DE1594633B1 - Process for the continuous production of lubricating greases - Google Patents

Description

The invention relates to a method for continuous shear force at a temperature within the The production of lubricating greases is subject to the range of the transition temperature putting saponifiable fatty acid material with a will. The grease mixture is continuously in the Metal base as a saponification agent in a tubular circulation through a shearing device, water-shaped Reaction zone under the condition that it is at a temperature within this bulent flow and through subsequent Ent- area is located.

soaking the saponified product in a drainage system. each zone for the formation of a calcium soap-grease-grease mixture with a predetermined ben. Here, a saponifiable material, e.g. B. tie-lube oil content a corresponding amount of lubricating oil io ric fat mixed with the saponifying agent, is fed. optionally in the presence of water and / or

For the production of lubricating greases, previously a small amount of mineral oil. The mixture is whipped, various types of continuous then continuously in a relatively small stream through processes were in the actual implementation a heating zone in which the temperature is not satisfactory on an industrial scale, although the mixture is based on at least the saponification temperature semi-continuous process, in which the temperature is increased beforehand will. The temperature produced is at least - ie in a special stage - kept at the level of the saponification temperature, soaps are used in the production process until the saponification is practically complete.
Lubricating greases have been used quite successfully. U.S. Patent 2,383,906 is also disclosed

could. The difficulties in developing ao a method for making soap thickeners of a successful, perfectly continuous mass known. It is mentioned in this patent before-procedure for the production of lubricating greases are beaten, a saponifiable material and a verin primarily to mix the critical process conditioners with one another and use them fertilize during those by metering pumps at high speed levels of the process in which the soap fibers feed 25 speed working mixer in which the are mainly formed, attention will be paid to ingredients being dispersed with each other. That have to; furthermore, the rapid implementation of this saponifiable material and the saponification agent are necessary steps in a continuous process - so that the then passed through a line in which a geman Both an economically viable throughput- suitable oil is added to the grease speed as well as a satisfactory composition. The mass obtained and a satisfactory product quality is achieved by a second mixer and a cooler can - associated with problems. Further device led.

there was a lack of the devices necessary for the

Carrying out the heretofore known continuous lent a process for the production of lubricating grease process had been developed, generally 35 materials by mixing a saponifiable of adaptability so that they do not have to be made up of a saponifying agent within a Positioning of lubricating greases of different types, extensive, unheated mixing zone, for which very diverse process conditions require heating of small amounts of the resultant could be used. Premix outside the mixing zone and reverse directions the way you would for a continuous 40 lead the same to the mixing zone until the Process for the production of lubricating grease is required, the entire mixture has been saponified practically completely and which is only known for the production of a lubricant. There will be a variety of fat of a special type can be used- mixing zones, one of which or However, several can be used for mixing in the production of lubricating grease, technical scale usually not economically 45 while the soap material is disenfranchised from another, neither for storage nor for a suitable

The US Pat. No. 3,079,341 describes the device for homogeneous mixing of the lubrication position is carried away by lithium hydroxy fatty acid soap lubricating grease.

grease in the presence of a relatively large one. In none of these US patents is a

Amount of lubricating oil known. The lubricating grease manufacturing process is disclosed in which fat mixture during the mixing operation in which the saponification step in combination with a Heat to a maximum temperature above about dehydration step can be performed. 149 ° C, but significantly below the melting point. The disadvantage of the known processes is in particular the soap is heated and then slowly cooled, which makes the manufacture of the grease many without that practically a dissolving effect due to the oil addition requires 55 hours and an extensive one, generally achieved will. A smaller stream of grease- mine made up of two floors of buildings mixture can make plant necessary during the heating process.

withdrawn and through an external return of the fat boiler. drive to provide that in a very short time

U.S. Patent 2,886,525 is historical, e.g. B. already in a few minutes, in high exhibition of grease, whereby a mixture of prey leads to first-class grease and except soap and a suitable oily liquid in which allows a system that only a proportionate amount of grease forming in a temperature moderately small space in Claims to use the process heated by above the solution temperature of the soap,
so that a homogeneous liquid mixture is formed. A process for the continuous formation of soap and the oily liquid has now been established. Then manufacture of lubricating greases by reacting this mixture with a relatively low saponifiable fatty acid material is cooled at a metal base rate, while it acts as a saponifying agent in a tubular reac-

tion zone under the condition of turbulent flow and by subsequent dewatering of the saponified product in a dewatering zone, each zone being fed a corresponding amount of lubricating oil to form a lubricating grease mixture with a predetermined lubricating oil content, which is characterized in that the saponifiable fatty acid material and the metal base are below a Reynolds number of at least 4000 corresponding turbulent conditions are introduced into the reaction zone and the grease mixture in the dewatering zone from the bottom to the top through a line having a shear valve operated ^{with a pressure drop of about 0.703 to 14.1 kg / cm 2 with} one sufficient to increase the volume of the recycled grease mixture during its average residence time within the dewatering zone to at least about five times the average total volume of the grease mixture within that zone Speed is returned. A device which can be used to carry out the method according to the invention and which has already been tried out very successfully in the production of a wide variety of lubricating greases takes up a space of only 2.44 x 3.35 m and a height of only 2.44 m and has a throughput rate of up to about 907 kg / hour. This capacity is equivalent to that of a large grease kettle occupying a two-story building, given the filling and waiting times required to operate such a kettle. Such a device can be built and operated economically in locations where large quantities of grease are required, or it can be movably mounted on a work vehicle for transport between such locations, thereby reducing the cost of packaging and shipping of the voluminous goods, which require specially equipped tank vehicles, are omitted.

The inventive method preferably has a cooling and completion stage in which the addition of a lubricating oil, which has a lower temperature than the lubricating grease mixture, take place or the grease mixture can be passed through a cooler. It is very beneficial the grease mixture either during or after cooling within a suitable temperature range subject to shear forces.

The device suitable for carrying out the grease manufacturing process according to the invention has a single zone for the dewatering stage and the soap conditioning stage, which is provided with a return line with a built-in shear valve, with the help of which the grease mixture is pumped from the bottom of the zone to the top of the zone and the returned one Electricity can be exposed to shear forces. This zone is designed to be under essential lower pressure than the saponification zone can be operated. The saponification zone acts it is preferably a flow-through reaction unit which very suitably comprises a section of pipe having an inner diameter of about 1.27 to 3.17 cm and preferably with a return or pumping system is provided, with the help of which the saponification mixture with pumped or recirculated through the reaction system at a sufficient speed, to maintain a turbulent flow. The device also preferably has a Completion section on, the facilities for cooling the grease mixture either by Has adding cold lubricating oil or by passing it through a heat exchanger. the The device furthermore has a completion section in which the lubricating grease mixture is carried out a shearing device, such as. B. a shear valve, can be returned or pumped around, namely either during or after this cooling.

When carrying out the process according to the invention, it is advantageous to use the saponification zone at at an elevated temperature and under a pressure at least sufficient that in the saponification mixture contained water in the liquid phase, and the drainage zone at an elevated temperature below the soap's melting point and below a significantly lower one Pressure to operate as the saponification zone so that the greater part of the water is entering through Relaxation evaporates as the grease mixture enters the dewatering zone. It has proved to be suitable according to the invention in detail, the grease mixture from the ground to the top of the at a temperature between 107 ° C and the melting point of the soap and below a pressure substantially lower than that of the reaction zone, preferably under a pressure of 127 to 635 mm Hg, operated drainage zone. Any remaining water will while the grease mixture is being pumped through the shear valve, the grease mixture by the pressure drop experienced by the recirculated stream as it travels through the valve, is subjected to a continuous flash evaporation process, removed. The cooling of the Lubricating grease mixture is preferably made by adding a lubricating oil that has a significantly lower Temperature than the grease mixture, and very advantageous in some cases with pumping of the grease mixture is carried out through a cooler. The procedure will be in some Cases also carried out very advantageously in such a way that the grease mixture during or after cooling by pumping through a shear device, which occurs at a temperature within a Range that varies somewhat with the different greases and mainly from the Properties of the soap used as a thickener is dependent.

In the manner described above, greases of excellent quality can be converted into good ones Yields and with greatly reduced production times, compared to the previously known processes, obtain. The advantages achieved according to the invention are to a large extent due to the influence those during the pumping over in the dewatering stage and the soap conditioning stage exerting shear force on the development of the soap fibers, and further on the combined effect of this shear force and the implementation of the saponification below turbulent conditions, as a result of which a grease mixture is obtained in which the soap molecules

5 6

or -irticellen in a highly dispersed state at a rate that leads to a

are present. Reynolds number in the range from about 4000 to

In the following the invention is based on the 100,000 leads. According to the invention it has to

Drawing further explained, the schematic achievement of the desired degree of turbulence as

Way, a device for carrying out the- 5 proved to be advantageous, the saponifiable fatty acid material

inventive method shows. rial and the metal base with a flow velocity

In the drawing, X means a tubular flush within the range from 2.63 to 52.6 liters Action vessel in the form of a pipe coil, which within a minute and per square centimeter of cross-section of the located half of a chamber 2 and introducing the reaction space into the reaction zone with lines 6, and 7 is connected. The chamber 2 is by a io In the preferred embodiment of the invention flange 3 closed and with an inlet line 4 according to the method, the saponification mixture and an outlet line 5 for water vapor or by means of the lines 6 and 7 and the pump 10 provide another flowable heating medium. The Ge is continuously pumped through the reactor 1 to Barrel 15 contains a saponifiable material or a product that provides a sufficiently high flow velocity from a saponifiable material and a 15 digkeit the flow of the reactants through Lubricating oil, which with the help of a heating device 16 to achieve the saponification zone. In this way will at a temperature above the melting point, a high flow rate through the reactors saponifiable material is held. Maintain habituation zone 1, that of the Beschiklich the vessel 15 is a mixture of the saponification rate is independent, and the turbubable Material and the lubricating oil contained in the 20 lente flow through the reaction zone can therefore the lubricating oil will maintain at least 10 weight percent of that even with a saponification mixture Mix. In general, preference will be given to that to bring about a practically fully a mixture is used that takes about 20 to 60 hours of conversion, a relatively long time contains weight percent of saponifiable material, whether it requires residence time or where due to other conditions In some cases, even lesser amounts of 25 cycles of the process have an inlet speed up to about 5 percent by weight and also higher is required, which is below that for a turbulent Amounts of up to 100 percent by weight of saponifying flow are required. The used reversible Material can be used. The guidance speed is related to the throughput vessel 20 contains an aqueous solution or an up-speed usually in a ratio of slurrying a metal base in oil. 30 about 10: 1 to about 100: 1, although in some cases

When carrying out the production of lubricating grease, also a slightly lower or a slightly higher one

Process arrives the saponifiable material with a recycle ratio that can be applied

regulated speed through the line 17, which such. B. a recycle ratio of about 1: 1

a valve 18 and a pump 19 in which up to about 200: 1.

Line 24, during a solution or a 35 The sludge of the metal base obtained under the above conditions from the container 20 with soaping products are for the subsequent stages of a regulated speed through the line of the process, in which the grease production 21, which a valve 22 and a pump 23 takes place, particularly suitably, because of the fact that it enters the line 24. Line 24 provides ease with which it accepts further lubricating oil, the mixture of the saponifiable material and the 40 rn _s , and the shorter soap conditioning times, metal base through line 25 on the suction which it compared to grease blends, the side of the pump 10 in the line 7 and passes from _un ter other saponification obtained wurder pump 10 through the line 6 in the zone 1 to require. The different physical properties of these products when saponification is carried out using an oil is evident from the fact that the metal base is slurried in an oil that when the saponification mixture is passed it is generally desirable to contain lubricating oil immediately upon cooling a small amount of water or water vapor form in the grease-like products, as opposed to introducing the reaction zone in order to accelerate the reaction to saponification products, which under different types. The reaction mixture has been obtained in the reaction conditions, such as. B. to prozone 1 is kept under a positive pressure of 50 Dukten, which have been obtained in reaction zones at least sufficient or during i where _{n is} the turbulence by other means aufder reaction, water formed in the liquid quite obtained was the existing one. Maintaining this different result phase, and at an elevated temperature, is probably due to the strong shear force sufficient to cause a rapid reaction between the reaction to which the metal base reaction mixture and the saponifiable material undergoes when it is passed through a pipe with proportion guarantee. As reaction conditions are very moderately small diameter under turbulent flows generally pressures in the range of about 0.703 to flow conditions.

21.1 atü and temperatures of about 82 ⁰ C up to The product coming from the reaction zone 1

Above the melting point of the current in the reaction reaches the dewatering zone 30 via the

formed soap suitable. Preferred reaction So line 7 and line 26, which contain a valve 27

conditions are pressures of about 3.51 to 14.1 atmospheres. The drainage zone 30 consists of one

and temperatures ranging from about 93 to about upright reaction vessel compared to the

177 ° C. to zone 1 a relatively large diameter

The flow of reactants is through the water and is closed by a flange 31-reaction zone 1 guided at a speed, 65 sen and provided with a line 32 which is connected to a which is sufficient to connect a turbulent flow within the pressure regulating device (not shown) Zone to ensure that the current is the one. It can be sheathed or otherwise the reactant is equipped with an indirect heating or cooling device through the reaction zone

be seen. The grease mixture is kept in the zone 30 at an elevated temperature above about 107 ⁰ C and usually at least about 121 ⁰ C, but below the melting point of the soap contained in the grease mixture, and at a pressure which is substantially below the pressure in the Reaction zone 1 is very suitably under a vacuum of about 127 to 635 mm Hg. In the preparation of lithium-12-hydroxystea-

a valve 50 contains, are supplied. Further lubricating oil becomes very beneficial in this way added that the lubricating grease mixture in line 26 has a lubricating oil content of at least about 10% 5 obtained if the saponification was carried out without lubricating oil or if only a small amount of lubricating oil is contained in the saponification mixture. This oil supply can continue as a means of warming of the grease mixture are used

rat thickened greases will the grease io den to the extent of water removal when

fat mixture in the zone 30 preferably on a relaxed the lubricating grease mixture in the zone 30

Temperature within the range of about 177 to will increase. That admitted for this purpose

Held at 190.5 ° C. Oil is preheated by using a pipe

During his stay in zone 30, 43 a, which contains a valve 45 a, is

the lubricating grease mixture is continuously passed through the guide direction 46.

device 33, which contains a pump 34 and valves 35 and 37, additionally or alternatively, lubricating oil from the can be returned or pumped around. The container 40 in the Versei valve 37 located in the zone 1 is a shear valve into which the mixture of molds is introduced, and in a suitable manner a slide valve which is partially fed into line 43 through line 47, the a valve 48 is held closed so that a 2 ° contains, and into the line 25. The pressure drop in this way of about 0.703 to 14.1 kg / cm ² , preferentially added oil is either in addition to or on as of about 1.76 to 8.78 kg / cm ² , used via the valve point of the lubricating oil that is obtained in the container. The return is preferably carried out after 15 is mixed with the saponifiable material, at a rapid rate so that the volume It is preferably preheated in a heater of the returned grease mixture within 25 46, preferably to a temperature of zone 30 within one minute, so that within the range from about 66 to 177 ° C. the mixture is returned, so to speak, once in addition to or as an alternative to that in the above period within this time. Preferably, the lubricating oil addition carried out in a manner sufficient to allow for at least about 5 recirculation of lubricating oil from the residence time of the lubricating grease mixture within the zone added to the container 40 to the lubricating grease mixture during the average end of the soap conditioning stage. The oil that is best returned at least about 10 times in this stage of the process can be ensured in the oil located in zone 30. The residence time of the grease-grease mixture through line 51, which the grease in zone 30 only needs to be sufficient, valve 52 is introduced. With special advantage in order to be able to achieve a practically complete drainage of the 35 grease mixture through the line, the 53, which contains a valve 54, in the return soap conditioning stage in this case direct flow of the grease mixture in the line 33 takes place in good time with the last dewatering stages. Preferably, the residence time is somewhat increased, assisted when a thick grease is kept in circulation for an additional soap conditioning time to be mixed, and furthermore to maintain, preferably by at least about 5 minutes, in some cases by increasing the temperature, in particular if the dewatering is already practically the return flow to serve an increase in the table completely at the initial or first dewatering speed. In the obi flash evaporation takes place. In the case of the Durchgen way, further oil is added in such an amount during the process under the preferred conditions that in zone 30 a lubricating grease condition can be maintained, the residence time of the lubricating grease is mixed, which is at least about 25 minutes in zone 30 up to about 1 hour weight percent of lubricating oil and preferably min, which mainly contains at least about 40 weight percent lubricating oil, or the type of lubricating grease mixture in addition to the function of the soap contained in the lubricating and to a lesser extent of 50 lubricating oil added to zone 30, other factors, such as the temperature, the soap being used as a means for setting the desired soap concentration of the lubricating fat mixture and the concentration, the oil addition can depend on the co-properties of the lubricating oil. For either heating or cooling the preparation of lithium and calcium hydroxy grease blends thickened greases to a temperature within fatty acid soaps, the grease blend residence time in the area appropriate to the desired soap conditioning temperature is. If the saponification at zone 30 is usually about 5 to 20 minutes, although shorter or longer times at temperatures above the melting point of the soap are used in some cases, this may be useful. lines 51 or 53 in the in zone 30. To the lubricating grease mixture introduced in various 60 grease mixtures, further lubricating oil from the lower temperature as lubricating grease mixture, container 40 can be added, preferably at stages of the process, to the desired one leaving the saponification zone. If the sizing soap concentration is to be maintained or in order to support the heating at a temperature below the tempera- ture required for the conditioning treatment to be subjected to the soaping or cooling of the grease mixture. This additional oil can be carried out in the lubricating grease 65 temperature range, the mixture as described above in the line 26 via the line 41, which contains lubricating oil preferably added before a valve 42, the line 43, which is heated by a pump. The temperature of the lubricating oil and the supply and a valve 45 contains, and the line 49, the given amount can be adjusted so that

109545/343

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the desired soap concentration is achieved in the grease mixture in zone 30 and that continues to achieve a temperature within the desired soap conditioning temperature range will.

Either in addition or as an alternative to the heating or cooling provided by the methods described above Once the oil has been added, the lubricating grease mixture in zone 30 can be heated indirectly

a valve 83 contains α, passed through a cooler 85 will. The lubricating grease mixture can be returned through the line 79 with the aid of a line 89 to achieve multiple passes through the shear-5 valve and cooler 85. From the line 79, a flow of the grease mixture is taken off through line 87, which is a valve 88 contains. Additional lubricating oil that is the same or one can be added to this stream of the lubricating grease mixture

or be cooled. Indirect heating or having a lower temperature, with the aid of a cooling system, can be carried out in a very convenient manner, which contains a valve 72, either by using a covered zone for zone 30 or in addition to that through the Line 66 is used as the vessel and, through the vessel jacket, a lubricating oil added as described above, conducts a flowable heat exchange medium. Become very much. If further oil is added in this way, in some cases the indirect heating 15, it mixes with the grease mixture, or cooling in the return stream of the grease mixture when the combined flow is made through the valve 88 grease mixture in the line 33 by passes, which is operated as a shear valve. The lubricating grease mixture with the aid of a line 33 a, the flow of the lubricating grease mixture, which in this way contains a valve 35 α, through a heat-added oil, can optionally be passed through exchanger 36. It is Z. B. in some falsifying 20 additional shear devices, len particularly advantageous to use the return flow in the lubricating grease additives.

this way to cool as a result of the more viscous det, so they will be in the during cooling Mixed grease produced on cooling, mixed grease introduced, usually when the to achieve an increased shear force. Lubricating grease mixture a temperature below

From the recycle stream in line 33 25 is about 121 ° C. As shown in the drawing, with the aid of a line 75, which a pump 76 can contain the additives from the container 90 with, a stream of a practically drained aid of a line 91, the valve 92 and a grease mixture is continuously withdrawn. To pump 93, the lubricating grease mixture located in the line 75 is fed into the lubricating grease mixture located in the line 75, after which the addition of the lubricating oil from the line 66 can be evaluated 61 from the container 60 with the aid of a line Valve 62 contains, and a line follows. When the lubricating grease mixture has reached the point 66, which contains a pump 67 and a valve 68, a sufficient amount of lubricating oil cannot be added at this point in time. It is ordinary temperature is low, which may In addition preferred to add this oil at a substantially below medium at some later time in the temperature of the lubricating fat blend ₃₅ of the cooling and finishing section added temperature. A very suitable tempe- will be. In the production of Stauffer greases, the ambient temperature is used in some cases. In
In many cases, however, it is advantageous to preheat the oil by using the line 66 a, which is a
Valve 68 contains α, through a heat exchanger _4O
70 is passed, especially if the addition of oil with
high speed is done or when desired
is to achieve a slower cooling rate.
Alternatively or in addition, oil can be removed from the container

40 by means of line 41, line 64, which contains a ₄₅ 100: 1 and "preferably from about 5: 1 to about valve 65, and line 66 into line 50 _: 1. The shear force-75 carried out in this way" is introduced The container 60 is used in the
Procedure in general only in conjunction
used with the container 40 when in the
Lubricating grease two different lubricating oils used _5o
will.

That in line 75 to the grease mixture
any given additional oil can be approximately 90 percent by weight of the total oil content of the finished grease

turn off. Usually, it is preferred to be ₅₅ commonly used for the preparation of the soaps USAGE grease manufacture in such a manner to perform, det, which are contained in the greases, that about 20 to 80 weight percent of in the sodium, lithium, potassium, calcium , Barium, Ma-grease contained in this total amount of oil contained in this magnesium, zinc, cobalt, manganese, aluminum, lead way at a temperature that can be around, etc., as well as mixtures of two or more metals 56 ° C below the temperature of the grease mixture 60 lies as a metallic component of the metal base in the line 75. act. Metal oxides, -hy-

From the line 75 the lubricating grease mixture gets used hydroxides or carbonates. Lubricating grease into the line 79 which has a pump 80 and valves 81 based on an alkali or alkaline earth soap or one and 83. The valve 81 is a mixture of two or more such soaps To a shear valve, such as a slide valve, which can be set at 65 according to the method according to the invention operated with a substantial pressure drop is very advantageous.

can. If further cooling is desired, the appropriate saponifiable materials included in the

Lubricating grease mixture with the help of a line 79 α, the method according to the invention can be used

the stabilization water is also added during completion when the grease mixture has a temperature below 99 ° C.

In general, it is advantageous to recycle the grease mixture through a shear valve 81 which is operated with a pressure drop of about 1.41 to 14.1 atmospheres using a Recycle ratios from about 1: 1 to about

treatment is preferably carried out at a temperature of the grease mixture below about 149 ° C and most advantageously in most cases at a temperature within the range of about 66 to 121 ° C.

The metal base used in the saponification can either be a hydroxide or another basic be reactive metal compound like them

Π 12

nen, the higher fatty acids are shown with about 12 to 32 drawing as well as introducing the Carbon atoms and the hydroxy substituted reactants and the additional lubricant Fatty acids, the glycerides of these fatty acids oils, for transferring the lubricating grease mixture and other esters as well as mixtures of these sub- zones and for withdrawing a prostance. The inventive method can also 5 duct stream. The reactor consisted of a 6.4 m Long 1.905 cm "Schedule 40" section applied to the manufacture of greases where higher fatty acids or their black plate pipe (inner diameter 2.09 cm). The derivatives in connection with lower fatty acids or ser was to a coiled pipe with an inner thread Derivatives such as B. deformed fatty acids with 1 to 6 diameter of 10.16 cm in Carbon atoms, their glycerides, and others in a 91.5 cm long section of 30.5 cm tube, Esters, can be used. These lower fatty acids, which served as a water vapor chamber, were attached or their derivatives can be used in such amounts. The recycle line at the reaction zone apply that a molar ratio of lower consisted of 275 cm 1.905 cm tube and contained one Fatty Acids To Higher Fatty Acids Below 1: 1 Recycle Pump which is a Vikingbis is about 20: 1. In connection with the 15 high-performance rotary pumps with a capacity of higher fatty acids and their derivatives can acted 68 liters / minute at 1200 revolutions, also fatty acids with intervening carbons. The capacity of the reactor and the number of recycle atoms used in various amounts pipe, including the pump, was 3.39 liters, usually in such an amount that the dewatering device consisted of one compared to the higher fatty acids or their derivatives - 20 91.5 cm long section from 25.4 cm "Schedule 40" - ten a molar ratio below about 1: 1 pre- black plate pipe with one blind flange and one lies. Bell cap on the ends and was replaced by a

As an oil-like liquid used according to the invention, a winding made of obstacles attached to the outside oils with lubricating properties are suitable, and wire rods are electrically heated. The return z. B. the usual mineral lubricating oils, the synthetic line on the drainage device consisted of see oils as they are used in the various refining processes with a 1.525 m long section from a pipe process, with the cracking and polymerization process an inside diameter of 2.09 cm, the one incurred. Other synthetic recirculation pumps of the same type as those in FIG oily compounds, such as. B. high molecular weight recycle line of the reactor was used, Ether and ester. The dicarboxylic acid esters, such as. B. 30 and a Fulflo valve included. The dehydration di-2-ethylhexyl sebacate, Di- (sec.-amyl) -sebacate, di-2-device was at its upper end by an ethylhexyl acetate, diisooctyladipate, etc. put a tube that has an inner diameter of 5.25 cm appropriate class of synthetic oils, with a vacuum connection and a condar and can either be connected as the only oily operator. The reactor and the drainage component of the grease act or in the graining device were among each other through a bination with other synthetic oils or mine-pipe with an inner diameter of 2.09 cm, the ral oils can be used. had a Fulflo valve connected. At the cooling

Suitable mineral oils are those that have a lower viscosity than a water-cooled Gra within the range of 100 to 8000 ham-Heliflow heat exchangers consisting of SSU (Saybolt Universal Seconds) at 38 ° C on a jacket and tube through which the grease is transported sen. It can be a mixture of low viscosity of 60 liters / minute and highly viscous either naphthene bases were left, resulting in a turbulent flow or paraffin-based oils.

Mixtures of two or more oils of these compounds The following materials have been used for lubricating

different types. 45 grease production used. With the saponifiable

In the production of lubricating greases from synthetic material, it was a question of commercially available table oils, which are hydrolyzed under the saponification conditions 12-hydroxystearic acid with a saponification number of 186, a neutralization number of 177 and one in the absence of the lubricating oil or in Ge iodine number of 3. The lubricating oil currently consisted of only a small amount of a lubricating mixture with a Saybolt universal viscosity for oils that, under the saponification conditions, practically 99 ° C for about 84 seconds. It was preserved in which is such. B. a mineral oil; the synthetic den by mixing 35 percent by volume of an oil is then added only during the later stages of the paraffinic distillate oil of a Saybolt universal lubricating grease production process in the above viscosity in the range of 175 to 190 seconds in the manner described. 55 38 ° C, with a steam treatment

The following examples serve the further refined and deasphalted Manvel residue oil Clarification of the invention on the basis of the production of a Saybolt universal viscosity at 99 ° C in the different Lubricating greases. ranging from 155 to 163 seconds. That used

The saponification agent was an aqueous lithium hydroxide

Example 1 _6o solution containing 9.3% lithium hydroxide.

A lithium-12-hydroxystearate thickened is now a detailed description of the

Lubricating grease was produced according to the manufacturing method according to the invention. A solution to the 14 dangers made in the following manner. weight percent 12 - hydroxystearic acid in the The device used in manufacture contained lubricating oil and in the hopper consisted of a coil reactor, which had been preheated to 65 ° C, was placed in the Dewatering device and a cooler as well as reactor with a speed of 39.1 kg / Auxiliary devices for pumping the grease hour introduced, and the aqueous lithium hydroxide mixture through each of these zones in the solution, which was at room temperature

13 14

into the reactor at a rate of The above data show that in the continuous

5.8 kg / hour introduced. The grease production plant operating in the reaction zone with an on-site mixture received ^{a very satisfactory grease under a pressure of total residence time of only 15.3 minutes in the 4.92 kg / cm 2} at the inlet end of the reactor pipe layer and of 4 , 78 kg / cm ² at the outlet end of FIG.

Reactor coil to a temperature of In contrast, is in the usual manufacture

Heated to 154 ° C. The recycle pump was operated with a lithium 12-hydroxystearate grease at a pumping speed of 68 liters / minute of a known low temperature operating condition which resulted in a recycle ratio of the processes an average time of about 80: 1. The recycle stream required 10 11.4 hours. The grease was taken from a product stream and continued to be obtained in optimal yield with expansion, which can be seen from the fact that a part of the grease device is introduced through a non-return valve in the drainage system, where it is under a va grease that has a passage through a 381 mm Hg vacuum was heated to a Premier Colloid Mill temperature at 0.0762 mm between -185 ° C. The lubricating grease mixture in the processed state was subjected to a distance in the dewatering zone 15 and had a penetration value of 284, ie it was returned at a rate of 68 liters / minute, and the same penetration value as the unmoved valve in the return line was worked in Product,
was set that a pressure drop of about 4.7 kg / cm ² Example 2

was achieved. Further lubricating oil that is in the bearing 20

Preserve the container at a temperature of 173.5 ° C. A thickened with calcium-12-hydroxystearate

had been heated, in the recycle stream grease was prepared according to the invention on the suction side of the recycle pump with procedures in the following manner:
introduced at a rate of 73.3 kg / hour. The same device as in Example 1 was used

The volume of the grease mixture used in the 25.

The drainage zone was at about 23.8 liters. resulting in an average residence time. With the saponifiable material of the grease mixture in the dewatering zone was commercial 12-hydroxyvone 10 minutes led. During this time, stearic acid, as used in Example 1, was added the mix averaged 28.6 times through the 30. The mineral oil used was Return line returned, d. that is, a paraffinic distillate oil with a Saybolt grease blend becomes during the average universal viscosity at 38 ° C of about 347 seconds Dwell time 28.6 times through the drainage points and by a small amount - corresponding approximately zone pumped. 1% of the finished lubricating grease - a »Manvel« -

From the recycle stream, residual oil with a Saybolt universal viscose side was made at the outlet the recirculation pump a product flow sity at 99 ° C for 55 seconds. Accepted as saponification and pumped through the cooler until medium became lime in the form of a 10% Aufer had cooled to 93 ° C. slurry used in lubricating oil.

A smooth or even lubricating grease from The following is a detailed description of the at

excellent texture and excellent 4 ° of manufacturing grease applied Appearance was carried out in the manner described above. A 20.3% solution of the saponifiable in a total preparation time of 15.3 minutes of material in lubricating oil preheated to 93 ° C obtain. The grease that was produced was fed into the reaction zone with a obtained the following analysis and test results: speed of 39.7 kg / hour introduced, and

4.5 the slurry of lime in lubricating oil, which Composition (%) was at room temperature, was

Lithium-12-hydroxystearate 6.0 introduced at a speed of 10.8 kg / hour. That

Free neutral fat 0.41 reaction mixture was taken in the reaction zone

Free fatty acid none heated to a pressure of 4.92 kg / cm ² (at the coil-free alkali 0.12 50 inlet end) to 3.51 kg / cm ² (at the coil-water 0.05 outlet end) to 127.5 ° C . The repatriation

at the reactor was at a rate of

Test results _{carried out 68} liters / minute, which led to a back penetration according to ASTM at 25 ° C lead ratio of 66: 1. The product unprocessed 272 ₅₅ stream, which has a calculated soap content of 17.2%

processed, had 60 operations, was introduced into the drainage zone,

or working hood 281 where it is at 139 ° C and under a vacuum of

processed, 10 000 working stroke was kept 287 127 mm Hg. The grease mixture

Drop point according to ASTM (° C) 193 was from the bottom to the top of the drainage

Oxidation in the bomb according to ASTM 60 zone at a rate of 68 liters

(Pressure drop in kg / cm ² per minute with the help of a return line.

100 hours at 99 ° C) 0.563, which is a recirculation pump and valve

Shell Rolling Bearing Test included the one with a pressure drop of about

(Shell roll test)) 4.43 kg / cm ^{2 was} operated. Other lubricating oil,

Original penetration 265 65 which had been preheated to 140 ° C was used in the

Penetration after the test in the return flow on the suction side of the return rolling bearings 283 lead pump at a speed of

Increase in points 18 62.5 kg / hour introduced. In the drainage zone

a volume of approximately 24.9 liters was maintained, resulting in an average residence time of the grease mixture for 10.7 minutes. During this time it got average Returned 29.2 times through the return line. The one coming from the drainage zone Product stream was pumped through the cooler at a rate of 68 liters / minute, what resulted in 30 passes of the reaction mixture through the cooling zone. The grease mixture was cooled in this way to 90.5 ° C.

A smooth, uniform grease of a butter-like texture was obtained. The received Grease had the following analysis and test results.

Composition (%)

Calcium 12-hydroxystearate 8.1

Free neutral fat 0.29

Free fatty acid 0.05

Free alkali none

Water traces

Test results

Penetration according to ASTM at 25 ° C

unprocessed 249

edited;, "279

Drop point according to ASTM ( ⁰ C) 151.5 ° C

Oxidation in the bomb according to ASTM

(Pressure drop in kg / cm ² within 100 hours at -99 ° C) ...... 0.28

The above data show that a grease with satisfactory lubricating properties works in good Yield had been obtained with the average total time only about 15.3 minutes fraud. In addition, the difficulties encountered with the known methods of lubricating greases to obtain this type in a satisfactorily smooth or even form when carrying out overcome the production in the manner described above.

Example 3

A grease thickened with sodium salts of tallow fatty acids was prepared according to the present invention Process prepared in the manner described below.

The same apparatus as in Example 1 was used except that in the Completion stage in the in F i g. 1 a shear valve has been attached.

The following starting materials were used. In the case of the saponifiable material acted it is commercially available hard tallow with a high acid content. In typical tests on such Materials will have a saponification number of 200, a free fatty acid content of 4.2%, a Iodine number of 52 and a titer of 41.6 ° C were found. The lubricating oil used was a deasphalted one and dewaxed residual oil from a paraffin-based crude oil having a Saybolt universal viscosity at 99 ° C for about 189 seconds. The saponifying agent was sodium hydroxide in the form of a 49% aqueous solution.

A detailed description of the process used in its manufacture follows. The saponifiable material and lubricating oil streams preheated to 99 ° C were introduced into the saponification zone at rates of 0.134 kg / minute and 0.253 kg / minute, respectively, while the alkali solution, which was at room temperature, was introduced at a rate of 0.0389 kg / Minute was introduced. The reaction mixture was heated to 168 ° C in the reactor under a pressure of 10.9 kg / cm ² (at the coil inlet end) to 7.73 kg / cm ² (at the coil outlet end). The recycle at the reactor was carried out at a rate of 68 liters / minute resulting in a recycle ratio of 144: 1. The product stream, which had a calculated soap content of 30.8%, was introduced into the dehydrator where it was maintained at 184.5 ° C and under a vacuum of 508 mm Hg, while flowing at a rate of 68 liters / o. Minute was passed through the return line. This had a shear valve which was set so that a pressure drop of 4.92 kg / cm ^{2 was} achieved. In this example, no additional oil was added to the grease mixture in the dewatering zone.

The height of the grease mixture in the dehydrator was kept at approximately 38.1 cm. resulting in an average grease blend residence time of 49.4 minutes. During this time, the grease mixture averaged 144 passes through the return line subject.

The dewatered product stream withdrawn from the dewater was cooled by the addition of lower temperature lubricating oil and returned through the shear valve at a recycle rate of 37.8 liters / minute, resulting in a recycle ratio of 14.8: 1 and one Total residence time of the grease mixture in the finishing section of 0.44 minutes. In this example there was no circulation through the cooler. The additional oil added at a temperature of 88 ° C. was introduced into the flow of the lubricating grease mixture at a rate of 1.88 kg / minute. The shear valve installed in the return line was adjusted so that a pressure drop of 9.84 kg / cm ^{2 was} achieved. The product stream was withdrawn from the completion section at a temperature of 90.5 ° C.

In the manner described above, a grease with the uniform, weakly stringy Texture as desired in a sodium soap grease of this type, and obtained superior lubricating properties. The product delivered the following analysis and test results:

Composition (° / o)

Sodium soap 5.3

Free neutral fat · 0.23

Free fatty acids 0.17

Free alkali none

Water 0.05

Test results

Drop point according to ASTM ( ⁰ C) 152

Penetration according to ASTM at 25 ° C

unprocessed 355

machined, 60 working hood 383

109 545/343

machined, 100,000 working hood ... 382
Shell rolling bearing test test

Change in penetration value

in points + 12

The above test results show that, according to the method according to the invention, sodium salts are used from tallow fatty acids thickened lubricating grease can be obtained in good yield and in a greatly reduced production time, the inventively Total required time is approximately 1 hour, as opposed to over 21 hours in manufacture a technical approach to this grease in a conventional grease kettle are required. Furthermore, the lubricating grease obtained according to the present invention was that produced by known methods Lubricating greases with certain properties, in particular with regard to shear resistance, consider what can be seen from the fact that there is a change in the Shell Rolling Bearing Test the penetration value of only 12 points occurs, compared to a change in the penetration value from 24 to 65 points for products manufactured in a known manner.

Claims (3)

Patent claims: 1. Process for the continuous production of lubricating greases by reacting saponifiable fatty acid material with a metal base as saponifying agent in a tubular reaction zone under the condition of turbulent flow and by subsequent dewatering of the saponified product in a dewatering zone, each zone for the formation of a lubricating grease IS Mixture with a predetermined lubricating oil content, a corresponding amount of lubricating oil is fed, characterized in that the saponifiable fatty acid material and the metal base are introduced into the reaction zone under a Reynolds number of at least 4000 corresponding turbulent conditions and the lubricating grease mixture in the dewatering zone from the bottom to the top through a Line which has a shear valve operated with a pressure drop of about 0.703 to 14.1 kg / cm ² , with one for the increase in the volume of the returned grease mixture during its average residence time within the dewatering zone to at least about 5 times the average total volume of the grease mixture within sufficient speed is returned to this zone. 2. The method according to claim 1, characterized in that the lubricating grease mixture from Bottom to the top of the at a temperature between 107 ° C and the melting point of the soap and under a pressure substantially lower than that of the reaction zone, preferably under a pressure of 127 to 635 mm Hg, operated dewatering zone is returned. 3. The method according to claim 1, characterized in that the saponifiable fatty acid material and the metal base ^{are introduced into the reaction zone at a flow rate within the range of 2.63 to 52.6 liters per minute and per cm 2 of} cross section of the reaction space. 1 sheet of drawings