TWI429479B - Process for mixing a liquid or mixture of a liquid and a fine solid present in an essentially self-containing vessel - Google Patents

Description

Method of mixing a liquid or a mixture of liquids and fine solids present in a substantially self-contained container

The present invention relates to a method of mixing a liquid or a mixture of liquid and fine solids present in a substantially self-contained container, wherein the restriction is that the liquid or mixture only fills the fluid phase can occupy a portion of the internal volume of the container, and the container The remaining occupies of internal volume are filled by the gas phase, the method comprising supplying substantially the same liquid or substantially the same mixture into the vessel as a power jet of the suction device disposed in the liquid or mixture in the vessel.

It is well known that liquid or liquid and mixtures of fine solids are stored in a substantially self-contained container (for example for storage purposes). Typically, such containers are also referred to as cans. Typically, such containers are not completely self-contained, but typically have, for example, at least one withdrawal point through which the contents stored in the container can be withdrawn by, for example, a pump. Correspondingly, the container also typically has at least one feed point through which the contents to be stored can be supplied to the container. A shut-off member, such as a valve or float valve, typically allows liquid or mixture to enter or exit while at the same time ensuring that leakage is prevented when the container is stationary. In a similar manner, an instrument for measuring the temperature, fill level and pressure in the tank (container) can be introduced into the vessel.

Typically, the liquid or liquid and the mixture of fine solids to be stored in the tank are not completely filled with the internal volume that the fluid (gas or liquid) phase can occupy. Instead, one of the internal volumes is partially occupied by the gas phase for a number of different reasons. When the liquid or mixture is stored under normal pressure, in principle substantially the self-contained container can be opened to the atmosphere on the gas phase side (for example via an exhaust system guided through the burner (or another exhaust gas purification system (eg gas scrubbing)) )). The cross-section of the opening is typically first made sufficiently small and secondly to balance the gas with a significant pressure drop during filling and emptying of the container. Usually, the average diameter of the cross-section of such openings 25 cm (usually in the fill volume) 100 m ³ , usually as high as 10,000 m ³ o'clock). Alternatively, in the case of high pressure or low pressure, the relevant storage container is usually also fitted with a device for pressure relief (for example, a shut-off valve) for a response pressure (which can be at or above atmospheric pressure). . Typically, the fill level in the storage tank is continuously measured at a predetermined height in the gas phase and the liquid phase by metering in a small amount (typically <1% by volume/hour based on the gas phase volume in the vessel). When the contents are known, the filling level is calculated in each case directly from the metering pressure difference required for this purpose.

In most cases, the contents of the storage tank as a function of time taken out and/or added need to be mixed from time to time or continuously to increase or ensure uniformity. The reason can be based on a variety of reasons. When the contents of the container are a mixture of liquid and fine solids (e.g., a slurry), there is typically a fine solid that precipitates under gravity during storage in the can, and thereby stratifies the contents of the can during the time period. risk. For example, in the case of extraction from a storage tank, the liquid that may be extracted is no longer the desired mixture but only the liquid present therein. Examples of the above include an aqueous suspension of the polymer. Depending on the specific weight of the liquid phase, the fine solids present in the dispersed distribution may also be creamy and enriched in the liquid/gas phase interface. One possible example of this is a polymer dispersion (also an aqueous dispersion of a polymer).

When only the liquid is stored in the tank (container), it can also be multi-phase (eg emulsion; examples include oil-in-water emulsions and water-in-oil emulsions) and stratify during long-term storage without intermediate homogenization, which is usually What I don't expect.

However, chemically homogeneous liquids can also form undesirable physical inhomogeneities during storage. These may include, for example, a non-uniform temperature distribution (eg, caused by solar radiation on one side of the can). Thereafter the result can be, for example, undesired crystal formation or undesired decomposition of the stored liquid. Typically, a portion of the stored liquid can be continuously withdrawn for the purpose of maintaining the desired storage temperature, directed through a preferred indirect heat exchanger and subsequently recycled to the storage tank. In this case, the storage container operator typically balances the temperature between the liquid still present in the storage container and the liquid circulated therein via the heat exchanger by proper rapid mixing.

For the safe storage of free radical polymerizable compounds (or solutions comprising such compounds), such as acrolein, methacrolein, acrylic acid, methacrylic acid and/or esters thereof (especially C ₁ - to C ₈ -alkyl esters) Not only must the temperature required to control the contents of the liquid tank be carefully controlled. Instead, so-called inhibitors (radical scavengers) must be added to the above-mentioned generally at least monoethylenically unsaturated organic compounds (monomers) to avoid and prevent the unintended initiation of undesired radical polymerization, in most cases. These inhibitors exhibit their full efficacy only in the presence of molecular oxygen, which in turn can be an inhibitor. For this reason, such monomers are typically stored under a gas atmosphere comprising molecular oxygen (see, for example, WO 2005/049543 and U.S. Patent No. 6,910,511), and the liquid monomer (or solution thereof) is not It will deplete the molecular oxygen dissolved in it. For example, the latter can occur when the monomer is temporarily partially crystallized and subsequently restored to solution. The resulting partial depletion of molecular oxygen can be equally offset by proper mixing.

Despite the above-mentioned preventive measures, undesired radical polymerization of the contents of the can still be triggered, by adding the medium for immediately terminating the free radical polymerization to the contents of the cans in a very short time and It is offset very quickly in the contents of the cans (see, for example, WO 00/64947, WO 99/21893, WO 99/24161, WO 99/59717). Also in this case, the contents of the cans need to be mixed extremely evenly and quickly after the addition of the medium.

In principle, the liquid contents of the can can be mixed by, for example, bubbling or spraying a suitable gas (for example via a "spray head") into the tank near the bottom (see Figure 1). The bubbles rising in the contents of the liquid tank complete the desired mixing by entraining the liquid. Thus, regardless of the height of the liquid level, all (in principle, the mixing action is even enhanced from the bottom up) the liquid container contents are thus covered by the large volume flow and effectively mixed. However, the disadvantage of this procedure is the continued need for a suitable mixed gas during mixing (on an industrial scale, a larger gas volume flow is required to mix the contents of the cans). In addition, the gas must be continuously directed back into the tank. In the case of bubbling through the contents of the liquid tank to be mixed, it is usually saturated with the liquid present in the tank, and due to the load (for example in the case of stored organic liquids) it is usually not released in a simple manner To the environment. In contrast, in most cases, relatively complex (expensive) exhaust gas treatment (e.g., combustion (in which case, the combustible gas is combusted in the combustor when it is full) or washing) is required. In principle, the mixed gas that is directed out of the tank can also be recycled back to it for bubbling through its liquid contents. However, an unfavorable system must require a separate circulating gas compressor that recompresses the exhaust gas to a certain pressure at the bottom of the vessel. These compressors are not only expensive but also result in high maintenance levels and considerable energy requirements.

Alternatively, the contents of the can can be mixed by means of a stirrer. However, it requires a separate drive source and a drive shaft that is transported through the walls of the vessel. However, it has generally been found that sealing of the rotating elements that guide through the walls of the container is particularly difficult. In addition, in the case of a tank with a large filling volume (the filling volume of an industrial-scale storage tank is usually 100 m ³ to 10,000 m ³ , usually 200 to 1 000 m ³ or 300 to 800 m ³ , and the characteristic is 500 m ³ ) The manufacture of agitators has been quite expensive.

Based on this background, it has been found that the contents of the liquid tank can be appropriately mixed by the following steps: a portion of the mixture of liquid or liquid and fine solid stored in the tank (container) is extracted therefrom by means of a pump suitable for tank extraction, and via a power nozzle disposed near the bottom of the tank and guided upwards (in the simplest case, a flow passage narrowed in cross section in the flow direction, wherein the pressure energy flowing through the liquid is converted into additional kinetic energy with low loss, and thus the liquid Flow acceleration) Circulates at least some of the extracted portion as a (power liquid) liquid jet (power jet) into the tank.

In this process, a liquid jet that passes through the path of the liquid present in the tank upwardly along its path according to the law of free jet is sucked by the liquid and the liquid medium is mixed. Alternatively or additionally, for mixing purposes, filling with a liquid or mixture (refilling, as well as for the first filling) can be achieved by supplying the liquid or mixture via the power jet described above.

However, the disadvantage of this hybrid method is that the mixing action of the free jet affects only a relatively limited space around it, so the resulting mixing is generally not entirely satisfactory (Fig. 2).

Another disadvantage is that due to the relatively high average momentum density (and velocity) of the liquid jet (especially in the case of a drop in the fill level in the tank), it can relatively easily leave the liquid phase present in the tank (through the liquid and The phase interface between the gas phases), and this departure may be accompanied by intense droplet formation (spray formation) in the gas phase. This is especially disadvantageous when the contents of the can include organic liquids whose gas phase may explode in the presence of molecular oxygen (eg acrolein, methacrolein, acrylic acid, methacrylic acid, esters of such acids or other organic monomers) (See, for example, German Patent No. DE-A 10 2004 034 515). First, the finely distributed droplets in the gas phase increase the content of the organic material, and as a result, the gas phase which was originally impossible to be exploded becomes an explosive gas phase, and the droplets formed are regularly rubbed due to friction as they fly through the gas phase. Put a charge on its surface. The resulting spark discharge can trigger ignition. When the droplets are droplets of an aqueous polymer dispersion, the particles may, for example, irreversibly form a film on the path through the gas phase in an undesired manner and interfere with the polymer dispersion in subsequent use. liquid.

When the content of the can is a slurry in which the fine solid is stored in the liquid, the solid which is thrown onto the inner wall of the container by the jet passing through the interface may adhere to the inner wall, so that the solid is self-storing the slurry in the container. Separated.

However, in the case of another liquid, especially since the small spray droplets have a high vapor pressure, it is also disadvantageous to establish spray formation as described above. This can result in undesired evaporative cooling that impairs the temperature constancy of the contents of the can.

To enhance mixing (see Chemie-Ing. Techn. 42, 1970, pages 474 to 479), in the prior art of Figure 3 of the present application, the mixing chamber (2) (open at the inlet and outlet) is placed in the power nozzle (1) Distal (the numerical number always corresponds to the diagram of this application). As a result, as in the case of free jets, the liquid present in the tank space is not drawn along the jet path, but the amount transmitted according to the law of momentum must pass through the inlet cross section (3) of the mixing chamber (in short) Also known as a momentum exchange chamber or as a momentum exchange tube; although the cross section need not be circular; however, the tubular embodiment is suitable from an application point of view). The arrangement of the power nozzle and the mixing chamber (for example, which is connected downstream of the power nozzle as a short tube having a larger cross section) is hereinafter referred to as a spray nozzle. In which a power jet having a higher velocity enters a smaller momentum exchange chamber than the tank volume (typically, the volume of the momentum exchange chamber is only about 0.0001 to 1% of the inner volume of the tank), and when so, the suction cycle The amount of liquid present in the tank. The manufacturer of such suitable spray nozzles is, for example, GEA Wiegand GmbH in D-76275 Ettlingen.

The mixture flowing out of the momentum exchange tube has a significantly reduced momentum of its elements compared to the power jet (average momentum density is reduced), thereby reducing the probability of the above-mentioned outlet accompanying droplet formation (spray formation) (which will only be at relatively low level phases) Enter at the interface and with attenuated average exit momentum density; see Figure 4). Together with the suction acting from below, the effluent flowing upwardly from the momentum exchange tube according to Figure 5 forms a large volume circulating flow field represented by a continuous field line, which is slightly raised in the spray nozzle obliquely upward and preferably mounted in the tank In the case (see, for example, Acrylate Esters, A Sum mary Of Safety And Handling, 3rd edition, 2002, compiled by Atofina, BASF, Celanese, Dow and Rohm & Haas), which can be improved compared to powered nozzles ( Especially more complete) mixing, however, it is still not entirely satisfactory. Furthermore, when the filling level (phase interface) falls below the suction level, the power jet here also passes through the momentum exchange tube unimpeded and is sprayed to form fine droplets of the above risk (Fig. 6). In general, the power jet liquid must flow through the valve before it enters the injection nozzle, and the valve closes and blocks flow therethrough when the fill level in the tank is below a predetermined level. The mixing action usually also drops from the bottom up.

In view of this prior art, it is an object of the present invention to provide an improved method of mixing liquid tank contents that is applicable to all of the above problems and, in particular, to faster mixing.

Accordingly, the present invention provides a method of mixing (storing) a liquid or a mixture of liquid and fine solids in a substantially self-contained container, wherein the restriction is that the liquid or mixture only fills the internal volume of the container that can be occupied by the fluid phase. a portion and the remaining inner volume of the container is filled with a vapor phase, the method comprising supplying a substantially identical liquid or a substantially identical mixture to the container as a power jet of a suction device disposed in the liquid or mixture in the container, Wherein the suction device draws in the gas from the gas phase present in the container by means of the power jet and releases the inhaled gas together with the power jet into the liquid or mixture present in the container.

Properly according to the invention, the process according to the invention can be carried out in a simple manner by the method comprising withdrawing a portion of the liquid or mixture from the container and circulating at least some of the extracted portion as a component of the suction device power jet. In principle, the power jet of the suction device in the method of the invention may also be at least some (or all) of the liquid or mixture previously present in the container from the container.

If desired, any part of the extracted portion that is not used as a power jet cycle can be transferred to other uses.

It will be appreciated that the process of the present invention can also be practiced with the liquid or mixture fed as a power jet to the vessel excluding the liquid or mixture withdrawn from the vessel. By way of example, this can be supplied to the container by means of a power jet intended to be directed into the container for refilling of the liquid or mixture as a suction device. It will be appreciated that the power jet of the suction device in the method of the invention may also consist of a mixture of liquid or mixture intended to be directed into the container for refilling purposes and a liquid or mixture previously withdrawn from the container.

Generally, the gas phase in the process of the invention does not undergo substantially any chemical conversion. In other words, the gas phase is substantially unconsumed in the process of the invention. In general, when a gas that is aspirated from the gas phase and released together with a power jet to a liquid or mixture present in the vessel is bubbled (rised) through the stored liquid or mixture, the gas 1% by volume, preferably 0.75 vol%, better 0.5% by volume or 0.25 vol% and best A chemical change occurred at 0.1% by volume.

In the simplest form, the method of the invention can be implemented as a suction device by means of an injector (i.e. by the principle of a water jet pump). In this case, the power jet is pumped through a power nozzle mounted in the injector in the following manner: when the power jet passes, for example, via a riser tube that projects into the gas phase of the vessel (which is typically held by a pipe fitting that is fixed to the vessel wall) The gas is aspirated from the gas phase as it passes through the nozzle and is released into the liquid contents of the storage container in the form of separate bubbles together with the power jet. The basic structure and marking of the ejector (also referred to in the literature and hereinafter also as the jet compressor) is shown in Figure 7 (see also Chem.-Ing. Techn. 47., 1975/5, page 209; Chemie- Ing.-Techn.MS201/75;vt>>verfahrenstechnik<<15(1981) No.10, pp. 738-749; "Untersuchungen an Wasserstrahl-Luftpumpen mit einem einzigen kreiszylindrischen Treibstrahl"[Investigations on water-jet air pumps With a single cylindrical motive jet], DIGvPawek-Rammingen, Thesis 1936, Brunswick Technical University; and "Mixing shocks and their influence on the design of liquid-gas ejectors", JH Witte, Thesis, Technical University, Delft (December 1962) ).

The ejector (see, for example, Figure 7) typically consists of (or includes) a power nozzle (1), a suction chamber (4) (which typically surrounds the power nozzle), and an inlet to the mixing chamber (usually a mixing tube) (5) ), mixing tube (mixing chamber) (6) and diffuser (7). A rapid jet of power liquid exiting the power nozzle, which is pumped into the injector at point (0), creates a low pressure in the suction chamber. As a result, the gas is drawn (sent) from the suction chamber (the inlet (8) is connected to the gas phase in the vessel (above the interface), for example via a gas permeable connection (for example a suitable riser)) and due to the mixing tube (mixing chamber) And the momentum exchange between the motive liquid and the gas in the diffuser is compressed, dispersed in the motive liquid and released together with the tank liquid. As the gas rises in the latter, the bubbles carry away the liquid and produce the desired mixing in the stored liquid or stored mixture (which becomes even more effective in the upward direction). The gas that has passed through the phase-cycle to the gas phase can be sucked in again and the like.

In a suitable ejector of the present invention, it is particularly advantageous for the nozzle opening to produce a power jet having a liquid jet that enhances turbulence, since the power jet with enhanced turbulent flow is particularly effective in carrying gas away from the suction chamber (gas phase and liquid The interphase contact surface is increased), thereby creating enhanced suction and increasing the amount of gas inhaled per unit time, thereby improving the desired mixing. When the power jet is given a slight vortex motion before passing through the power nozzle, another improvement in the widening of the power jet from the power nozzle can be achieved. This can be achieved, for example, by installing a suitable vortex body (9) just upstream of the power nozzle. Such vortex bodies useful in the present invention are preferably, for example, blade rings as shown in Figure 3 of vt>>verfahrenstechnik<<15 (1981), No. 10, page 739. However, when a vortex body that imparts a jet of liquid through a large vortex (i.e., a superfluid turbulent flow force jet) is used, the pumping performance can also be impaired. In principle, the vortex can also be generated by a tangential power liquid supplied to the power nozzle.

Alternatively and/or additionally, for the vortex of the power jet, for example, since the outlet cross section of the power jet has a plurality of outlet holes (the cross section of the power nozzle is provided with a power jet splitter), it can be divided into Multiple separate jets). In the simplest form, this is achieved by incorporating a screen (plate) having a plurality of passage holes (in the simplest case annular) into the outlet cross section of the power jet, as for example by JH Witte. This is shown in Figure 2 on page 14 of the cited paper.

For example, the present invention also uses slotted nozzles (e.g., concentric annular gaps) in place of holes (in this case, screen or porous nozzles).

In view of the fact that in the present invention the mixing action in the ejector is achieved, in particular by spraying a gas into the stored liquid or a mixture of the stored liquid and the fine solid, the ejector (e.g., the spray nozzle) in the storage container does not need to be inclined upward. There is no need to raise the placement slightly. Instead, the injector can be mounted against the bottom of the storage tank. In addition, the power nozzles (in the ejector (and thus the ejector itself)) can be incorporated parallel to the bottom of the storage tank (ie, the standard level) without substantially losing mixing performance. As a result of horizontal inclusion, the phase interface (liquid interface) in the storage vessel can be reduced to a significantly lower level before the liquid is not adequately covered. In the case of further reducing the liquid interface below the diffuser of the horizontally mounted injector, the horizontal jet exiting the injector widens, especially in the case of its pre-formed vortex and/or split, and when it collides with the container wall with the spray nozzle A reduced amount of spray is produced. The design of the ejector used to mix the contents of the storage tank (which depends, for example, on the material data of the contents of the can and the geometry of the can) can be implemented in accordance with the discussion made in the cited documents. Useful manufacturing materials suitable for the properties of the liquid/mixture to be stored include stainless steel and plastics (e.g., fiber reinforced plastic substrates, as suggested in European Patent No. EP-A 245,844). When the contents are stored as acrolein, methacrolein, acrylic acid, methacrylic acid, an ester thereof or a solution thereof, the proposed ejector material is specifically stainless steel of DIN material numbers 1.4541 and 1.4547. In principle, the use of the injector of the invention is sufficient for the method of the invention. Suitably according to the invention, the ejector is placed in the container in such a way that the diffuser outlet is located in the middle of the container. It should be understood that a plurality of injectors can be operated simultaneously in the same container in accordance with the present invention. In this case, appropriately the injector of the same size should be used in accordance with the present invention. The injectors can in principle be arranged in the tank at any position relative to each other and, for example, form a star or star shape. Advantageously, the pump for delivering a power jet can be the same as the pump used to extract the liquid/mixture stored in the container (however, two pumps can be used for both purposes). In the case where the stored liquid comprises (meth)acrylic monomers (or other chemicals stored in liquid form), it is useful to have such a transport pumping system (for example) as suggested in WO 2004/003389 with a double slip ring seal. Transport the pump.

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The amount of gas inhaled from the gas phase per unit time by means of an ejector for use in the process of the invention (and with which mixing is achieved) can be enhanced according to the invention by the following (generally 2 to 3 times): the method of the invention The benefits of the ejector are at the beginning of the document (and, for example, also described in German Patent No. DE-A 24 04 289). The advantageous features of the injection nozzle are combined in a suitable manner to obtain a so-called injector nozzle as a present The injector is intended to be used in place of the injector, which is schematically illustrated in Figure 8 (the principle of the injector nozzle is described, for example, in Chemie-ing.-Techn. 47., 1975/第5) Page 209, Chemie-Ing.-Techn. MS201/75, Chemie-ing.-Techn. 61 (1989) No. 11 pp. 908-909, German patent DE-A 24 10 570 and German patents DE-A 15 57 018).

In terms of physical relationship, the reason is that the gas in the injector is only in contact with the power jet liquid, while additionally injecting a large amount of power jet from the surrounding liquid in the momentum exchange chamber of the injection nozzle. Expressed in its simplest form, the injector nozzle is simply a nozzle in which the power jet used is a mixture of the inhaled gas formed outside the power nozzle of the injector and the mixture of motive fluid pumped through the injector power nozzle.

For this purpose, the suction chamber of the injector component of the injector nozzle does not have a seamless transition to the mixing tube (mixing chamber) as in the case of only the injector. Rather, the suction chamber is here designed to provide a mixing nozzle (10) that is open to the mixing nozzle, a mixture of the motive fluid from the "injector" and the inhaled gas (eg, a jet of power in the case of a nozzle) From the mixing nozzle, it is injected into a momentum exchange tube (usually a momentum exchange chamber (open at the inlet and outlet)). In the injector nozzle, the suction chamber usually has a constant cross section first and then generally opens to the diffuser in the direction of flow (but not necessarily) (the diffuser has a widened cross section in the flow direction). Thus, the amount of liquid drawn in the transition environment of the mixing nozzle/momentum exchange tube from the storage tank per unit time is a multiple of the motive liquid pumped into the injector component per unit time (usually 1 or 2 to 10 times, usually 4 to 8 times).

Therefore, the amount of liquid (in always per unit time) entrained in the injector nozzle along the entire flow direction is significantly greater than in the case of a pure injector. This results in a significantly higher suction force and thus an enhanced mixing effect (for the purposes of the invention). In its simplest form, the separate liquid droplets in the mixing tube of the ejector deliver a continuous gas phase, while the liquid stream in the momentum exchange tube of the ejector nozzle delivers bubbles distributed therein.

In accordance with the present invention, advantageously, the power jet nozzle of the injector component of the injector nozzle also includes an element that widens and/or shunts the power jet exiting the power jet nozzle. As explained in detail in the description of the jet compressor, such useful elements are, for example, vortex bodies and/or perforated or slotted screens (power jet splitters). Another benefit of injector nozzles compared to pure jet compressors is the appearance of a finer gas distribution that also has a beneficial effect on the desired mixing. In summary, in the injector nozzle, the inhaled gas in the injector component is directed into the mixing nozzle together with the inhaled power jet and the materials are mixed therein. The kinetic liquid-gas mixture thus obtained is introduced (sprayed) into a momentum exchange chamber (at its narrowest cross section), the momentum exchange chamber being arranged in the stored liquid medium along the kinetic liquid-gas mixture The direction extends and is very small compared to the volume of the container (typically, the volume of the momentum exchange chamber is one to one hundredth of a million or one part per million of the maximum liquid capacity of the container). At the same time, (in this document a jet that exits (flows out) through the center of the narrowest cross-sectional area of the mixing nozzle in the absence of the stored liquid medium (and is directed into the momentum exchange chamber) is referred to as a self-mixing nozzle leading to momentum The central jet of the exchange chamber (see (11) in Fig. 15) draws in the stored liquid medium from the environment when the motive liquid-gas mixture flowing from the mixing nozzle enters the momentum exchange chamber. Due to the relatively narrow cross section of the momentum exchange tube ( Into the momentum exchange chamber), the "second" liquid flow drawn in is greatly accelerated. As a result, a static pressure is reduced in the injector component that is reduced to the gas suction pressure. At the same time, the liquid is drawn in the second portion after entering the momentum exchange chamber. The kinetic liquid-gas mixture is highly intensively mixed. This results in a sudden change in the dispersed phase such that the gas is entrained in the form of bubbles that are finely distributed in the liquid.

The design of the injector nozzle for a particular mixing problem can be implemented with reference to the documents cited in this document as well as the injector nozzles (the useful materials of construction are those described for the injectors).

The speed of the motive liquid after leaving the mixing nozzle is typically from 10 to 100 meters per second, preferably from 15 to 70 or to 30 meters per second. The average diameter of the inlet holes of the momentum exchange chamber is usually 1.1 to 4 times, preferably 1.2 to 2 times the average diameter of the mixing nozzle, and the length of the momentum exchange chamber is usually 3 to 30 times the hydraulic diameter thereof, preferably 3 Up to 10 times.

Leaving the mass flow rate of the momentum exchange chamber typically has a ¹⁰³ to ¹⁰⁵ N / m ^2, an average momentum density is preferably ^{from 3} to 2.10 ⁴ 5.10 N / m ² of. In contrast, the method of the present invention, the average momentum of the motive jet line density is typically ^4-10 2.5.10 ⁷ Newtons / m ^2, from 10 ⁵ to 5.10 ⁶ N / m ^2.

It should be understood that the average diameter refers to the diameter of the circle having the same surface area as the cross section of the nozzle or the momentum exchange chamber inlet aperture (which may also be a polygonal shape), and the cross section of the nozzle or inlet aperture need not be rounded. The momentum exchange chamber typically has a constant cross section, while the diffuser typically has a cross section that expands in the direction of flow. In principle, the momentum exchange chamber can be constructed in a variety of forms, which is preferably adapted to the form of a mixing nozzle.

In general, the momentum exchange chamber used is typically a cylindrical tube and the diffuser is a cone. When the momentum exchange chamber is constructed as a cylindrical tube, its length is usually 3 to 30 times, preferably 3 to 10 times its diameter, in which case its diameter is simultaneously the hydraulic diameter thereof. When the momentum exchange chamber does not have a circular cross section or a constant cross section over its length, its length is usually 2 to 30 times, preferably 3 to 10 times its hydraulic diameter. It should be understood that the hydraulic diameter means the diameter of a cylindrical tube that exhibits the same pressure drop as the momentum exchange chamber at the same throughput and the same length.

In a suitable injector nozzle of the present invention, suitably from the application point of view, the narrowest cross-sectional area of the mixing nozzle is located between 1 and 10 times the narrowest hydraulic diameter of the mixing nozzle from the power nozzle of the injector component.

Further, suitably in accordance with the present invention, the narrowest cross-sectional area of the mixing nozzle in the injector nozzle of the present invention extends into the momentum exchange chamber (usually at the center) to a degree no greater than the narrowest hydraulic diameter of the power nozzle. 0 to 3 or 2 times deeper.

Suitably according to the invention, the mixing nozzle extends into the momentum exchange chamber. In principle, the narrowest cross-sectional area of the mixing nozzle can also have a distance to the momentum exchange chamber which can be, for example, up to 1 or several times the narrowest hydraulic diameter of the power nozzle.

Further, suitably from the application point of view, the narrowest cross-sectional area of the mixing nozzle suitable for the injector nozzle of the present invention is 1.5 to 15 times, preferably 2 to 10 times the cross-sectional area of the narrowest power nozzle. The speed of the power jet exiting the power nozzle in the injector component is typically 20 to 50 meters per second in a manner suitable for the injector nozzle of the present invention.

The discussion herein regarding the possible dimensions of the injector components of the injector nozzles also applies to individual injectors.

The method of the present invention can also use a plurality (one bundle) of injector nozzles in place of only one injector nozzle in the same storage container as described in the context of using a pure injector. As in the case of an ejector, the present invention suitably positions the injector nozzle (or ejector) vertically downwardly in the middle of the container (especially avoiding deposits of fine solids in the mixture to be stored in the present invention). In the case of an injector nozzle, the invention may also combine a plurality of injector components including their mixing nozzles with a combined momentum exchange chamber, in which case the inlet cross-section should be equal to that in its individual use. The sum of the cross sections required for a particular mixing nozzle.

In principle, the momentum exchange chamber and the injector components of the injector nozzle (also including the mixing nozzle) can be connected via a connecting element (preferably via three connecting elements (which can be placed completely satisfactorily in the center), in each case Both are connected to each other around 120°). However, these can also be screwed into each other. In this case, the installed slots are suitably permitted to draw in the surrounding liquid.

Typically, where the method of the invention is carried out with an ejector nozzle, the ratio of the total liquid volume delivered to the momentum exchange chamber to the volume of gas supplied may be between 0.1 and 10.

The momentum exchange in the momentum exchange chamber and the conversion of kinetic energy to pressure energy in the diffuser create static pressure buildup in the injector nozzle. This compression operation occurs because a large amount of liquid has better performance than an injector. Another advantage is that the central wall friction is due to the momentum exchange chamber (which typically has a larger diameter than the mixing chamber of a conventional injector), and the flow loss is less due to the lower flow rate under other identical conditions.

Figure 9 is a schematic illustration of an embodiment of the initial gas-initiated mixing of the present invention of a canister filled with a mixture of liquid or liquid and fine solids and using a preferred injector spray nozzle as the suction device. According to Figure 10, the possibility of horizontally installing the injector nozzles reduces the liquid interface (phase interface) to a relatively low level before the liquid is sufficiently covered. In the case where the liquid interface (phase interface) is further lowered below the nozzle, no other liquid is inhaled. However, when the horizontally exiting jet collides with the vessel wall (especially in the case of an additional vortex body upstream of the power nozzle in the injector component) (Fig. 11), it no longer produces a large amount of spray because it cannot be used as a beam jet. Reach the container wall.

In a particularly preferred embodiment of the invention, the suction device according to the method of the invention according to Fig. 12 can also be an injector nozzle, wherein the suction region between the mixing nozzle and the momentum exchange chamber (momentum exchange tube) The surrounding liquid is provided with a sleeve having at least one hole (at least one inlet hole (at least one suction hole)), wherein the restriction is that the at least one hole is below the central jet exiting the mixing nozzle into the momentum exchange chamber (here, Below it means going down the jet from the center in the direction of the bottom of the container or tank). The at least one access opening is preferably designed as a immersion tube (opening outward) towards the bottom of the container and thus arranged close to the bottom of the container (this can result in extremely fast mixing due to suction from below). In principle, the cross section of the immersion tube can be circular, elliptical or polygonal as desired. Typically, the cross section of the immersion tube in the method of the invention is constant over its length. The immersion tube having a circular cross section of the present invention is preferred. The average diameter of the at least one suction orifice below the central jet leading away from the mixing nozzle to the momentum exchange chamber is typically from 1 to 20 times, preferably from 2 to 10 times the average diameter of the mixing nozzle. Typically, the immersion tube is constructed in such a way as to produce a minimum pressure drop through the flow therethrough. In principle, the at least one suction opening can also be designed as a hole and/or a slot distributed in the wall along the length of the immersion tube. The immersion tube can also be bent upwards like a meat hook when its end is placed close to the bottom so that the suction hole does not point to the bottom of the container but to the top (cover) of the container. The bend can also be designed to be as open as a golf club and open outwardly with a suction aperture parallel to the bottom of the container. Further, the immersion tube including the suction hole can be extended into the kettle, and the top of the kettle is opened and rested on the bottom of the container. It is also advantageous if the suction opening of the immersion tube and the outlet exiting the momentum exchange chamber (tube) can be positioned independently of one another in a spatial relationship (for example at a maximum distance from each other) (not necessarily associated with one another in their spatial position). Even in the case of very low fill levels in the storage container, use a immersion tube (which can be welded seamlessly to the sleeve, or screwed into the sleeve, or joined to a suitable connection placed in the sleeve (eg flanged to The embodiment of the connection to the short tube)) still leaves substantially no substantial damage to the performance of the method of the invention. In the worst case, this problem occurs when the delivery pump is temporarily cut off. In this case, the immersion tube no longer fills the mixing nozzle with the stored liquid or the mixture of the stored liquid and the fine solid, but fills the gas. However, in the case of an injector component of the injector nozzle, the power jet of the power nozzle is sufficiently vortexed and/or shunted (eg, by means of a tangential feed of the vortex body and/or the power jet splitter and/or the power jet) The suction force generated after restarting is sufficient to immediately raise the liquid or mixture level in the immersion tube to the desired level and to continue the procedure of the present invention.

The volume of the gas phase in the vessel in the process of the invention should be at least 5% by volume or at least 10% by volume of the volume of liquid or mixture stored in the vessel. However, based on the same standard, it may also be 30% by volume, 60% by volume, 90% by volume, 150% by volume, 250% by volume, 350% by volume, and higher.

In addition, when the liquid contents per minute per liter of storage container in the method of the present invention are injected with at least about 10 ^-5 standard liters (gas volume expressed in units of liters at 0 ° C and 1 atm) (but usually no more than 1 × 10 ^- The invention is also advantageous when ¹ standard liter).

The container itself preferably has a cylindrical (e.g., having a circular or square or rectangular cross-section) structure that terminates at the top with a conical top or a hemispherical or domed top.

The process of the invention is particularly suitable for the storage of all of the liquids described at the beginning of the document (but may also be, for example, benzene, toluene, alcohols, other hydrocarbons) or mixtures of liquids and fine solids. These are typically transported by a gas that is saturated with the liquid vapor (i.e., the gas phase typically consists not only of the evaporated liquid).

Useful Such gases include (e.g.) an inert gas (e.g. N _2), rare gas (e.g., Ar) and / or CO _2.

We should be aware that these gases may also be air or other mixtures of molecular oxygen and inert gases. The absolute pressure in the tank can be, for example, from atmospheric to 50 bar; the temperature in the tank can be, for example, 0 (or lower) to 100 (or higher) °C.

The above two parameters are not subject to any limitation in the method of the present invention.

When the stored liquid system is at least one monoethylenically unsaturated organic compound (for example, N-vinylformamide, vinyl acetate, maleic acid ester, styrene, and/or N substituted acrylamide) or includes at least The process of the invention is particularly advantageous when it is a solution of a monoethylenically unsaturated organic compound, especially when it comprises an additional polymerization inhibitor for the purpose of inhibiting unwanted free radical polymerization.

Other examples of such at least monoethylenically unsaturated organic compounds include acrolein, methacrolein, acrylic acid, methacrylic acid, and an ester of acrylic acid and/or methacrylic acid with a mono- or polyhydric alkanol. The esters specifically include those in which the alcohol has 1 to 20 carbon atoms or 1 to 12 carbon atoms or 1 to 8 carbon atoms. Illustrative representatives of such esters include methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, t-butyl acrylate, 2-ethylhexyl acrylate, hydroxyethyl acrylate, hydroxy acrylate Propyl ester, hydroxyethyl methacrylate, hydroxypropyl methacrylate, methyl methacrylate, ethyl methacrylate, n-butyl methacrylate and t-butyl methacrylate. Useful inhibitors for free radical polymerization of the above monomers and their solutions in organic or aqueous solvents are, for example, hydroquinone monomethyl ether (MEHQ), hydroquinone, phenol (eg, 2, 4-Dimethyl-6,6-butylphenol), hydrazine, butyl catechol, phenothiazine, diphenylamine, p-phenylenediamine, nitrodecyl and/or nitroso compounds (eg nitro Phenol) (and may also be all other polymerization inhibitors described in WO 00/64947). The amount of polymerization inhibitor added for storage purposes may be from 0.5 to 1000 ppm by weight (usually from 1 to 600 ppm by weight or from 2 to 500 ppm by weight) based on the monomer content. .

Acrylic acid in ice In the case of 99.5 wt%), 200 ± 20 ppm by weight of MEHQ is usually added as a storage inhibitor (storage temperature recommendation: 15 to 25 ° C). In n-butyl acrylate (n-butyl acrylate content) In the case of 99.5 wt%) and other (meth) acrylates, 15 ± 5 ppm by weight of MEHQ is usually added as a storage stabilizer (storage temperature recommendation: 20 to 35 ° C). MEHQ is also a preferred storage stabilizer for other (meth)acrylic monomers and solutions thereof.

As already mentioned above, the above polymerization inhibitors (especially MEHQ) generally exhibit their full inhibition only in the presence of molecular oxygen. However, especially (meth)acrylic monomers and molecular oxygen can form explosive mixtures.

Even in the case of spraying (spray formation) in order to eliminate the corresponding explosion in the storage tank, it is necessary to periodically prevent this spray formation or correspondingly limit the oxygen in the gas phase of the storage tank by means of liquid level control which can be widely adopted from a safety technical point of view. The content is as suggested in the context of U.S. Patent No. 6,910,511 to WO 2005/049543.

In contrast, the use of the inventive procedure (even if the liquid level in the container is relatively low, by which the spray formation can be prevented) makes it relatively simple and reliable to cover the contents of the can with air saturated with the liquid stored in the can. However, when the stored acrylic acid (aluminum stored) is obtained by heterogeneously catalyzing partial gas phase oxidation of propylene in the presence of propane or acrylic acid (acrolein) obtained by heterogeneously catalyzed partial gas phase oxidation of propane itself, After the acrylic acid (to store crude acrolein) is separated from the product gas mixture, it is usually obtained in a form saturated with propane. In this case, the gas mixture additionally comprises combustible propane. For safe storage, in this case it is desirable to meet the lower limit of the limiting oxygen concentration in accordance with WO 2005/049543 in a gas-lean storage system.

In principle, as the fill level in the storage vessel continues to decrease, the feed (circulation) rate at which the power jet is formed can be reduced in the process of the invention.

In general, it is very simple to introduce molecular oxygen into the liquid to be stored or to introduce the mixture to be stored in the process of the invention.

Especially for this reason, the process according to the invention is particularly suitable for storage tanks containing a particularly large amount of can contents.

Thus, the present application specifically includes the following embodiments of the invention:

Example:

CLAIMS 1. A method of mixing a liquid or a mixture of liquids and fine solids present in a substantially self-contained container, wherein the restriction is that the liquid or mixture only fills the fluid phase can occupy a portion of the internal volume of the container, and the remainder of the container The occupied internal volume is filled by the gas phase, the method comprising supplying substantially the same liquid or substantially the same mixture into the container as a power jet of the suction device arranged in the liquid or in the mixture in the container, by means of which the jet The suction device draws in gas from the gas phase present in the container and releases the inhaled gas along with the power jet to the liquid or mixture present in the container.

2. The method of embodiment 1, wherein the suction device comprises at least one injector having a power nozzle and a suction chamber, the suction chamber being connected to the gas phase (via the gas that can be drawn from the gas phase by the gas chamber) Connected) and delivers a power jet via its power nozzle.

3. The method of embodiment 2 wherein the power jet is imparted with a vortex motion prior to passing through the power nozzle.

4. The method of embodiment 3 wherein the vortex motion is imparted by a vortex body disposed upstream of the power nozzle.

5. The method of embodiment 3 wherein the vortex motion is imparted by tangentially supplying a motive liquid to the power nozzle.

6. The method of any one of embodiments 1 to 5 wherein the power jet is shunted as it passes through the power nozzle.

7. The method of embodiment 6, wherein the powered nozzle is a screen nozzle or a slot nozzle.

8. The method of embodiment 1, wherein the suction device comprises at least one injector nozzle having a power nozzle, a suction chamber surrounding the power nozzle and open to the mixing nozzle, and the mixing nozzle outlet facing a momentum exchange chamber, the suction chamber is connected to the gas phase (via a connection from which gas can be drawn from the gas phase), and the power jet (which is a mixture containing the sucked gas) passes through the power nozzle through the mixing nozzle Transfer to the momentum exchange chamber.

9. The method of embodiment 8 wherein the power jet is imparted with a vortex motion prior to passing through the power nozzle.

10. The method of embodiment 9, wherein the vortex motion is imparted by a vortex body disposed upstream of the power nozzle.

11. The method of embodiment 9, wherein the vortex motion is imparted by tangentially supplying the motive liquid to the power nozzle.

The method of any one of embodiments 8 to 11 wherein the power jet is shunted as it passes through the power nozzle.

13. The method of embodiment 12 wherein the powered nozzle is a screen nozzle or a slot nozzle.

The method of any one of embodiments 1 to 7, wherein the ejector is horizontally mounted in the container.

The method of any one of embodiments 8 to 13 wherein the injector nozzle is mounted horizontally in the container.

The method of any one of embodiments 8 to 13 and 15, wherein the transition from the mixing nozzle to the momentum exchange chamber is provided with a sleeve having at least one hole, wherein the limiting condition is that the at least one hole is located in the self-mixing The nozzle is introduced below the central jet (11) of the momentum exchange chamber.

The method of any one of embodiments 8 to 13 and 15, wherein the transition from the mixing nozzle to the momentum exchange chamber is provided with a sleeve having at least one opening that opens to the immersion tube leading to the bottom of the container .

The method of any one of embodiments 1 to 17, wherein the liquid comprises at least one organic compound from the group consisting of acrolein, methacrolein, acrylic acid, methacrylic acid, esters of acrylic acid, and An ester of acrylic acid.

The method of any one of embodiments 1 to 17, wherein the liquid comprises N-vinylformamide.

20. The method of embodiment 18 or 19, wherein the liquid comprises at least one dissolved polymerization inhibitor.

The method of any one of embodiments 1 to 20, wherein the gas phase comprises molecular oxygen.

The method of any one of embodiments 1 to 21, wherein the gas phase volume in the vessel is at least 5% by volume of the volume of the liquid or mixture stored in the vessel.

23. The method of any one of embodiments 1 to 22, wherein at least 10 ^-5 standard liters of gas per minute per liter of the liquid or mixture of liquid and fine solids present in the vessel is withdrawn from the gas phase and released to Present in the liquid or mixture in the container.

The method of any one of embodiments 1 to 23, wherein the liquid or mixture fed as a power jet into the container comprises a portion of the liquid or mixture that has been previously withdrawn from the container in the container or All.

The method of any one of embodiments 1 to 23, wherein the liquid or mixture fed as a power jet into the container does not include a portion of the liquid or mixture present in the container that has been previously withdrawn from the container.

The method of any one of embodiments 1 to 25, wherein the liquid or mixture fed to the vessel as a power jet has been previously passed through a heat exchanger for delivery.

27. A container further comprising a gas phase, a liquid or a mixture of liquid and fine solids, and also comprising at least one injector comprising a power jet and a gas phase (which is capable of drawing gas from the gas phase) Suction chamber.

28. A container further comprising a gas phase, a liquid or a mixture of liquid and fine solids and also comprising at least one injector nozzle and a connection to the gas phase from which gas can be drawn from the gas phase, the injector nozzle having A power nozzle, a suction chamber surrounding the power nozzle and open to the mixing nozzle, and a momentum exchange chamber toward the mixing nozzle outlet.

29. Use of an ejector for gas-induced mixing of a liquid or a mixture of liquid and fine solids in a substantially self-contained container, wherein the restriction is that the liquid or mixture only fills the fluid phase can occupy a portion of the internal volume of the container, And the rest of the container can occupy the internal volume and is filled by the gas phase.

30. Use of an ejector nozzle for gas-induced mixing of a liquid or a mixture of liquid and fine solids in a substantially self-contained container, wherein the restriction is that the liquid or mixture only fills the fluid phase and can occupy the internal volume of the container Part of it, and the rest of the container can occupy the internal volume filled by the gas phase.

31. An injector nozzle having a power nozzle, a suction chamber surrounding the power nozzle and open to the mixing nozzle, and a pulsation exchange chamber to which the mixing nozzle outlet is directed, wherein a transition from the mixing nozzle to the pulsation exchange chamber There is a sleeve and the sleeve has at least one connection for the immersion tube or at least one immersion tube for introduction into the sleeve.

The process of the invention is also suitable for intimately mixing another liquid or another mixture into a liquid or a mixture of liquid and fine solids present in a substantially self-contained container, wherein the limiting condition is that the liquid or mixture is only filled with a fluid phase A portion of the internal volume of the container is occupied and the remaining internal volume of the container is filled with the vapor phase (and the specified fill level in the container is also not considered). In this case, the procedure carried out in the simplest manner is intended to be a mixture of the power jet supply of the present invention or other liquid or other mixture to which the liquid is completely mixed. Properly according to the present application, in order to further promote the formation of a homogeneous mixture in the container after the supply of other liquids or other mixtures, the liquid or mixture present in the container at this time is then totaled by means of, for example, a pump for container withdrawal. A portion of the quantity is withdrawn from the container and at least some of the extracted portion, if appropriate after it is directed through the heat exchanger, as a suction device for use in a liquid or mixture present in the container and used in accordance with the present invention The power jet is recirculated into the container.

Alternatively, the procedure may be preceded by the use of other liquids or other mixtures with a mixture of liquids or mixtures in which a portion of the liquid or mixture has been pre-extracted as the power jet of the suction device to be used in the present invention. Properly according to the present application, after the total amount of other liquids or other mixtures to be supplied is supplied, in order to further promote the formation of a homogeneous mixture in the container, then the pump, for example for the extraction of the container, will then be present at this time. A portion of the total amount of liquid or mixture in the container is withdrawn from the container and at least some of the extracted portion, if appropriate after it is directed through the heat exchanger, is present in the liquid or mixture present in the container and according to the present The power jet of the suction device used in the invention is recirculated into the container.

If appropriate, after the total amount of other liquids or other mixtures supplied is supplied, it is also possible to promote the formation of a homogeneous mixture in the container by supplying substantially the same liquid or mixture as a power jet without previously withdrawing it from the container. .

a liquid which is present in the container or a mixture system present in the container, which comprises at least one compound having at least one ethylenically unsaturated moiety (for example, acrolein, methacrolein, acrylic acid, methacrylic acid, acrylic acid ester) And/or the liquid or mixture of methacrylic acid esters (usually in the form of being stabilized by the addition of a polymerization inhibitor), undesired radical polymerization for various reasons. In order to make it extremely fast to terminate before this radical polymerization is expected to become more pronounced, it is proposed in the prior art to mix the high concentration radical polymerization inhibitor solution substantially immediately (see WO 00/64947, WO 99/21893, WO 99/). 24161, WO 99/59717).

Such solutions may, for example, be liquids to be incorporated in the present invention as described above. In particular, such "short-term termination solutions" may include inhibitor solutions of at least 10% by weight of phenothiazine, 5 to 10% by weight of p-methoxyphenol and at least 50% by weight of N-methylpyrrolidone. .

Alternatively, use all other "short-term termination solutions" as suggested in the above WO document.

Accordingly, the present patent application additionally includes the following examples of the invention: 32. A method of mixing another liquid or another mixture into a liquid or liquid and a mixture of fine solids present in a substantially self-contained container, wherein The limitation is that the liquid or mixture only fills the fluid phase can occupy a portion of the internal volume of the container and the remaining internal volume of the container can be filled by the gas phase, the method comprising treating other liquids or other mixtures as liquids or mixtures present in the container a power jet of the suction device is supplied to the container, wherein the suction device releases the gas from the gas phase present in the container by means of the power jet and releases the inhaled gas together with the power jet to the container In a liquid or mixture.

33. The method of embodiment 32, wherein the liquid present in the container comprises a compound having at least one ethylenically unsaturated moiety, and the other liquid system inhibitor solution supplied as a power jet, the inhibitor solution comprising at least 10% by weight Phthathiazine, 5 to 10% by weight of p-methoxyphenol and at least 50% by weight of N-methylpyrrolidone.

Working example

According to Figure 13 (cylindrical footprint, diameter 8.5 m and height 10 m up to the beginning of the conical top) in an outdoor tank (wall thickness: 5 mm, material of manufacture: DIN 1.4541) stainless steel, at a desired internal temperature of 20 ° C Store 200 ppm (by weight) MEHQ stabilized glacial acrylic acid (GAA) under normal pressure and maximum fill height. The maximum filling height in the storage tank is 9 meters. The remaining gas volume is 69 ^m3 at the maximum fill height.

The tank withdrawal was carried out by means of a CPK 50-200 centrifugal pump from KSB Aktiengesellschaft in D-67227 Frankenthal.

A mixture of ethylene glycol and water present in a barrier flow system in a pump with a double slip ring seal. The ice acrylic in the storage tank is covered by air. By means of an exhaust system (conical top hole cross section = 20 cm ² ) which is open to the atmosphere via a burner, gas can be released from the gas phase of the tank to the burner for pressure release during filling.

In a corresponding manner, air is replenished via pressure holding means for pressure equalization during the withdrawal of glacial acrylic acid from the tank. As can be seen in Figure 13, near the bottom, the injector nozzle of Figure 14 (made of DIN-1.4541 stainless steel) is mounted horizontally with its diffuser extending into the middle of the can. The dimension in Figure 14 is the attached dimension (nominal width) in millimeters and the angle in degrees (NW represents the nominal width). The wall thickness is 1 to 6 mm. Figure 15 additionally shows the vortex body disposed upstream of the power nozzle of the injector component from the side and front side with a vortex angle of 30°. Figure 14 also shows the connection (12) of the riser tube extending into the gas phase of the canister to the suction chamber of the injector component of the injector nozzle.

A centrifugal pump was used to continuously draw 40 m ³ /hr of glacial acrylic acid from the tank over a period of 1 week, and was circulated as a power jet into the injector nozzle via the heat exchanger of FIG. Regardless of the external temperature (which varies over a range of ±15° during the experiment), the temperature was kept constant at 20 ± 1 °C at the withdrawal point of the storage tank.

Finally, 1 liter of a solution of 0.1% by weight of phenothiazine in glacial acrylic acid was introduced into the tank at one time from the top (at the maximum filling height). After 5 minutes, the equally distributed concentration of the added phenothiazine was within about ±10% of its theoretical value at the point of withdrawal.

Subsequently, the circulation rate was maintained, but the extraction rate was increased to 20 m ³ /hr, that is, the can was emptied at 20 m ³ /hr. 99% of its liquid contents can be withdrawn from the tank without any problem without forming a spray in the tank (in principle, glacial acrylic acid can also be withdrawn from the tank without being directed through the outlet of the circulation pump) .

Figure 16 additionally shows a three-dimensional view of the vortex body used.

For purposes of illustration, Figure 17 shows a three-dimensional view (cross-section) of the injector nozzle, and Figure 18 shows a corresponding exploded view.

In addition, the abbreviations in Figure 13 indicate: TIA ⁺ means "temperature indicator alarm"; LIS means "liquid level indicator switch"; if overfill protection (+) and if not filled with protection (-); TIS ⁺ means "temperature Indicator safety"; FIS means "flow indicator safety"; F means "flow" (small safety flow is protected as a pump).

In addition, Figure 13 shows the two-way shut-off valve on the top of the vessel and a single-acting (open only) shut-off valve at the far end of the pump but withdrawn upstream.

U.S. Provisional Patent Application Serial No. 60/846,095, filed on Sep. 21, 2006, is incorporated herein by reference. Many modifications and variations of the present invention are possible in light of the above teachings. Therefore, the invention may be practiced otherwise than as specifically described herein within the scope of the appended claims.

0. . . Entry point

1. . . Power nozzle

2. . . Mixing room

3. . . Entrance cross section

4. . . Suction chamber

5. . . Enter the entrance of the mixing chamber (mixing tube)

6. . . Mixing tube (mixing chamber)

7. . . Diffuser

8. . . Suction chamber inlet

9. . . Whirlpool

10. . . Mixing nozzle

11. . . Central jet

12. . . connection

Figure 1 shows a prior art method in which the liquid contents of the can are mixed by, for example, bubbling or spraying a suitable gas against the bottom into the can.

Figure 2 shows another prior art method in which the mixing action of the free jet affects only a relatively limited space around it.

Figure 3 shows a further prior art method in which the mixing chamber (2) is arranged outside the power nozzle (1).

4 shows an embodiment of the invention in which the mixture enters only at relatively low levels of the phase interface and at a reduced average exit momentum density.

Figure 5 shows an embodiment of the invention wherein the effluent flowing upwardly out of the momentum exchange tube forms a large volume circulating flow field represented by a continuous field line.

Figure 6 shows an embodiment of the invention in which the power jet passes through the momentum exchange tube unimpeded and sprays to form fine droplets when the fill level falls below the pumping level.

Figure 7 shows the basic structure of the injector.

Figure 8 shows an injector spray nozzle to be used as a suction device of the present invention as an ejector substitute.

Figure 9 shows a schematic of an embodiment of the initial gas-initiated mixing of the present invention of a canister filled with a liquid or a mixture of liquid and fine solids and using a preferred injector spray nozzle as the suction device.

Figure 10 shows an embodiment of the invention in which the possibility of horizontally installing the injector nozzles allows the liquid interface to be lowered to a relatively low level before the liquid is insufficiently covered.

Figure 11 shows an embodiment of the invention in which no more large amounts of spray are produced when a horizontally exiting jet collides with the vessel wall.

Figure 12 shows a suction device for use in the method of the invention.

Figure 13 shows an embodiment of the invention in which an outdoor can is used and the injector nozzle is mounted horizontally with its diffuser extending approximately midway into the can.

Figure 14 shows an injector nozzle for use in the present invention and its dimensions.

Figure 15 shows an embodiment of the invention in which the vortex body disposed upstream of the power nozzle of the injector component is shown from the side and the front side with a vortex angle of 30°.

Figure 16 shows a three-dimensional view of a vortex body for use in the present invention.

Figure 17 shows a three-dimensional view of an injector nozzle for use in the present invention.

Figure 18 shows a corresponding exploded view of Figure 17.

(no component symbol description)

Claims (28)

A method of mixing a liquid or a mixture of liquids and fine solids present in a substantially self-contained container, the restriction being that the liquid or mixture is only filled with a portion of the internal volume of the container that the fluid phase can occupy, and the remainder of the container can be occupied The internal volume is filled by a gas phase, the method comprising supplying a substantially identical liquid or a substantially identical mixture to the vessel as a power jet of a suction device disposed in the liquid or mixture in the vessel, wherein the suction device The power jet draws in gas from a gas phase present in the vessel and releases the inhaled gas along with the power jet to a liquid or mixture present in the vessel, the restriction being when aspirating from the gas phase and After the power jet is released into the liquid or mixture present in the container, the gas is bubbled through the stored liquid or mixture, the gas A chemical change occurred at 1% by volume. The method of claim 1, wherein the suction device comprises at least one injector having a power nozzle and a suction chamber connected to the gas phase and transmitting a power jet via its power nozzle. The method of claim 2, wherein the power jet is imparted with a vortex motion prior to passing through the power nozzle. The method of claim 3, wherein the vortex motion is imparted by a vortex body mounted upstream of the power nozzle. The method of claim 3, wherein the vortex motion is imparted by tangentially supplying the motive liquid to the power nozzle. The method of any one of clauses 1 to 5, wherein the power jet is shunted as it passes through the power nozzle. The method of claim 6, wherein the power nozzle is a screen nozzle or a slot nozzle. The method of claim 1, wherein the suction device comprises at least one injector nozzle having a power nozzle, a suction chamber surrounding the power nozzle and opening to a mixing nozzle, and a mixing The nozzle outlet faces a momentum exchange chamber therein, the suction chamber being connected to the gas phase and the power jet being transmitted through its mixing nozzle to the momentum exchange chamber via its power nozzle. The method of claim 8, wherein the power jet is imparted with a vortex motion prior to passing through the power nozzle. The method of claim 9, wherein the vortex motion is imparted by a vortex body mounted upstream of the power nozzle. The method of claim 9, wherein the vortex motion is imparted by tangentially supplying the motive liquid to the power nozzle. The method of any one of clauses 8 to 11, wherein the power jet is shunted as it passes through the power nozzle. The method of claim 12, wherein the power nozzle is a screen nozzle or a slot nozzle. The method of any of claims 1 to 5, wherein the injector is mounted horizontally into the container. The method of any one of clauses 8 to 11, wherein the injector nozzle is mounted horizontally into the container. The method of any one of claims 8 to 11, wherein a transition from the mixing nozzle to the momentum exchange chamber is provided with a sleeve having at least one hole, the limit The condition is that the at least one hole is located below the central jet exiting the mixing nozzle into the momentum exchange chamber. The method of any one of claims 8 to 11, wherein the transition from the mixing nozzle to the momentum exchange chamber is provided with a sleeve having at least one opening that opens toward one of the immersion tubes leading to the bottom of the container. The method of any one of claims 1 to 5, wherein the liquid comprises at least one organic compound from the group consisting of acrolein, methacrolein, acrylic acid, methacrylic acid, an acrylic acid ester, and methacrylic acid. ester. The method of any one of claims 1 to 5, wherein the liquid comprises N-vinylformamide. The method of claim 18, wherein the liquid comprises at least one dissolved polymerization inhibitor. The method of any one of claims 1 to 5, wherein the gas phase comprises molecular oxygen. The method of any one of claims 1 to 5, wherein the volume of the gas phase in the vessel is at least 5% by volume of the volume of the liquid or mixture stored in the vessel. The method of any one of claims 1 to 5, wherein at least 10 ^-5 standard liters of gas per minute per liter of liquid or liquid and a mixture of fine solids present in the container are withdrawn from the gas phase and released to the presence In a liquid or mixture in the container. The method of any one of claims 1 to 5, wherein the liquid or mixture fed as a power jet into the container comprises a portion or all of the portion of the liquid or mixture present in the container that has been previously withdrawn from the container. The method of any one of claims 1 to 5, wherein the liquid or mixture fed as a power jet into the container does not include a portion of the liquid or mixture present in the container that has been previously withdrawn from the container. The method of any one of claims 1 to 5, wherein the liquid or mixture fed as a power jet into the vessel is pre-guided through a heat exchanger. A method of mixing another liquid or another mixture into a liquid or liquid and a mixture of fine solids present in a substantially self-contained container, the limitation being that the liquid or mixture is only filled with the internal volume of the container that the fluid phase can occupy a portion of the container and the remaining internal volume of the container being filled by the gas phase, the method comprising supplying the other liquid or other mixture to the container as a power jet of a suction device present in or in the liquid in the container Wherein the suction device draws in gas from the gas phase present in the container by means of the power jet and releases the inhaled gas together with the power jet into a liquid or mixture present in the container, the limiting condition being a gas that is aspirated from the gas phase and released into the liquid or mixture present in the vessel together with the power jet through the stored liquid or mixture A chemical change occurred at 1% by volume. The method of claim 27, wherein the liquid present in the container comprises a compound having at least one ethylenically unsaturated moiety, and the other liquid system-inhibitor solution supplied as a power jet, the inhibitor solution comprising at least 10% by weight Phthathiazine, 5 to 10% by weight of p-methoxyphenol and at least 50% by weight of N-methylpyrrolidone.