DD210299A5 - METHOD AND DEVICE FOR CONTINUOUS MANUFACTURE OF LUBRICANT - Google Patents

Abstract

The invention relates to a continuous process for the production of lubricating grease and to an apparatus for carrying out this process. The process according to the invention comprises, as usual, the steps of saponification, removal of the water and / or of the solvent, dispersion under heat treatment and homogenization and cooling. For the invention is characterized in that these steps are carried out in so-called. Static mixing units. Neither these static mixing units nor their elements perform mechanical movements during the operation of the device. The mixing and dispersing effect as well as the homogenization come about exclusively by the fact that the mixture - in whole or in partial flows - past static mixing elements with different, Tutbulenz causing speed by alternately narrowing or further rooms stroemen, contacted each other, etc.

Description

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Process and apparatus for the continuous production of lubricating grease

Field of application of the invention:

The invention relates to a method and an apparatus for the continuous production of lubricating grease.

Characteristic of the known technical solutions:

It is known that the processes for producing grease differ from one another depending on the type of gel-forming component used, but essentially from the saponification, from the dehydration of the water formed during the saponification or introduced into the mixture and / or solvent content or Desolvation of the latter, dispersing the soap melt and cooling and homogenizing the mixture.

The saponification includes, as far as the operations are concerned, the mixing of the components and the heat input required to accelerate the reaction. This step is omitted if prepared, preformed soaps or other gelling agents are used.

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ΠΚΤ1333 * 1ί> 2343

The dispersing is partly parallel with the saponification, since the latter is carried out in most of the known formulations in a mineral oil as a medium. The dispersion can be improved by stirring, heating and by taking advantage of shear forces.

The formed in the saponification or introduced into the system water and solvent is removed by dehydration or desolvation. In modern continuous processes, this is usually done in paddles equipped with paddles. By appropriate design of the rotor of Rotationsfilmeindampfer can be achieved that comes to be heated or to be liberated from water and solvent material as a very thin film in very strong turbulence with the heat transfer surface for only a very short time in touch. In the case of highly viscous and non-Newtonian liquids, local overheating which damages damaging the front wave can practically not occur. It can not cause deposits or caking on the wall; come, there * as a result of the large speed of the rotor the film is constantly renewed.

The gel structure, which leads to the crystallization of the soap melt and its corresponding dispersion, is formed in the heat treatment and cooling device.

Cooling is often done by adding the remainder of the oil component followed by indirect cooling. Finally, the consistency of the final product can be adjusted by shear forces to the desired extent.

The operations mentioned are usually carried out in heatable and coolable boilers in which counter-rotating,

Known and applied in many cases, a high-speed mixer in which the mixture is forced to pass through a relatively narrow space, whereby a good heat transfer and an excellent dispersing effect are ensured.

The continuous technology for the production of Ca, Na and Li based lubricating greases (US Pat. No. 3,158,574) can be divided into three sections: the reactor, the dehydration section and the cooling section. In the first section of the reactor, operating at 27 kPa pressure and 150 ° C, the components are metered with a pump according to the recipe to give a 5 minute dwell. The dehydration unit operates at 33 kPa pressure and 19O ° C , In the end section of the cooler, a residence time of less than one minute is maintained.

Also known is a process in which the saponification at 108 /, 5''1Pa; and 340 C in a tube reactor. In another continuous process for producing engine grease, saponification is carried out at room temperature in a milling apparatus. In this, the fatty acid-containing oil component and the alkalis move at high speed between the high-speed corrugated rotor and the stator, whereby the reaction and the dispersion occur simultaneously.

For saponification, a heat exchanger Oispergator is also known, which consists essentially of two concentric cylinders. The outer cylinder is surrounded by the heat transfer medium while the inner cylinder is rotating. By attached to the surfaces

Shovels are scraped from the wall of both cylinders of the material, whereby a Mahlwirkung is achieved. With this device, a very intense heat exchange can be achieved.

Also known is a homogenizer in which the components disintegrate on a turntable due to strong shear forces into elementary particles and mix.

Finally, for the production of lubricating greases with a fixed lubricant content or for the production of lubricating liquids in the first step, the solid lubricants are also ground in vibration mills in the presence of a grinding fluid. The suspension is mixed in static stirrer tubes with the additives and the oil component, the grinding fluid is then separated in a film evaporator and recycled to the first step of the process. Thus, in this method, the dispersion takes place in a special device, in the vibratory mill, and the homogenization of the suspension is carried out in another device with static stirrers. In the pipes containing static mixing elements suitable for carrying out such processes, the material flow cross sections are identical and merely serve to mix the material. Accordingly, in these static mixers, the speed of the material flows is the same, and this does not allow for such thorough mixing that at the same time the flow of material is also dispersed. Therefore, the material must be dispersed in the vibration mill.

In summary, it can be said that in the described methods most often with mechanical stirrers, dispersed in grinding devices, and the devices

for the heat treatment scratch blade or the like included. Aim of the invention;

The aim of the invention is to perfect the previously known methods and to devise a method or a device which can be dispensed with while retaining the advantages of the continuous operation of the mechanical stirring devices. The aim of the invention is to considerably reduce the number of devices required for carrying out the method, the investment costs and the operating costs. In addition, the production process is to be accelerated, whereby a grease is delivered with constant quality.

Explanation of the essence of the invention:

The invention accordingly provides a process for the continuous production of lubricating greases in which; Course of oil, glycerides; and / or fatty acids and / or "oxidized paraffin and / or oxyfatty acids and / or other additives dispersed in the mixture and saponified dehydrated and / or desolvated the reaction mixture and the resulting fat base with stirring in a heat treatment device - if necessary with the addition of other oil components and / or other additives - if necessary cooled with dispersion and homogenized.

It is characteristic of the process according to the invention that the material streams of the components of the starting mixture are separated from one another and / or combined and, if appropriate preheated, introduced once or more times into a reactor which forms a static mixing unit,

then treated the dehydrated fat base after addition of the oil components in a heated, forming another static mixing unit heat treatment device and finally the mass, optionally after the addition of further oil components and / or other additives, in a likewise forming a static mixing unit cooling device, as a stream of material or as a plurality of parallel and rectified streams of material, that in this case the speed of the flow of material or material flows constantly changes in the opposite sense , wherein in individual sections of the speed change in at least two mutually separated by a partition wall space parts media in contact - Brings that optionally one or more media with one or more streams of material in flow, and thereby changed the direction of the flow of material and in this way in the reactor d is dispersed and saponified, and that in the Wärmehanidungsvorrichtung (holding the dehydrated fat base at its temperature, with a single or repeated, at least partial recirculation :) the fat structure is formed and finally in the cooling device cools the fat, homogenized and adjusted its consistency.

According to an expedient variant of the method according to the invention is generated in the static mixing units, in one or more of their material flows, at least in a portion of the portion of the alternately opposing velocity change deviates from the main direction of flow in the axial direction, in extreme cases to this ^ approximately perpendicular flow ,

It is advantageous to produce in the static mixing units the material flow which deviates from the main striae running in the axial direction and, in an extreme case, approximately perpendicular to this material flow at the end of the oppositely alternating section and / or thereafter.

The deviating from the main flow, in extreme cases radial flow component can also be caused by the curvature of the partition generates a radial forced flow. In a preferred embodiment of the method according to the invention, therefore, the flow of material in the static mixing units deviates from the main direction in the flow direction, in an extreme case in approximately the radial flow direction, by means of the partition walls of a forced flow: subjected.

In the method according to the invention, the material streams are contacted by discontinuities (holes) of the partitions. The contact can be made at or through the discontinuity. In the interest of better mixing, a faster stream of material is always brought into contact with one or more slower flowing streams of material. Between the faster-flowing and slower-flowing streams of material, the contacting can occur in any section of the speed change, the acceleration or the deceleration. For this purpose, in the inventive method in the static mixing units in the individual sections of the speed changes the material flows at interruptions of the partition walls brought into contact with each other »

In the process of the invention, the quality or degree of saponification, crystallization, dispersing, heating, cooling

and the homogenization are further increased by dividing the parallel material streams separated from one another by partitions at the discontinuities of the partitions by means of the flow of oppositely directed edges of the partitions simultaneously or in the flow direction into subflows displaced relative to one another.

According to another preferred form of the method according to the invention, the parallel material streams in the static mixing units are divided into partial flows by edges positioned behind the discontinuities of the dividing walls, directed counter to the flow and twisted by a certain angle relative to the end of the preceding dividing wall.

The invention relates to farner a device for carrying out the method according to the invention, The device consists of B _e containers for the starting materials, stirring, a heated saponification reactor, a dehydration and / or Desolvatationskonstruktion, a heated heat treatment apparatus and a cooling and homogenizing device.

According to the invention, this device is designed so that its heated saponification reactor, its heat treatment device and its cooling device are each formed as a separate static mixing unit, which are provided in the interior with arranged around the longitudinal axis demarcation and partitions, and the saponification reactor, the Wärmehanldungsvorrichtung and the cooling device , Static mixing unit hereinafter called :, are formed so that their with the in the direction of the longitudinal axis and / or with the direction of a plane passing through the longitudinal axis or with the order

form the longitudinal axis around delimiting walls at least partially alternating acute and obtuse angle enclosing partitions together with the boundary walls existing in the direction of the longitudinal axis at least partially from alternately further and narrowing spaces existing space.

It is expedient for the static mixing units to have, in their interior, partitions which alternately include acute and obtuse angles with the longitudinal axis or with a predetermined plane passing therethrough or with the boundary walls extending around the longitudinal axis.

Furthermore, it is advantageous if inside the mixing units partitions with discontinuities are arranged.

It is also expedient if, in the interior of the mixing units, helical partitions are arranged which, with the longitudinal axis, alternately include acute and obtuse angles and with a plane defined by the longitudinal axis a continuously changing angle.

It is also favorable when in I _n partners of the static mixing units opposite successively helically extending partitions are arranged.

According to a further feature of the invention, in the interior of the static mixing device, the dividing walls following the end of a dividing wall are offset from the first by a certain angle.

It is also advantageous if inside the static mixing units partially self-contained, a certain space part enclosing partitions are arranged.

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Finally, it is still useful if arranged in the interior of the static mixing units, with the longitudinal axis and / or a predetermined, extending through the longitudinal axis plane or with the delimiting around the longitudinal axis delimiting walls at least some part alternately acute and obtuse angle enclosing partitions of opposing tip or obtuse angle enclosing, narrowing and widening space parts forming, self-contained; · Parting walls are crossed.

With the method according to the invention greases can be produced with minimal mechanical effort and minimal energy consumption with high productivity and consistent quality.

, Ausführungsbe.ispiele:

The invention will be explained in more detail with reference to the following embodiments with reference to the drawings. It. demonstrate:

1 to 14: for the saponification reactor,

for the heat treatment device and for the cooling device used static mixing units in section,

Fig..l5 to 17: the Scheraatische arrangement of

The embodiments belonging complete device for the production of grease.

As shown in FIG. 1, in this case the boundary wall is circular, and the partitions 2 form with the longitudinal axis.

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Axis, for example, in the direction of arrow AB changing tip and obtuse angles · In the illustrated embodiment, the designated angle supplemental angle · The space part I is in the direction of the longitudinal axis, ie · in the direction of arrow AB close, while the space part II in the same Direction becomes wider, The only of the circular boundary wall 1 _; surrounded room part

III has a constant cross section, the room part ·

IV becomes narrower in the direction of the longitudinal axis and the space part, V in the same direction. So.werden the room part I and the following on this space parts IV and VII, or the room parts II-V-VIII, etc. .. alternately narrow and on, and at the same time narrow and widen the room part I and II, or IV and V, etc.

According to another embodiment of the device according to the invention, the room parts I, IV, VIl, etc., become alternately narrower and wider, while the cross-section of the room parts II, V, VIII, etc., constantly remains the same, the partitions; 2 in Fig. 1 can also be considered as a single partition 2, which has discontinuities at the points 5. In Fig. 1, the arrow A indicates the entry of the one, the arrow B the entry of the other material strata, while the arrow A3 indicates the exit of the mixed material flow.

In Fig. 2, the section C-C of Fig. 1 is shown. Within the circular boundary wall, a single partition wall 2 is arranged, which divides the space into two room parts. In FIG. 3, three partitions 2 enclosing an angle with each other can be seen, which divide the space within the boundary wall 1 into three parts. According to Fig. 4, six partitions 2 meet in the axis., And accordingly, the inner space is divided into six Raurateile.

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As shown in FIGS. 5 and 5, the boundary wall 2 encloses a square, the partitions 2, 3 and 4 are of different lengths, the partition wall 3 extends to the boundary wall

1 and allows the lateral introduction of the material flow B. The partitions 2 and 4 form a single, continuous partition, the discontinuities 5 has. In Fig. I, the discontinuity is a perforated hole or a mesh fabric.

According to FIGS. 7 and 8, the dividing wall 2 alternately includes acute and obtuse angles with an ebb, a-b, extending through the longitudinal axis. In FIG. 7, the selected plane a-b is perpendicular to the plane of the drawing. Based on this level, the partition wall 2 alternately forms acute and obtuse angles, but also forms relative to the longitudinal axis of acute and obtuse angles. Fig. 8 shows an extreme case of the preceding device, in which the selected plane a-b with the drawing plane, a zulibigen Winks! includes and the partitions 2 with the plane A-B alternately include acute and obtuse angles. Turning the plane a-b in the plane of Fig. 8, so close the partitions 2 with the plane a-b in part a right angle, so are perpendicular to this.

According to the embodiments, which are illustrated in dan FIGS. 9 and 10 include the partition walls 2 do not together an angle, but lie in one plane. The partitions 2 can also act as a single partition

2, which has discontinuities 5. At the boundary wall 1, which has a square cross-section in this embodiment, are formed by indentations 6 ,, by round and square indentations 6, constrictions. These form together with the partition wall 2 in the direction of flow first a narrowing, then a further becoming space. FIG.

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Fig. 11 shows a static mixing unit divided into four partitions by two partitions 2 crossing at right angles.

Referring to Figs. 12 and 13, the partitions 2 are formed as helical parts including an angle with the longitudinal axis. As a result, close the partitions 2 with the previously selected, passing through the longitudinal axis of the plane from a constantly changing angle. The consecutive TsennwändQ.'2 _; extend in the opposite direction helically, and with respect to the end of the previous partition wall 2, the beginning of the following partition wall 2 is offset by a certain angle. The cross sections through the partition. S, formed room dividers are constantly changing.

According to FIG. 14, the dividing walls 2, which are arranged alternately at acute and obtuse angles, are crossed by self-contained dividing walls 8, which become narrower and wider. Form space parts and are arranged in acute or obtuse angles.

In the work of mixing units according to the invention, neither their units nor their elements make any movement ". Through the units you can flow at least two Teilströrae; it may also happen that the two partial flows are identical, in this case they differ, for example, in a physical constant, such as the temperature. However, in the interests of better miscibility, they may also have previously been divided into two parts. According to the figures flow the material streams A and 3 in the direction of the arrow in the device and leave this completely mixed at the end of the static mixing unit as a material flow AB.

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The invention will be explained in more detail with reference to the following examples.

example 1

In a equipped with a stirrer 10 heated container 11 315.5 kg of lubricating oil component are pumped and heated to 70-80 C. Then, 5.5 kg of aluminum distearate, 55.2 kg of stearic acid and 0.06 kg of foam curing agent are added.

In another heatable container 13, which is equipped with a stirrer 12, 120 liters of water to 70 C eräwmrt and treated with vigorous stirring with 7.2 kg Kalkyhdrat, 2.3 kg of sodium hydroxide and 50 kg of calcium acetate.

From the containers 11 and 13, their contents by means of the pumps 14 and 15 continuously and in the ratio 2: 1, transferred in total at a metering of lOO kg / h in the provided with static mixing elements heatable reactor 15 ', where the saponification at 9O ⁰ C takes place. The exiting reaction mixture was fed into a rotary evaporator 17 with 1.3 m area and 15O ⁰ C jacket temperature, in which the mixture iss water present is completely evaporated.

The water-free fat base exiting at the bottom of the evaporator 17 is pumped by means of a pump into a heat treatment device 18 provided with static mixing elements. In the first section, the fat base is additionally added a mineral oil component, which was previously provided with the required amount of additives.

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In the heat treatment apparatus 18, the ί-bed is heat-treated at 220 ^° C. with continuous feed and continuous recirculation. The amount of grease continuously discharged from the heat treatment device 18 at a rate of 100 kg / hr is conducted into the static mixing element-equipped cooling device 19 where it is cooled to 30-80 ° C and packaged continuously. In addition, the consistency of the fat is adjusted and homogenized in the cooling device 19.

3eispisl 2

In a provided with a stirrer 10, designed as a duplicator Sehälter 11 315 'kg Sch'mierölkomponenta, introduced the solution of 2.3 kg of sodium hydroxide in 20 liters of water and 0.06 kg of antifoam agent by means of a pump. The mixture is heated to 70-80 C and then added with 5.6 kg of aluminum distearate, 55.2 kg of stearic acid, 7.2 kg Caiciuinhydroxyd and 50 kg Calciumac'etat.

Under pre recessed by means of the pump 14 constant recirculation of the prepared Suspansion is fed at a rate of 230 kg / h into the reactor equipped with static mixing elements 15 where at 90 ⁰ C, the soap formation takes place. The exiting Reaktionsgsmisch is passed in the film evaporator 17 mentioned in Seispiel ..1 and there freed from the water contained in it *

The aftertreatment of the fat with the lubricating oil component containing the necessary additives is carried out in the manner described in Example 1.

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Example 3

In dan first section of provided with static mixing elements, heated, pressurized tubular reactor 20 from storage containers, not shown by means of a pump 180 kg / h Schmierölkoraponente 30-40 ⁰ C temperature and in the second section bai 90 C 46 kg / h 12-hydroxystearic introduced.

After in the first and second sections of the tubular reactor 20, the oil and the 12-hydroxystearic acid were heated to 90 ⁰ C, 40% aqueous Lithiurahydroxydlösung is added in an amount of 23.4 kg / h at the beginning of the third section. Soap formation takes place in the last one. Section of the reactor 20,

The reaction mixture is passed into the heatable rotary evaporator 17, from which the water content in the form of vapor emerges. At the Sodsn of the Filraverdampfers the 160 C warm fat base exits and is transferred by means of a pump in the provided with static Mischaleraenten heatable Warraebehandlungsvorrichtung 13. In the heat treatment apparatus 18, the inlet from a storage vessel, not shown, is continuously added with 200 kg / h of lubricating oil component at the location. In the Warraebehandlungsvorrichtung 18 is under constant recirculation at 180-21O ⁰ C, the dissolution of the soap in the oil. To the fat leaving the tub treatment device 18 continuously in an amount of 430 kg / h, in addition, the necessary additional amount of cold oil component is also passed. The fat is homogenized in cooling device 19 containing static mixing fluid. The finished grease exits from the cooling device 19 and reaches a packaging machine (not shown).

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Claims (12)

invention claim 1. A process for the continuous production of lubricating greases, in the course of which oil, glycerides and / or fatty acids and / or oxidized paraffin and / or oxyfatty acids and / or other additives dispersed in the mixture and saponified dehydrated, the Raaktionsgemisch. and / or desolvated and the resulting fat base with stirring in a heat treatment device - if necessary, with the addition of other oil components and / or other additives - cooled if necessary dispersing and homogenizing, characterized in that the material flows of the components of the starting mixture separated and / or combined and optionally preheated once or more times in a static mixing unit forming reactor, then the dehydrated fat base after addition of Ölkoraponente treated in a heated, another static mixing unit heat treatment device and finally the mass, optionally after the addition of further Ölkoraponenten and / or other additives , in a likewise forming a static mixing unit cooling device, but as a flow of material or as a plurality of parallel and rectified material flow, that one here the speed of the flow of material or of the Ma streams constantly changes in the opposite sense, bringing in individual sections of the change in speed in at least two separate from each other by a partition Raurnteile flowing media into contact, that optionally one or more media with one or more material streams added in flow and thereby changed the direction of the flow of material and dispersed in this way in the reactor and saponified, - 18 - and that in the heat treatment apparatus the dehydrated fatty base is maintained at its temperature. under unique or repeated , at least partial recirculation, the fat structure is formed and finally in the cooling device cools the fat, homogenized and adjusted its consistency » 2. »Method according to item 1, characterized in that in the static mixing units, in one or more of their Ma.teriaiströme, at least in part of the portion of the alternately opposing speed changes deviating from the main direction of flow in the axial direction, in extreme cases to this generates approximately perpendicular flow. 3. The method according to item 2, characterized in that in the static mixing units deviating from the- in the axial direction, in the extreme case approximately perpendicular to this running material flow at the end of the oppositely alternating section and / or thereafter, testifies * 4 »Method according to item 1 to 3, characterized in that in the static. Mixing units subjects the flow of material in Stfömungsrichtung deviating from the main direction, in an extreme case in approximately radial flow direction by means of the partition walls of a forced flow. Process according to items 1 to 4, characterized in that in the static mixing units in the individual sections of the speed change the material flows are contacted by continuous interruptions in the partitions. - 19 - 6. The method according to item 1 to 5, characterized in that in the static mixing units separated by partitions, parallel material flows at the discontinuities of the partitions by means of the flow of opposing edges of the partitions simultaneously or in the flow direction against each other shifted divided into partial flows, 7. The method according to item 1 to 6, characterized in that in the static Mischsinhaiten the parallel-extending material flows through lying in the flow direction behind the discontinuities of the partitions, the flow opposite, forming the beginning of the next partition and, based on the end of the preceding Dividing wall, divided by a certain angle offset edges in partial streams. 8. Apparatus for carrying out the method according to item 1 to 7, consisting of containers for die.Ausgangsstoffe, stirring elements, heated saponification reactor, a Dehydratatiohs- and / or Desolvatationsanlage, a bar- heated Wännebehandlungsvorrichtung and a cooling and homogenisation device, characterized in that _t that their heated saponification reactor (16, 20) , Their heat treatment device (18) 'and its cooling device (19) are each formed as a static mixing unit in which one or more delimiting (1) and partitions (2) are provided around the longitudinal axis, and that dia rait in the direction of the longitudinal axis and / or with the in the direction of a plane extending through the longitudinal axis (ab) or with the delimiting walls (1) extending around the longitudinal axis at least partially abrachseInd and enclosing parting walls (2) together with the boundary walls (1) a in Direction of the longitudinal axis at least partially from alternately further and narrower again - 20 - future space (l-VIII). 9. The device according to item 8, characterized in that the static mixing units in their interior partitions (2, 3, 4) having, with the longitudinal axis or passing therethrough, previously determined level (from) or with around the longitudinal axis extending boundary walls (1) alternately include acute and obtuse angles " 10. Device according to item 8 or 9, characterized in that inside the static mixing units with discontinuities (5) provided partitions (2) are arranged, 11. The device according to item 8 to 10, characterized in that 'inside the mixing unit helical partitions (2) are arranged, with the longitudinal axis alternately acute and obtuse angles and fiiit with a plane defined by the longitudinal axis (from) a continuously changing angle lock in, 12. The device according to item 11, characterized in that arranged in the interior of the static mixing units consecutively opposite helically extending partitions (2). .13. Device according to items 8 to 12, characterized in that, inside the static mixing units, the following dividing wall (2) is offset from the first by a certain angle on the end of a dividing wall (2); 14. The device according to item 3 to 13, characterized in that in the interior of the static mixing units partially in, self-contained, a bestirntsten Raurateil enclosing partitions (7) are arranged. - 21 - 15. The device according to item 14, characterized in that arranged in the interior of the static mixing units, with the longitudinal axis and / or a predetermined, extending through the longitudinal axis of the plane (ab) or with the longitudinal axis extending around boundary walls (1) at least Partially alternating acute and obtuse angle enclosing partitions (2) of opposing acute or obtuse angle enclosing, narrowed and widening space parts forming Τ in self-enclosed Rerr partition walls. (7) to be crossed « - For this 11 sheets drawings - - 22 -