this virus value, because it occurs

: an irregular ignition when you try to keep the flame

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point of liquids with a higher flash point is than about 85 C,

<It is now an object of the invention to provide an apparatus

to provide, which is particularly suitable, a liquid to check that has a relatively high flash point temperature, as is the case, for example, with a lubricating oil distillate; However This device can also be used to test liquids that have a relatively low flash point.

For this purpose the .hrfiiidunj sees a device for testing or measuring the fla-iinpunktes of liquids before that with improved irritants for the resulting vapors and / or is equipped for the liquid to be tested.

A feature of the invention is the device with separate heating means! verser.en for the steam room of the flame chamber; this x ^ itfianunuii.fskaminer *. is referred to in the föl end as the steam chamber. The steam chamber is adjacent to the liquid chamber and is preferably arranged above the latter. The liquid tank and the steam chamber together form the de-flaxnmun ^ skananrr; Usually there is a splash guard, for example an intermediate floor with a bubble cap between the two lianmern. Stationary an.'Gorai.et t -In the preferred embodiment of the invention: xtecel means are provided that respond when the inflammation detector detects an ignition to the separate Heizini tel for the Darrpfka tuners temporarily. Switch on or reduce their effectiveness. Jie V'erringerur.r the -ie i ζ effect or switching off this .. ^r -izr: ± \ ~ el can affect the

s / e e

i'alls, _t ^: ed ^ ^Y. : ._: '.: ν v. ^ twe. licer ^ veice in a r «eziel * .ua - to the

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_4- ι via. VWν «. 1Δ-30 216 time interval between the individual sparks. .

A second feature of the invention relates to the use of a preheater for the supplied liquid stream in connection with control means, which depend on the temperature difference at the mentioned main heating means for the liquid or for both the liquid and the gas, when the two substances are heated together in the main heating device, this arrangement being used for this purpose to keep the temperature difference mentioned at a constant value or at least essentially at a constant value. In a preferred embodiment of the derate, both are Features provided at the same time.

Preferably, the liquid stream and the Gaestrom in a combined heating device are respectively "a saturator heated, which is closely adjacent the Entflammungskammer and forms a structural unit with it · The saturator, which is usually heated from the inside, for example by means of a patronenformigen heater _t can be formed by a helical channel which opens into the liquid chamber.

As already mentioned, the known device for determining the flash point of a liquid is with a heating device which serves to maintain the temperature of the liquid

to increase gradually; control means are also provided, which are controlled by the flame detector to the The temperature of the liquid is at least substantially at the To hold the value at which ignition occurs. At a loading

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In the preferred embodiment of the invention, the heating effect is progressively increased as long as no ignition occurs} as soon as an ignition is detected, the heating effect is progressively reduced during the ignition period, and when there is no more flame, the heating effect is gradually increased again, etc.

When checking or measuring the flashpoints of liquids The known flash point detectors have a relatively high flash point proved to be unreliable, primarily because of the high temperatures that occur in the steam chamber. Now a new device has been developed which comprises a housing with a membrane, the membrane preferably consisting of the one protected by law Designation consists of Teflon available material; this membrane is in open connection on one side via a pipeline with the steam room.

The occurrence of a pressure wave caused 'by a fire is generated, leads to a displacement of the membrane and this displacement can be in a suitable manner, e.g. mechanically, optically or electrically displayed, registered and / or in a control signal being transformed. Preferably, the other side of the diaphragm affects an electrical circuit, e.g., through actuation an och switch. The connection line is usually made as short as possible. This device offers the the added benefit of not having them in the steam room resulting combustion products is contaminated.

The device for measuring the flash point temperature can be used be to a process based on the flash point of a

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Product to regulate this process. A sample bromine of the product is fed to the device, the flash point temperature is measured, and a signal corresponding to the measured temperature is fed to a controller; the output of the regulator is then used to regulate the process in such a way that the product of the process has at least approximately a constant flash point. Alternatively, the sealing can serve to prevent the flash point of the product from exceeding a predetermined limit value. Such a regulation can, for example, in the case of propane deasphalting; of asphalt-containing residues as well as in ^: extraction processes used, e.g. in furfural extraction or when dewaxing lubricating oils with the help of solvents. ·

The solvents used are made up of the various ! Phases that arise in these processes are removed; eggs The flash point of these phases is a sensitive indicator of the extent to which the * solvent »removal is carried out the solvent from the phases in question can be used with help of the invention Sö'emäxien device in the above-described V / can be regulated.

j The invention is described below with the aid of hand sclie ^ atiscner Drawings explained in more detail using an exemplary embodiment.

Fig. 1 shows schematically and in a vertical iJchnibt one form of an apparatus for erfindun _o sgeraäßen Lessen of Flamiapunkttemperaturen. This uerät essentially comprises two main parts, namely an inflammation chamber 1 and a heating or saturation device 2, which is immediately adjacent to the Kamtier 1 and forms a structural unit with it. the

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Inflammation chamber comprises a liquid chamber 3 and a • directly above this arranged steam chamber 4. The steam chamber is equipped with spark generating means 5 *, which at 6 connected to a high voltage source or a spark generator are; also at 7 is an outlet for the vapors

[ intended. At 5 v / sparks earth at regular intervals generated by e.g. 10 see. Direct current is commonly used for this purpose, but alternating current sparks can be used if desired work.

The steam chamber is through a short line 8 with a Flame detector 9 connected, the essentially one Includes membrane 10, which can act on an electrical switch 11 · The membrane is preferably made of Teflon, and its · Diameter can be about 150 mm. Shock waves generated by an ignition in the steam chamber become detected with the help of the membrane, which opens or closes the switch 11 briefly with every ignition /.

The liquid to be tested is supplied at 12 according to FIG. 1 ι a measured flow of an oxygen-containing gas * normally by air, is supplied at 13 and'mit the Liquid mixed before these substances in the saturation device 2 are heated. In one particular case, it was fraudulent. the liquid or oil throughput about 4.5 ltr / h, while the throughput of oxygen-containing gas (air) was about 14 ltr / h; these throughput rates can vary within wide limits; they depend, among other things, on the type of liquid to be tested and the oxygen-containing one used

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The saturation device comprises a cartridge-shaped one Heating element 14, which is in a helical channel

15 is arranged. The electricity is supplied to the heating element via connections

16 supplied.

The liquid and gas mixture rises up along the helical channel 15 and enters the liquid chamber 3 at 17. Here, the ocher force causes the liquid to be separated from the vapor; a splash guard 18 prevents drops of liquid from being carried along and entering the steam chamber M.

The heated liquid forms a puddle in the liquid chamber 3; a constant height of the puddle is thereby maintain that for the liquid as an outlet an over-7 Running pipe 19 with a weir 20 is provided.

A temperature measuring device 21, e.g. a thermocouple, is arranged in the outlet 17 of the saturation device in order to Measure the temperature of the liquid under test under the test conditions; this temperature can be recorded by a recorder are displayed.

According to the invention, the steam chamber is provided with separate heating means 23, for example an annular heating element, which can be connected to a power source at 2.M-. In order to compensate for the heat of combustion that is generated when the steam in the steam chamber is ignited, the heat supplied by means of the conduction device 23 is reduced, or the heating device is preferably switched off as soon as an untflarxur.-; occurs, "if-the formation of the flaim ceases, becomes

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the supply of heat with the aid of the heating device 23 again recorded.

According to a further feature of the invention is. in the Line 12 a preheater for the liquid flow to be supplied is switched on} this preheater is in FIG. 1 at 25 indicated schematically} it can be of a similar construction like the saturator, i.e. it can essentially be a housing, a helical channel for the Liquid and a cartridge-shaped one arranged inside Include heating element. |

Thus, through the saturation device 2 only 'one Part of the heat to be supplied to the supplied liquid flow is applied, and usually most of the heat is with it The aid of the preheater 25 is supplied. A temperature controller 26 a signal for the temperature difference along the saturation device is fed, and this controller causes that the temperature difference by controlling the energy supply. to the preheater 25 on a constant or at least im essential & constant value is kept. For this purpose, j a temperature measuring device 27 is provided, by means of which the temperature at the inlet of the saturation device is measured; the The temperature at the outlet of the saturation device is, 'as before mentioned, measured at 21. Corresponding to these two temperatures Signals are fed to controller 26.

j According to FIG. 1, at 28 on the Hegler 26, a past. !

Btiminter .nert of the temperature difference 'is set, the län ^ s the saturation device is to be maintained} this Temperature difference is usually 15 to 50 ° 0. On this

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Way is' the by the heating element of the saturation device j work to be performed largely constant and the device] can stably cause large disturbances in terms of the misband and the properties of the liquid to be heated; this proves to be particularly advantageous when the liquid flow to be tested has considerable deviations with regard to it shows its flash point.

The device is usually in an explosion-proof Housing arranged, which optionally · with a '-Temperature- control device can be provided.

* The device described above can be operated to determine the flash point of liquids, e.g. to indicate whether a liquid has a predetermined flash point temperature exceeds or not. The heating of the saturation device can in this case be regulated in a manner not shown here so that the amount supplied to the inflammatory chamber Liquid-gas mixture is kept constantly at the predetermined temperature mentioned.

When the device is used for actual flash point measurements is not only used to indicate whether a flash point has occurred that is below a selected temperature, the means for heating the liquid are arranged and operated so that a progressive increase in temperature the liquid supplied to the liquid chamber is fed, and control means for the heating means are also provided, around the temperature of the liquid at least in the v / es borrowed to hold at the value at which ignition occurs. The energy supplied to the heating cartridge 14 is used for this purpose

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decreased or increased, depending on whether the steam in the steam chamber ignites or not «

The complete cone system for the preferred form of training of the apparatus for measuring the flash point temperature is shown in Figs. In FIG. 2, the saturation device 2 is only indicated schematically in comparison to FIG. 1, however, the reference numerals in Fig. 2 correspond to those inFig. 1 reference numbers used.

A direct current spark is generated in the steam chamber every 10 seconds generated with the help of a spark generator 29, which is connected to the terminal | 6 is connected; the generator 29 is powered by an IJotor 30 driven, which performs one revolution in 10 seconds.

If the liquid to be tested has a temperature below its flash point, no Z'Mung occurs and the supply of heat. to the heating cartridge 14 is gradually increased. The saturation device is connected with its connections to an adjustable transformer 31, the is driven by a reversible motor 32, which makes one revolution every 40 minutes. The Lotor 32 drives | the adjustable transformer in such a way that the dem Heating element 14 to = -drained voltage is increased. With this one The ring-shaped heating element of the pressure chamber is in operation electrical energy supplied.

As soon as the "itflanunung" begins, the JEntfla: .un.urv; sdetektor 9 a ^ relay 33 · This x «l .... s is kept in the switched-on -UFi'aad for 9 seconds, and zv: ar durc * a <- »c:. age 34, which is _{betKtict by the w} ie.caen - .. author Ji., which döäi

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Spark generator drives. The relay 33 comprises Eontakte, by means of whose during the period of 9 see the drive motor 32 for the adjustable transformer reversed and the heating of the annular heating element 23 is interrupted. At the end of 9 seo, the heating is switched off again, the ring-shaped heating element is switched on again and the drive of the adjustable transformer is reversed again. A second after that, a new spark is created, and when there is another ignition, it will just be described operation repeated.

Fig. 3 shows a horizontal time scale 35, which extends between 0 and 140 sea. It is assumed that the the first six sparks and the last two sparks cause ignition; this is long the timescale by short vertical lines indicated.

The two lines below the time scale schematically represent the state of the heating element 23 for the steam chamber (upper line 36) and the heating cartridge 14 (lower line 37) represent.

The heating element 23 is either switched on or off, between the 60th and 130th, see is the heating element switched on continuously.

Line 37 illustrates the movement of the drive motor for the adjustable transformer; The output voltage will be from the beginning of the gate passage shown up to rar 60th see of the adjustable transformer continuously extended, however, with the exception of the 1 second period on

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End of each interval of IO sec between two consecutive following spark.

Between the 60th and the 130th see the output voltage continuously increased.

The device described was, among other things, with good success in the continuous determination of the flash point of
Used lubricating oil distillates from a vacuum distillation unit, with flash points of about 22Q ^Q 0 and the viscosity being about 230 centistokes at 38 ° 0.

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Patent claims:

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Claims (9)

P α i1 ü Xi ΐ λ ι «ω 1 'η. U 1J H -ei 1. Device for determining or measuring the flash point of a liquid, characterized by an ignition he scrambled with a liquid comb. and one of these neighboring and preferential, iron above ar) ordered steam chamber, Spark generating means within the steam chamber, "". Means for Evidence of the occurrence of a jintflanimun ^ in the inflammation chamber, Means of heating the liquid to be examined, Means for heating an oxygen-containing gas, i »üttel for ™ Introduction of the heated liquid and the heated gas into the liquid chamber, wherein the heating means or at least the means for heating the liquid for the pouring device are designed in this way are that they enable the I'emperabur of the Liquid to be supplied liquid progressively to increase, with the help of Hegel means, which are re-controlled by the inflammation detector means, to the temperature to keep the liquid at least substantially at a value at which ignition takes place, means to a puddle of liquid with a constant or substantial Maintain constants atand height in the liquid chamber, Means for determining the temperature of the liquid under the test conditions, separate means for heating the vapor chamber and / or pre-heating means for the liquid, which are combined with the sealing means and to it serve, the! temperature difference lan s of the mentioned main heating means for the liquid or for the liquid and the gas at a constant or essentially constant Worth keeping. 009816/1000 BATH ORIGINAL -15- 1Δ-30 216 2. Device according to Claim 1, characterized by regulating or control means to the separate heating means for the steam chamber depending on the detection of ignition temporarily closed by the flame detector means throttle or switch off. 3 »Device 'according to claim 1 or 2, geke η η ζ eich η et by means to bring about a common heating of the liquid and the gas, as well as by means to introduce the gas into the liquid before the liquid-gas Mixture enters the heating device i, which heats the two substances. 4 · Device according to claim 3 »characterized in that the device for heating the liquid and of the gas a heated, preferably an internally heated, helical channel uar ate, which in the Liquid chamber opens. 5 * Device according to claim 3 or 4, characterized in that the heating device for heating the Liquid and the gas of the ignition chamber is immediately adjacent and forms a structural unit with her. 6 · Device according to claim 1 to 5> characterized ge k e η η that a splash guard between the liquid skamm he and the steam chamber is arranged. 7. Device according to claim 1 to 6, characterized in that »iaS the läittel zum i," aol: Y; e ± sen of an inflammation a housing with a preferably made of i'eflon Lenbraa. "ur.fasseii, aas on one oeite of the membrane nit 009816/1000 ORIGINAL BATHROOM -16- 1Δ-30 216 is connected to the steam room, 8. Apparatus according to claim 1 to 7 * characterized in that the control means f ', ir the main heating device are suitable for the supply of heat to the main heating device depending on the fact that an ignition by the flame detector means is proven. 9. Method for regulating a process, e.g. for distilling, dewaxing, extracting or deasphalting, on the basis the flash point of a product of the process, characterized that a sample stream of the product is fed to a device according to claims 1 to 8, that the 2? it is measured that a signal corresponding to the measured temperature is fed to a controller, and that the ■ "■ output signal of this controller is used to control the process ». to settle such that the product of the process takes at least approximately a constant flash point, or that will prevent "that the flash point of the product exceeds a predetermined limit value" \ " 009816/1000 BATH