DEST006156MA - - Google Patents

Description

FEDERAL REPUBLIC OF GERMANY

Registration date: March 24, 1953 Announced on January 5, 1956

GERMAN PATENT OFFICE

The invention relates to a method for the production of lubricating greases, after which to achieve a maximum dispersion of the soap shear stress fields can be applied without this intermixing the crowd enters.

The invention also relates to a method for producing roller bearing greases, after which one Mineral oil or a synthetic oil of high V.l. (From left = viscosity index) a mixture of mixed soaps forming substances and an oil with a low V.l. adds, the mixture cools quickly and then exposed to the action of high shear rates without simultaneous mixing of the mass.

In the known production of soap-thickened In greases, the soap is dispersed in the mineral oil with heating. After complete melting the final distribution is brought about by the soap. The actual formation of the solid fat phase takes place by crystallization of the dispersed soap on cooling. To follow this procedure a sufficient To get a stable structure from which no oil separates, you have to use enough soap, so that the oil is enclosed in the fat structure by interconnected fat crystals. After In the present invention, the fat is prepared in a conventional manner by heating the mixture of oil and soap

509 627/154

St 6156 I Vc / 23 c

iM'il permanent cooling ninl Krisialli-ation her JiI ¹ Si ( ¹ IIl, there is, however, no additional mechanical energy ills another means of I) ivjiiTL'it-runir the soap.

NiH ¹ Ii Ki'ist; illis.it ion the soap and lüldunt 'the Fettsliiiktui becomes the relatively cool fat of the W Ii k Ii in; by Sehei Spanniuii'sfeldcrn oline simultaneous liieelianiselir | ^ grouping suspended. l'xi this I! el iii in 11 im ;: will the Sei lew irl; redevelopment and equal mäliigi r κι dispersed, as it was previously held for inö;. 'borrowed hall. The advantage the-, he more complete :! Dispersion of the ropes is that dal! one for the first production of fats (. ', corpse!' consistency required wavy! soap!

ids according to the previous methods llei lower

1.1 Rope halls slallt see the Thioxothropi.- d "S Svifeii-Verdiekeis better le.eln, and also! al '.-, si'! ι dl. Penetration of the IYi !!! 'products- easily on the gain (hleii set value.

1 »inch the visionary activity; ¹ u inl the soap in the form of a

2 "highly oriented linear < icbilde-dispei fourth. Except This linear Oi ieiit ieninj 'are the little ones! (ider Mi / hurry de] ropes !: I am aiii in one! '. at ic ge-dl ort, and the erhall cue I ii-.ptTsion is approaching that at all attainable finest Wi division. Do not wild the fat

2. ^r ) mechanical cooling or subjected to Ml · <h \ organ · ¹ , mi lilrilil diet · dispersion in your fat. If, however, I \. \ -, ^{I 1} VtI is mechanically stirred or mixed after the action of the shear force, this particular part of the dispersion is destroyed, and soaps

H <> particles oiler krislalle agglomerate to a dispersion together, as in the previously common lubricating greases is present.

Fs is therefore essential in the sense of binding, dall according to the finw irkuni of the shear forces, and preferably

: t5 wise also before and during their Hinv. effect, no mechanical I tuielmiischun · / des I'ettes statllindet.

Sehergeseliw indigkeiien from about io ono to 500,000 see or more is preferred. ! Cine

Ί "Considerable increase in cost can be achieved with a visionary frequency of about 10 (ion see 'or flour' ei hallen to I the consistency of the 1 ¹ YrI ir product it can in this case be precisely regulated by the visionary 'indigkeil For technical Purposes

Ί · ^Γ > are j ^ iw Γι! 1 nli (l 1 Scherrcsohw 'indk'keiteii im l'ercieh from 100000 to.) Oo 000 see' required.

I'.ei der Aiisfüliniii; ' des crrmdiiiH ^ j / einalieii \ 'learned wild the I'ett first in the usual way fiebildel and then a shear force without mechanical

.I "k'ührmif or Durchmiseliuii !. ' subjugated by making it cover a laminar st röimin: ^r .swej 'with high (leschwindiflaii and under high pressure. This can be done in a simple manner in a (iaulin I Iomo ;; enisierniaschin;' eifokvn, in which the FYtt

, ^r i. ^r i oh 11 ei η Di piece by a k'olir and then at tu \ Yrlass, the cabbage .n by a rini'foi inij'en channel hindurchp; e] is neltt, the tapered from a standing under I ^r (dcrdruck \ 'entil or stopper and a daziuyhöi i; ^f en conical barrel.' at the outlet end

fin des Kohns is formed for the same purpose can also roll mills in which the FYtt between steel whales with its f.; erin; rem distance from each other through; '! ·! is rubbed, or known Morehoiise mill to be used in which the (rode passes between high-speed discs with very little gap width. You can also use a pressure fluid use if it is operated at a sufficiently high pressure. Others with shear effects too working devices can be used, provided that there is no simultaneous mixing of durohms of the (intes.

D.is method according to the invention is on pelts applicable in which the thickener consists of mixed soaps of two or more ingredients. Mixed soap fats made from rapeseed oil soaps and fats that contain Complex high molecular weight soaps and low molecular weight Salts, such as acetates, furancarboxylic acid salt, and acrylates are thickened, are named after the erlin- (limgÄgemälien Process made. Fats that have been thickened with simple fatty acid soaps are piled up apparently not using the procedure described above.

According to one embodiment of the invention, the lubricating grease is initially formed as follows:

Refined, unblown rapeseed oil and an equal to double amount of lubricating oil are placed in a directly heated ¹ liter boiler together with small amounts of the sodium salt of a petroleum sulfonate. The kettle is equipped with a powerful stirrer or with mixing paddles. Sufficient sodium hydroxide solution is then added to the kettle, (IaM an excess of 0.3 to _{0.13 / (|} Sodium hydroxide, based on the finished IVtt, is present. The mass is increased to about 120 until complete saponification and dehydration The rest of the oil is then added and the mass is slowly heated to about 2 (> c "until the mass is completely melted. The (icniisch is then cooled to () _5" with stirring. During the cooling process, the Recrystallization of the soap, after which inhibitors are added.

If you work according to this experience, about 20 to 50 ".""Soap are required to obtain an I ¹ Vlt with a flexed exposure of 200 to 350 mm / ro according to (Ίο shocks. This as far as known per se Well-made I ¹ Vtt is ideal for the lubrication of ball bearings.

Invention genius now follows the following work step:

After cooling the mass to about 93 "and the addition of the additives is the mass added to a Weiler Voluintcil oil. This additional oil, W ⁽¹ IcIiCS may be a mineral or synthetic product, sets the soap content to about f> to i8 ^u / The fat obtained in this way does not have the desired fat structure, but rather a semi-liquid mass which is not suitable for the lubrication of roller bearings. This semi-liquid mass is now subjected to high shear speeds without mechanical penetration.

If one attempts to make a grease from the Natriumsoifo of not blown rapeseed oil, which contains only (> until iH ⁿ / _(l soap on the previously customary manner, one obtains a FYtt whose structural stability is far below that for use as roller bearing high-temperature lubricant is necessary. According to dom erundungsgoinäl.ien procedure

(, 27

St 6156 IVc / '23c

However, if a fat having a content of only 6 to i8 ° / ₀ soap, which is useful as a lubricant of roller bearings with a long service life and stable against retrogradation.

As the synthetic lubricating oil for blending the mixed soap grease, any of known synthetic Oils are used. In general, synthetic ester-based lubricants are recommended, z. B. the esters of monobasic or polybasic acids,

ίο Esters of glycols, polymerized glycols, glycol ethers, mixed esters such as alcohol-dibasic acid-glycol esters or alcohol-dibasic acid-glycol monobasic acid esters or mixtures of esters. In general, esters having from about 10 to 30 carbon atoms with branched or straight chains are preferred. Examples of particularly preferred synthetic lubricating oils are: di-2-ethylhexyl scbacate, dioctyl sebacate, di-nonyl sebacate, di-2-ethylhexyl adipate, di-C ₇ oxoadipate, di-C ₈ oxoadipate, di-C ₁₃ oxoadipate,

ao also mixed esters, such as those prepared by reacting two moles of a half ester of a C ₄ - to C ₁₀ alcohol and a dibasic acid with one mole of a polyethylene glycol, and mixtures of the above-mentioned compounds.

In addition to the ester-based synthetic lubricating oils, other synthetic oils can also be used will. Polymerized silicone oils, long-chain formals, carbonic acid esters, polymerized olefins, copolymers aliphatic and aromatic compounds, etc. are also in the process of the invention usable; the only condition that these synthetic lubricating oils must meet as blending oils, is their suitability in relation to the finished grease. The following examples serve to illustrate the invention.

example 1
Rapeseed oil

A fat of the following composition was prepared in the following manner:

Weight percent
20.9
1.0

o, 5

1.0

76.6

Components

Sodium soap from rapeseed oil
Oxidation retarder (phenyl

ci-naphthylamine)
Metal deactivator (condensation product of propylenediamine and salicylaldehyde) Stabilizer (sodium petroleum

sulfonate)

Mineral oil (Coastal type) viscosity 6.3 cSt at 98.9 °.

Procedure: The rapeseed oil soap and half of the mineral oils were placed in a heated fat kettle and heated to over 204 ⁰ . At 260 ^° the heating was interrupted, the remaining amount of oil was added, the molten mass was pumped into a cooling vessel and cooled there with stirring. At 113 ° the inhibitors were added, then the fat was removed,

'io filtered and chilled in cooling pans.

A sample of this fat was then driven six times through ^{a Gaulin homogenizer at 211 kg / cm 2.} This application of shear forces without simultaneous mixing made the fat hard as a result of the better dispersion of the soap.

table I. To
application
the
Shear force In front
application
the
Shear force 178 Walk penetration after
60 thrusts, mm / 10 286

Example 2

The fat according to Example 1 was blended with 100% mineral oil in the Fettkesscl. The mixture was soft and runny. This by-product was subjected to various shear rates in a pressure viscometer. In this apparatus, the fat was forced through a capillary 0.4 mm in diameter and 16 mm in length using varying pressures up to 211 kg / cm ² . The flow rate was determined by collecting the fat flowing out in a measured time. The shear rate in see " ¹ was calculated from Poiseuille's formula -, where Q is the flow rate in parts of space per second and R is the radius of the capillary. After the sample had flowed through the pressure viscometer, it was allowed to ^{cool to room temperature (25 0} ). After processing in a micro-fat kneader with 4 strokes, the micro-penetration was determined using a sieve with a mesh size of 0.25 mm.

The values obtained are given in Table II:

Table II

Micro-walk penetration Shear rate in mm / 10 see— ¹ after 4 thrusts in the micro-kneader 157 2I, 800 123 63,800 106 184,000 98 278,000 99 413,000 97 534> °° o 94

These values are entered in FIG. It is seen that the hardening most see at shear rates up to 100 000 ^"1. Although it is also shear rates up to sooooosec" ¹ are effective, the slope of the curve is less than at lower shear rates. It can also be seen that practically shear rates up to about 400 00OSeC ^{-1 can} be used, with shear rates of 100,000 to 400,000 being preferred and those of 150,000 to 250,000 sec- ^{1 being} particularly preferred.

509 627/154

St 6156 IVc / 23 c

By choosing the appropriate shear rate Dian can also use fats of the desired hardness llrrstelleu.

Jieispie] 3

Effect read according to the method ·? , ■ Ulf the FYtt key figures

T.

ίο According to your usual method in ^{Sehmierfetterhnik an I 1} YIt was produced, which contained 23.8 ° _MI sodium soap from rapeseed oil and 76.2 ",,, mineral oil. This IYlt was divided into two parts. Part I? was in one (iauliii 1 homogenizing machine at a pressure of 210 kg / cm ² , while portion Λ was not homogenized. The samples were then examined for their ASTM penetration and their head point. They were also tested for 30 days at () .H, <) "and 30 days at normal temperature

ao stores. I ¹ YnIeI 'they were subjected to your ASTM wheel bearing test, which is described in the appendix to the ASTM manual from November H) | 8. For this test, the sample is placed in a normal Ford wheel bearing and this is done for 6 hours at io | ^{r run} with / \\. = 0 RPM. If the Piobe fails or i) \ runs out of storage after the test, the result is unsatisfactory.

The I ¹ Yt (samples were also subjected to the spindle test of the Annular Hearing Kngineering Committee and the National Lubricants and Grease Institute. In this test, the sample is used to lubricate a bearing no ) I "/ min is operated until it fails. The results are given in hours or the duration of the lubricating time of the fat. In addition, the fat samples were subjected to the Norma-Floffmann oxidation test Oxygen bomb is introduced and oxygen is introduced up to a certain pressure.The bomb is then kept at constant temperature until a pressure drop of 0.3 kg / cm ² has occurred, and the result is given in hours.

Part H

A lubricating grease mixture which contained about 18.7 "/" sodium soap from raw rapeseed oil was prepared according to the invention, that is, a base grease was first made which contained about 30% soap. This was then below the solidification temperature (below about 93 ^° Sufficient mineral oil was then added to the mass that its soap content was about 38.7%, based on the finished product. Part A was not homogenized, Part H was subjected to a Gaulin homogenization machine at a pressure of about 210 kg / cm ^2. The products were then subjected to the tests described in Part A.

Part C.

Another FYtt produced according to the invention Contained about 12% sodium soap from rapeseed oil. Share Λ of this was not homogenized, but proportion Ii was. These samples underwent the same tests subject. The key figures obtained in this way are given in Table III.

Table III

Effect of homogenization at high viewing speeds Gaulin homogenizing machine - pressure: 210 kg'cm ²

Ziii; inunen \ et / un · .;

"/" Soap

"/" Mineral oil

properties

Spindle test at looool '/ min

(Ball bearing Nl. 20. | at 121 '), hours

Penetration at 25 ', mm Ίο

Cow penetration

Walk penetiation ((mi Stölte)

Tiopfpunkt, '(

Bleeding after 30 days of storage

Kadlagcitest

, Oxidation resistance according to

Nornia Holiniann (hours until the oxygen pressure drops around 0.5 kg'cm'-)

Part Λ part A; Portion Ii

2 ₃ ,, p

not homogenized

2 ₇ , p. 280

, .- 260 noticeable

enough

200

homogenized

\ - 2 Γι ο

none is sufficient

Part H
Part A ' Part B

18.7

not
homogenized

3 ° 3
344

strong

enough

not

homogenized

930

182
201
232
none
enough

Part C.
Part A Part H

12.0
88.0

not
homogenized

too soft

strong

enough

not

homogenized

770

2 (> 2

275
204

none
enough

34 °

627 151

St 6156 IVc / 23 c

The grease from Part A, Part A, provided for all Investigations excellent results except for bleeding. After 30 days During this storage, noticeable amounts of oil had separated out. The worked penetration of 286 mm / 10 is clearly within the permissible limits of 200 to 350. Part B, that of homogenization was subjected to was far too hard to lubricate roller bearings. A comparison of the proportions A and B of the Parts B and C clearly show the advantages of the present process. The proportions A show that the fat with low soap content is too low in consistency without homogenization. the However, proportions B show that, in addition to approximately twice the fat yield, by homogenization, excellent, Smooth, lubricious products are obtained without any noticeable even after 30 days of storage Bleeding occurs.

The greases of Part A, Part B, and Part C, Part B, according to Table III, were tested in a roller bearing which was operated for 300 hours at working temperatures of 38 to 70 ^° . Part A of Part A had a penetration of 173 after the test. This hardening is attributable to the high soap content and makes the grease unsuitable for the lubrication of roller bearings. The fat sample part C, however, did not change its consistency.

Example 4

Lithium mixed soap grease based on mineral oil

Following the procedure described below, a grease of the following composition was obtained manufactured:

Components by weight

Hydrogenated fish transacids .... 20.0

Glacial acetic acid 4.0

Lithium hydroxide monohydrate. 6.2

Inhibitor according to example 1. .. 1.0
Mineral oil (coastal oil), viscosity

6.3 cSt / 98.9 ⁰ 68.8

Procedure: The fish transacids and half of the mineral oil were placed in a directly heated fat kettle and heated to 66 ° with stirring. Then the glacial acetic acid and immediately thereafter the lithium hydroxide as io ° / _n igc aqueous solution was added. The temperature was increased and at 104-121 ⁰ then added to the rest of the mineral oil, while the temperature rose further to 271 °. The inhibitor was then added and the entire mixture was cooled with stirring. Further mineral oil was added at 93 °. The final composition contained about I2 ° / _O soap and gave on cooling a soft, lubricious product.

A portion of the fat was subjected to a high shear rate without simultaneous mixing by forcing it three times through a Gaulin homogenizer ^{under a pressure of 352 kg / cm 2.} A second portion of the fat was diluted with further mineral oil to a soap content of 6%. This product was soft and semi-liquid and was forced through a Gaulin homogenizer at 352 kg / cm ² . The penetration values of the fat samples are given in Table IV:

Table IV

Walk penetration after
60 thrusts, mm / 10

After dilution to 6%
soap

Original
fat

350

To
application

the
Shear force

167
284

These experiments show that lithium mixed soap greases can be obtained by the process according to the invention can be produced advantageously.

Example 5
Furfural fat

A furfural fat of the following composition was prepared by the method described below :

Components by weight

Furfural 10.6 ⁹ ^

Hydrogenated fish transacids .... 15.0

Sodium hydroxide 5.38

Oxidation inhibitor according to

Example 1 1.0

Mineral oil (coastal oil), viscosity

3.2 cSt / 98.9 ° 30.0

Mineral oil (coastal oil), viscosity

12 cSt / 98.9 ⁰ 38.62

Procedure: The light mineral oil and fish transacids were placed in a steam-heated fat kettle. The sodium hydroxide was then added as a 40% igc aqueous solution. During this, the temperature increased to about 38 to 41 ^° . Now the furfural was added. The aldehyde entered into a Cannizzaro reaction with the excess sodium hydroxide in the presence of the fish transic acid soap. Allowed this reaction to proceed 1 hour, the temperature rose to about 45 ^0th After ι hour the temperature was increased to about 135 ⁰ by supplying heat. Then, the heavy oil was added and the mixture heated with stirring to about 165 ^0th The oxidation inhibitor was then added and the total mixture was cooled in the kettle while stirring.

The fat thus obtained was in a Gaulin homogenizer at different pressures of the effect subjected to shear stresses without simultaneous mixing. The effect of this treatment is given in Table V below.

509 627/154

St 61 r> 6 IYr / 23c

Dim ·. · Ί al el e \ HH 1, 11th η 'ι ,, (- '->, <>) ■ ü ¹ Ί Ii Γ, ■ m-tr.it W. .itk- mo tl < IN THE I " IH tiation il hi Κι ,1,, il-tli-t I. (ι '" SlolV! 'i -It) (never according to 355

.! IO

I> c i S]> i e 1 (ι

Following the procedure of Hi Npiel 5, a l'iii furolfetl made by folgeiidii "composition:

Ingredients (levvichtspn. Vnt

! • 'in lurol κι, ο

llydiieite fish! 1 acidic .... 15. '»

Sodium Hydroxide 5. "

Oxidation inhibitor ingenious'.

I am playing ι 1.0

Mineral oil (Coastal (M), \ 'iskosity

i. |, li cSt (jS, (| '. <-} 5

Mid conl incut oil, viscosity

12 (St i) S, i) 3 1.5

Part ι

Kilir l'lube this fat has been used by different people

Printing in a (iaiilin I lomogenizer b works. The ASTM values of the l'iob.n are in Table YI an

i'ej'el μ 11.

I) i iirli. Kf Ί in '"'

ο (nil lit In inn li'ei
sated)

Yl

4 »2IO

W'.t II.] "Iirt ι .11 ion. Mm '1 c

31.0

Jl "

3.Ϊ "J-"

Part 2
Kille ZWeile l'lobe this fat- W Ul (Ie several times

M, | ,, i .no and 2S1) kg cm- driven through the (iauliii-Homogenisalol. The wave for the WaIk] K ¹ IIetialion are given in Table 11

Table \ 'II

I inn

\ V.ilK | ii-ticti. (Tii> ii, mm 10. • κι lit '' (m- 'j -'S ·' Kv Ί m-

■. | Oo

_'So

This example shows that with furfural her-Γκι Asked Mixed Soap Filling '-. r, inä Ii won will ki'iimen

According to a further characteristic of the curvature, one first makes a mixture of a mixed soap and a mineral oil of low V.I. , heats it to over 250 "in order to completely dissolve the soap, and cools it down so quickly to a temperature between room temperature and I2 () ^r from the entire Külildauer dal.i is only 2 to 10 hours. When the has (iemisch reaches this Temjieratur, another mineral oil is added, the X. I. substantially holier than that of the (is inindlageöls, whereupon one subjects the whole (iemisch high speed wedge), without a thorough mixing takes place at the same time.

It is essential that the mineral oil used for drying has a high flash point and a high λ '. I. owns. Additives to improve A · <Y. I have no effect since they crystallize on the soap particles, so that only the original YI of the base oil is effective. Such oils cannot be used for the initial dispersion of the soap due to the insolubility of the molten soap It has also been found that when the skins are made according to the usual method of slow cooling * the skin cannot be added with any mineral oils of high V.1.

After the fat has been blended with the oil of high V, I., the (linseed high Shear rates of 10,000 to 500,000 see 'or mine' subject. You work in one Apparatus in which no simultaneous mixing takes place, as described above.

The original soap sound before the addition of the high λ 'mineral oil. I. is 20I) ISTO ⁰ Z ₁₁ . With the slow cooling that was common in the past, a soap layer in this range was necessary in order to achieve the desired ASTM penetration of 200 and 350111111/10. With the further addition of the mineral oil of high YI, the soap level of the finished product drops to (1I) ISlK ⁰ Z ₁₁ . The subsequent homogenization at a high selection speed then leads to a product with a penetration of 200 to 350, preferably 275 to 300 mm ole. ICs it should be noted that one of the considerable degradation

set / .ung the cooling time apart from the desired

Penetration with a part of what was previously necessary respected soap content achieved.

The lubrication time of a roller bearing lubricant was generally considered to be proportional to the amount of soap. It has now been found that the lubricating greases according to the invention, which _{contain only about 1/1 to 1; i of} this amount of soap, have a duration that is absolutely equivalent to the known 1 "et th. This result, which is based on the addition of an oil of high YI is1, could not be achieved with the bis-in method of slow cooling *.

In the following examples, this characteristic is the Krfmdung explained in more detail.

! ■> ei *]) iel 7

a) According to the manufacturing process described below a fat was made with the following composition:

{'27 I'M

St 6156 IVc / 23 c

Components

Rapeseed oil

Sodium Petroleum Sulphonate in Solution

Sodium hydroxide

Oxidation inhibitor according to

Example ι

Metal deactivator according to

Example ι

Mineral oil '(from a coastal crude oil), viscosity

65 cSt / 37.8 ⁰ (VI 50)

Weight percent

22.0 0.5 4.75

1.0

o, 5

71.25

Method of preparation: rapeseed oil, Natriumerdölsulfonat (5o ° / ₀ solution in oil) and ¹ I ₃ of the mineral oil were introduced into a directly heated grease kettle and heated to 65 ^0th Then 4O ° / ₀ aqueous sodium hydroxide solution was added and the mass heated with stirring to 150 ^0th After the dehydration, the rest Liehe mineral oil was added and heated to 260 the fat ^0th At this temperature, the heat supply was interrupted and cooled the fat to 93 ^0th During the cooling (at about 135 °) the inhibitors were added. At 93 ° the fat was drawn off and filtered. This packaging temperature of 93 ⁰ was reached in 20 to 22 hours.

b) 75 percent by weight of this fat was mixed with 25 percent by weight of the same mineral oil. The fat obtained in this way contained 18% soap compared to 24% in the fat according to Example 1 and was too soft for the usual tests. The mass was forced through a Gaulin homogenizer at a pressure of 352 kg / cm ^2. As a result of this exposure to high shear rates without simultaneous mixing, the mass hardened to a solid fat.

The two above greases gave the following test values:

Table VIII

Penetration, mm / 10 at 25 ⁰

Resting penetration

Walk penetration after
60 pushing

Drop point, ⁰ C

Oxidation test according to
Norma-Hoffmann,
O ₂ pressure drop around
0.3 kg / cm ² , hour

Lubrication duration (spindle test),
hours

Original fat

(a)

318

326> 260

286 1900

After application

the shear force

(b )

28 ₅

227 320

i6o5

Example 8

75 percent by weight of a fat according to Example 7 (a) were with 25 percent by weight of an oil of high V. I. blended, which was obtained by phenol extraction of a mid-continent crude oil and had the following key figures:

Density (15.6 °) 0.879

Color value (Robinson) 9

Flash point, ⁰ C 246

Ignition point, ⁰ C 268

Viscosity cSt / 37.8 ⁰ 83.1

cSt / 98.9 ⁰ 8.7

V. I 103.2

Melting point, ⁰ C - 9.4

This mixture was semi-liquid and did not harden to a fat consistency even when it was circulated through the Gaulin homogenizer ^{at 352 kg / cm 2.}

Example 9

a) A fat was produced according to Example 7 (a) with the only difference that the cooling from 260 to 93 ° not slowly but quickly, namely within 8 to 10 hours.

b) 75% of this fat was mixed with 25% further base oil, for which purpose the low VI coastal oil distillate described in Example 7 was used. This mass was exposed to high shear rates without simultaneous mixing by forcing it through the Gaulin homogenizer five times ^{at 210 kg / cm 2.} The test results for the two greases were as follows:

Table IX

Orig
liches
fat Offcuts nes fat
after
application
the (a) Shear force (b) Penetration, mm / 10 at 25 ⁰ 275 Resting penetration 195 Walk penetration after 260, 60 pushing 201 Walk penetration after 274 100,000 thrusts > 2Ö0 - Drop point, ° C 241 Oxidation test according to Norma-Hoffmann, O ₂ - pressure drop around 275 0.3 kg / cm ² , hour 268 Lubrication duration (spindle 1315 test), std 927

Example 10

50 percent by weight of the fat according to Example 9 (a) was combined with 50 percent by weight additional base oil. In this way, a fat was obtained with a total soap content of I2 ° / _O. This fat was also homogenized in a Gaulin homogenizer at 352 kg / cm ² .

509 627/154

St 6156 IVc / 23 c

The lubricating grease then has the following bacterial counts:

A STM penetration, mm / io

at 25 "

Back penetration 270

Walk penetration after (> o pushing 276

Drop point, "C 204

Oxidation test according to Norma-Hoff-

jnann, hours 340

Lubricant (spindle test), hours ... 769

Example

11th

50 percent by weight of the FYtIes according to Example 9 (a) was _{mixed with 50 ° / (l} of the high VI oil described in Example 8. By homogenization at high shear rate without simultaneous

Table X

Mixing in the Gaulin homogenizer was obtained an excellent, stable fat structure based on the following key figures:

ASTM penetration mm / 10
at 25 °

Resting penetration 299

Walk penetration after

60 thrust 300

Dropping point, ⁰ C igfi

Oxidation test according to standard

H off man, hrs 220

Lubrication time (spindle test) hours 1365

The long lubrication time is particularly noteworthy as the grease only contained 12% soap.

The values given in Examples 7 to 11 are listed in the following table:

liri.spiel %
soap Kiilil-
fast-
speed VI des
Additional oil homo
embarrassed walk
penetration
mm / 10 Lubrication duration
at the
Spindle test,
hours 1315 7 00 24 slow " no 326 19ΟΟ 927 7 (1 ') 18th slow low j ^a 3 " 1605 769 8th l8 slow high ) ^Ά (no fat structure) 1365 0 00 2 1
I. fast - no 269 y (I «) l8 fast low J ^a 201 10 12th fast low i ^{: i} 276 I I 12th fast high i ^a 300

These values and the drawing show the improvement achieved with the present process. Example 7 shows that a fat of good structure and good duration of exposure can be produced if a fat ^{with a soap content of 24 0} Z _0, obtained by slow cooling according to the previous procedure, is mixed with an oil of low V. 1. to iS "/ (i Soap diluted and then homogenized. Example 8 shows that a high VI oil cannot be used for blending if one cools slowly. Examples 9 and 10 show that a lower lubrication time is obtained when a rapidly chilled fat with an oil of low V. 1. Example 11 shows the advantage of the ciTnKlungsgeniül.ien working method: A fat with only 12 "/" soap is produced by rapid cooling, and yet the lubrication time is considerably improved and the structure within the desired penetration range. These values are shown graphically in FIG.

In the following examples, the fat base is used

a synthetic oil was added before the shear homogenization.

Example 12

^{The I 1} Vtt according to Example 7 (a) served as the basis.

A synthetic lubricating oil was added to this which consisted of a mixed ester (ionic of 65% di-2-ethylhexylsebacal and ] ^e > ^l 'j " , which was obtained by reacting 2 mol of the 2-ethylhexyl half-

esters of adipic acid with 1 mole of a polyethylene glycol of a molecular weight of about 200 was obtained. About 50 percent by weight fat and Fifty percent by weight synthetic oil mix was mixed in a fat kettle. The soft, semi-liquid mass excreted clear oil on standing. The mass was passed through a Gaulin homogenizer sent and thickened. The fat then had the following key figures:

ASTM penetration, mm / 10 285 at 25 ° Resting penetration Walk penetration after 385 60 o, t6 after 100,000 bumps 180 Free alkalinity Drop point, ° C Oxidation test according to standard Hoffmann (duration of the Ab 43 » if the oxygen pressure around 0.3 kg / cm'-), std i860 Lubrication duration (spindle test, 10 000 rpm, 121 ⁰ ), hours ...

Example 13

Using the fat base and procedure of Example 12, a second fat was made manufactured. This was a liquid phenyl silicone

627/154

St 6156 IVc / 23 c

(Dow Coming, Fluid 710) as a synthetic lubricating fluid used.

The properties of the fat after homogenization were the following: 5

Penetration, mm / 10 at 25 ⁰

Rest penetration 290

Walk penetration after

60 shocks 310

Walk penetration after

100,000 joints (perforated plate with 270 holes

to 3.175 mm) 420

Drop point, ⁰ C 223

Oxidation test according to Norma-Hoffmann (duration of the decrease in oxygen ^{pressure by 0.3 kg / cm 2} ), hours> 508

Example 14

This example corresponded to Example 13 with the proviso that a formal was used as the synthetic liquid which was prepared by reacting C ₈ -OxO-alcohol with formaldehyde. Properties of the fat:

AS TM penetration mm / 10
at 25 ⁰

Rest penetration 285

Walk penetration after

60 shocks 320

Walk penetration after
100,000 shocks 410

Drop point, ⁰ C 200

Oxidation test according to Norma-Hoffmann (duration of the decrease in oxygen pressure by
0.3 kg / cm ² ), Std 398

The fats according to Example 12 to 14 showed in one accelerated test for bleeding (50 hours at 98.9 °) an oil excretion of less than 3.0%.

Claims (4)

PATENT CLAIMS: 1. A process for the production of lubricating greases, characterized in that a lubricating grease obtained in a known manner from a mineral oil and a complex soap of a high molecular weight and a low molecular weight fatty acid with the further addition of a mineral or synthetic lubricating oil is subjected to a strong shearing action at a shear rate of 10 000 to 500 00OSeC- ¹ without simultaneous or subsequent mechanical mixing. 2. The method according to claim i, characterized in that that the hot mixture of soap and oil before the further addition of oil quickly to a temperature below the solidification temperature of the Fat lying temperature cools. 3. The method according to claim 1 and 2, characterized in that there is a further oil that is used which has a higher viscosity index than that for initial mixing with the Soap owns oil used. 4. The method according to claim 1 to 3, characterized in that there is a complex soap Rapeseed oil soap is used. 1 sheet of drawings © 509 627/154 12. 55