CS220309B2 - Lubrication grease - Google Patents

Abstract

Org. liqs. are thickened using sulphonates of Gp I and II metals, followed by heating and/or milling the mixt. Pref. the obtd. compsns. contain 60-95 wt.% lubricating fluid and 5-40 wt.% sulphonate of an alkaline earth metal, Zn or Al, derived from >=1 alpha-olefine. The process is used for prepn of lubricants, esp. greases. The lubricants have high resistance to stresses and loads, and high drop points.

Description

The ^y .se finding relates grease based liquid lubricant selected from mineral oils, polyglycols, esters, silitony and sulíonátu ^to ovu П. or III. StopIN periodicto ^system píučemž said sulfonate is the sulfonate containing 12 to 24 carbon atoms and said sulfonates having increased alkalinity expressed excess al ^{Alice to} ACTIVE Ionia ^ ² correspond to 0 and ^Z 90 milligrams of potassium hydroxide per gram of said ^sulphonate. K ^{p s} ALN mazteo TVOne 60-9 ^5% hmotnostníc ^h and this sutíonát:

^and 40% hmohrostnícte azaC ^{t M} u ^k is poorly ^PS en ^Star mecliarncto and ^fy zikálněchemické properties.

The present invention relates to a lubricating grease based on an oil component and a sulphonate which is formed by the concentration of liquid organic substances using metal sulphonates belonging to the second and third groups of the periodic table.

Use of liquid lubricants, even though it is very common for easy application, wide range of uses and the ability to dissipate heat by friction, has the disadvantage that it is necessary pn aplikarn těctto lubricants ^p ou ^live tesnicmh systems, to avoid losses. This problem can be overcome by use. hardened lubricants, which are commonly called greases. These fats usually form a mineral oil component and a stiffening agent which causes the stiffness of the mixture.

Fatty acid soaps with lithium, sodium, calcium and aluminum and, to a lesser extent, potassium, magnesium, barium and lead are commonly used as reinforcing agents. The fatty acids mentioned are usually palmitic, oleic, stearic and other carboxylic acids. Other reinforcing agents, such as asphaltenes, carbon black, organobentonite and other silicate colloids, have not been industrialized.

In most cases the application is used as the oil component of the lubricant of the petroleum fraction, while for special applications such as extremely high temperatures; b y equal ^yl when ^p Raven ^Y lubricating the ^alkyl having from ^{y to} yc ^h ntetic oil microcapsules such as aliphatic diesters, polymerized ethylene oxide, siloxane and fluorinated hydrocarbons. Oxidation stability and extreme lubrication capability can be improved by the addition of compounds that are used for the same purpose in liquid lubricants.

The most important properties of lubricating greases are the density (expressed in penetration value) and the viscosity of the preparation liquid. Density is generally reported using the depth of penetration of the cone into the various sizes of the grease in advance ^^ (^ b ^ c ^ ikovaných conditions. The density depends on struMuře lubricants and / No ^b ^ of the rnterakcmh ovacfch components as mentioned above.

Used ^to ovovýc ^{h sulfone She's,} especially at ^é · suh metal sulfonates or alkaline earth additive and also as thickeners for solid lubricants is known. ^T and ^to the many compounds anUkorožtenteh inhibitors for the solid lubricant comprises an alkaline earth metal sulfonate or sulfonates of alkaline earth metals. However, the use of sulfonates of different nature to improve the properties of lubricants, such as corrosion resistance and homogeneity, may affect other characteristics, such as resistance to water. In many cases there is even a strong tendency to overly thin.

BACKGROUND OF THE INVENTION Lubricating compositions according to U.S. Patent No. 2,951,809 based on a fatty acid soap solidified with a C12-22 fatty acid ^{and an} —SO3H group attached to an alpha-carbon atom and an alkali metal group are known in the art. and alkaline earth metals, as well as by U.S. STOT America ^to ACTIVE no. ²⁵³⁵ W1 to bases ^and mineral · lubricating oil which is thickened oil-soluble sulfonate having a molecular weight of sulphonate radicals greater than 300 and an oil-insoluble sulfonate-sulphonic acid of molecular weight range from 96 to 250, and also greases according to U.S. Pat. No. ^2,854,408 to ^Ba Zi mineráhhho ^to ovu and aliphatic sulfonic acids in a substantially straight chain containing 10 to 20 carbon atoms per molecule in the aliphatic chain.

It is an object of the invention to provide a lubricating grease with improved mechanical and physicochemical properties, in particular ^x density, load resistance, anticorrosive and water resistance, as compared with the prior art.

Summary of the grease according to the vynMezu ^{SPO, or} in ^a · ^P o ^dL e said VYN ^s climb in that it comprises a liquid lubricant in an amount poh ^ ujmta in a ^pH in the range from ^60% to 95% ^h motnostn ^I C ^{h, the} ter ^é is ^{characterized} br ^and come from the group consisting of mineral oils, polyglycols, · wherein said polyglycol is preferably polyglykolpolyoxypropylen, esters wherein said ester-m ^ is preferably dioctyl sebacate, silicone, wherein said silicone is preferably dimethylpolysiloxane, and that the salt on ^{F whether} for metal II. and III. sku ^p m ^yp eriodické system in an amount ^{ranging, and} from 5 to ^40% hmotnostmc ^ wherein said sulfonate is the sulfonate containing 12 to 24 carbon atoms, and said sulfone ^sulfates · maj ^also increased zásadites ^ rubbed ^BC e ^would tkem alkahckých ions, odpovteaj ^I C ^{d ≥ 90} and ²⁰ milligrams of potassium hydroxide are ^hydroxy per gram of sulfonate.

Preferably, the metal is an alkaline earth metal, zinc and aluminum.

It is also advantageous if said oil _E has a viscosity in the range of viscosity grades are characterized viscosity maxima ^AL n ^{E 13} 0 ^{2 0} mm ^/ s at teptete -Г · ^{7.8 C} C until viscosity grades with a viscosity of 25-43 mm ² / s at 98 ° C, the freezing point is less than ³⁰ ° C and ^b is at least 150 ° C from the flash point.

In the case of lubricating grease according to the invention it is further advantageous if said polyglycols, esters and silicones have viscosities Move ^I C ^s in the range from 6.3 .lit ⁶ m ^{2 /} s. to ^1.52 . . ¹ 0_ ⁴ m ^{2 /} sp ^r i te ^pl OTE ⁵⁰ ° C ^P s ^No em ^f ziůstevaj ^{s t} e ^k at ^the temperatures ntéšmh not ^from - ²⁰ ° C, and at the same time exhibit a high resistance to oxidation according to ASTM D 942, which means that after ^kl es Ua ^{to run} with EM lOOhodinového test ntéší than 20.7 kPa.

The solid lubricants prepared according to the present invention generally have a high resistance to mechanical stress, a higher resistance to load and a high drop point. In comparison with the prior art, the greases according to the invention have a higher load resistance as measured by a four-ball apparatus for testing the strength of a lubricating oil film, compared to the products of U.S. Pat. No. 2,535,101. these values for products according to the invention range from 300 to ^{40 kg} / cm ² . Furthermore produ ^KTY according to the invention exhibit a loss in promývámm ^d ou less than ^1% and odlumvost oil microcapsules is not ^of MeNH 2% (standardrn tests at air pressure).

The organic liquid component which are thickened in order to prepare the grease of this invention may generally be substances which have a viscosity values regarding that ^no EM ^P rc ^h avos ^y in a range of values of t ^{yp ic} ACTIVE ^P ro ^ORG amck ^é after the solvent to values typical for lubricating oils. For example, the organic liquid may be selected from acyclic, aliphatic and cyclic alcohols, ketones, aliphatic or forged ^^ chterovanýc ^h aromatmkých uhtevodíto and sihtonp pncíemž may ^b e ou ^tp ^ ito tec ^h it you ^from the EC alone Neto ^MU YT ^b e used as well a mixture of these tate ^k .

If th e ^No ovovýc ^{to h} are the sulphonates ^b Proceed with ^the ovov altíatícto sultená ^é ^ o interpreted alkylmonosulfonáty ^{b, b} of not alkylendisulfonáty ^{hydroxyacetophenone plurality of projections y} and ^y lmonosu ^LF sulfonate. The sulfonates are preferably obtained from suitable olefinic fractions, in particular from 12 to 24 carbon atoms. It is preferred to use α-monooleflnů having different molecular ^h option ^to ter ^s after show sultonarn and conversion to the sodium and ammonium salts are converted into the corresponding salts of metals of the II. or III. groups of the periodic table. Can thus be used sulphonates napnklad lime ^ p ⁱ and ^bar, zinc or aluminum totem j and ^k in the ^f orm ^of the sultená ^ ^k i · disulfide sulfonates.

In addition, the amount of metal (particularly calcium) found has been found^praven^y jato bazicto zave^dním p^riadavné an amount of metal (especially calcium) provides a thickener that is better than the corresponding neutral. sulfonate.

An organic liquid component which is kneaded ^p ^ átezp compliance in particular mineral oil, polyglycol (e.g., polyoxyethylene or polyglytolpolyoxypropylen) further potyeste ^ ^P r ad ^IKL ^ o ^ ^ a ^ LSE or silicone, such as dimethylpolysiloxane.

^{From d} UVO ^chloride in světlenýc ^{h y} are hereinafter mfeen an organic liquid component and a sulfonate-oxide of the same metal which is present in the sulfonate: u.

A large number of experiments have been carried out to determine the optimum degree of basicity of the sulfonates to obtain good thickening ability.

For practical purposes, when determining the optimum degree of alkalinity for the best thickening ability, it is necessary to uv ^ ^ om that while the technical center including ^{the Capital sneeze} charakteristhc is generally more desirable it ^{harder e s} t ^u stem bazictí ^ ^ ucts are; which has ^j í í higher ^with a degree ^of basicity of ekonomrnkého toedisto ^pickle and ^E i ^width. Now ^y in accordance with the above ^{Uve e} d Nym is generally the largest width ^{h j} odně stitedm basicity value.

^{Vol Y o} ies basicity means ^that iiěkteré teiara ^ enstteto VTA-stoostí ZTE ^ ujg e.g. ^example tod spotted onto ATE other vlastoo ^ i ^mo h ^{ou be} in that direction less US ^ ko ^ v ^ ^to pnktad ly ^from Nost thickening.

^pokud se^concerns m °^medicineat^lO^!in^E weight «^-olefms used for production^bin sulphonates, there is about^becn^E siteace such^, The lower fraction of napnktads C12 to C11^poskytuj^and thicken^ovadla^,which^Nothey are in^ždy zceta uspotojwá from behold^diska resistance to separation^Ole^Yippee mm^{ziva while} fraction o v^higher mo^lekulov^E wt C20 to C24 are directed to the production of lithium^1, at. whose^pWhen used, a solid lubricant having a net weight of approx^Enet^racand.

The preparation of the solid lubricant after ^dL e indicated in ^y nátezu spomvá in that ^ the mixed liquid lubricant selected from mineral oils, polyglycols, being preferred polyglycol is polyglykolpolyoxypropylen, esters, and the preferred ester is dioctyl sebacate, silicones, the preferred the silicone is dimethylpolysiloxane, with the metal sulfonate II. or III. groups of the periodic table, wherein said sulfonate containing 12 to 24 carbon and exhibits increased alkalinity expressed excess alkali metal ions corresponding to 20 to 90 .miligramům potassium hydroxide per gram of said sulfonate and said sulfonate is present in the mixture · amount ranging from 5 ^s % to about ^40% based on the total weight of the sulfonate and liquid lubricant, wherein said treatment is conducted at a temperature ranging from 15 to 50 ° C, and the sulfonate and ^k and ^p alnýni mazhem is equal Ito ^to YSL ^IR jj same tov ^ which is present in the ^sulphonate.

Without otoedu ^whether b ^yl adhered 'desired degree ^of bases ^ MUTE ^b yl ^sulfone he ^ate heated in ^ with the presence of nejnteně is ^d Noho ^you Kav ^Star him ^{of solvent} under AA in the ^d or pndání ales ^p he often thickened ^br fovan ^{s k} and ^p ahte hundred ^{of z} to ^y (or other Neto ^g AMC ^Ké topaliny) ^R ° zpou ^{width of} tedta evaporated to eno ztytek which is C ^o in drotien intenztemmu mtetí tolotomm ml ^ý nu or otherwise drop the APAR ^ATURA e.

Description given in p^yn^álezu se vztatoje k tu^hLubricants from d^atwater of its in^elké commercial^dimportance^and, Ata is rubbing them^band you uv^ìdO^mthat most^postup^at uve^denýc^h in a relationship^UKhere^hThe lubricants are apl^ikoin^{atelná i} n^{- for}huš Or^Gand nothing^toýc^h topalm.

In násletajfcrn herein either ^{dou given} y pnklad ^y tu ^H yc ^H vernix caseosa Come ^{loan E} Day it ^at y ⁿ Alez and methods for their preparation, which illustrate Uve ^d said preceding ^y n ^and lies AMZ would ^j ej j ^if ýmtol ^iv way limit . ^The HTO ^ec t p l ^{RIK the institutions as}

Ί 8 it should be noted that the procedure in one case is similar to the previous one, taking into account that, despite the specific differences, these examples are identical quantitatively and qualitatively under the conditions of preparation.

In these examples, it is also shown that when using C15-C18 crolefins and a mixture of fractions having a lower molecular weight and a higher molecular weight fraction than the range of 15 to 18 carbon atoms, for the preparation of lubricating agents of the fats according to the invention, equally satisfactory results can be obtained.

Example 1

In this example, 200 g of calcium monosulfonate from an α-olefinic C 15 -C 18 mixture is mixed with 500 grams of toluene and heated to reflux for 30 minutes. Thereafter, the thus treated mixture was heated under reflux was added 800 g of mineral oil (mainly naphthenic component with a viscosity at 50 ° C ^C E 8.75 and a viscosity index of 60), and then the added solvent, i.e., toluene removed by evaporation.

The product thus obtained is homogenized in a colloid mill until the desired consistency is achieved.

The main characteristics of the obtained product were as follows:

initial penetration 250 dmm penetration after 60 dvojzdvizích 255 dmm penetration of 100,000 dvojzdvizích 295 dmm drop point ASTM 235 Noc: 2 ° C

Example 3

In this example, 20 g of calcium oxide powder is mixed with 300 ml of methanol with vigorous stirring. Carbon dioxide is added to the resulting mixture, whereby an athermic reaction takes place with subsequent formation of a gelatin product.

Separately, 160 grams of calcium monosulfonate obtained from monosulfonic acid of an α-olefinic mixture containing 15 to 18 carbon atoms is dispersed in 600 cm ^{3 of} toluene, and the mixture is then heated under reflux for 30 minutes, after which the mixture is cooled and is placed in a container containing calcium oxide. The increased basicity, expressed as an excess of alkaline ions, is 20 in this case (basicity measured in milligrams of KOH per gm of sulfonate).

The resulting mixture was homogenized and bubbled through carbon dioxide for 30 minutes.

At the end of this interval, distillation of the solvents used (methanol and toluene) is started, with 200 grams of mineral oil (a mixture containing 25% paraffin oil and 75% naphthenic oil similar to Example 1), the paraffin oil having a viscosity at 50 °. 30 ° E and a viscosity index of 95, and a paraffinic oil having a viscosity of 8.75 ° E and a viscosity index of 60) at the same temperatures.

After removal of the solvents, the product was homogenized in a colloid mill while slowly adding an additional 600 grams of mineral oil. The resulting lubricating grease had a perfectly homogeneous short-fiber appearance and was almost transparent.

The main characteristics of the product thus obtained were as follows:

In these cases, ASTM means that the drop point was determined in accordance with ASTM D 566-64. The penetration determination was made according to ASTM D 217-68.

Example 2

The procedure of this example is similar to that of Example 1 except that an equal weight amount of calcium disulfonate from the same α-olefinic fraction containing 15 to 18 carbon atoms was used instead of calcium monosulfonate. The mineral oil used was the same as in Example 1.

The main characteristics of the product were as follows:

initial penetration 270 dmm penetration after 60 dvojzdvizích 275 dmm penetration of 100,000 dvojzdvizích 320 dmm drop point ASTM 220 DEG

initial penetration 265 dmm penetration after 60 dvojzdvizích 265 dmm penetration of 100,000 dmm dvojzdvizích 300 drop point 260 ^C C

Example 4

The procedure was similar to that described in Example 1 except that 200 grams of calcium alkylene monosulfonate was replaced by 200 grams of calcium alkylene disulfonate.

The main characteristics of the final product are as follows:

initial penetration 250 dmm penetration after 60 dvojzdvizích 260 dmm penetration of 100,000 dvojzdvizích 255 dmih

Example 5

The method of this embodiment is analogous to that of Example 1, the only difference is in the replacement of 800 g of a mineral oil per 800 g of silicone fluids it vistoztě ^s p ^s tepteto otol ⁵⁰ ° C 8 ° E.

The ductile characteristics of the resulting grease are as follows:

^Hl AVN ^Typical Properties ^TX tedn ^eh the bow ly up followed ^{by d j} u ICI:

initial penetration 250 dmm penetration after 60 double strokes 250dmm penetration after 100 000 double strokes 285dmm drop point ASTM 210 ° C

Example 9 Initial Penetration Penetration after 60 Double-Penetrations Penetration after 100,000 Double-Penetration ASTM Drop-Point

Example 6

230 dmm

230 dmm 3 dmm

250 ^° C

The procedure of this example is similar to that of Example 1 except that the mineral oil is replaced with an equal amount of liquid silicone and the calcium mercapto-sulphonate of an olefinic mixture of 15 to 18 carbon atoms is replaced with the same amount of calcium disulfonate of the same said olefinic mixtures.

The main characteristics of the grease according to this example are as follows:

initial penetration 240 dmm penetration after 60 dvojzdvizích 245 dmm penetration of 100,000 dvojzdvizích 280 dmm drop point ASTM 200 C

Example 7

The procedure of this example is similar to that of Example 1, except that the mineral oil is replaced by an equal amount of polyglycol with a viscosity at 50 ° C to 6 ° C.

The main characteristics of the resulting grease are as follows:

initial penetration 250 dmm penetration after 60 double strokes 230dmm penetration after 100 000 double strokes 285dmm drop point ASTM 258 ° C

Example 8

The procedure of this example is the same as that of Example 1, except that the monosulfonate is used instead. Here calcium was used disulfonate calcium from alpha-olefin fractions having 15 to 18 carbon atoms, and the mineral oil was replaced by ^p ol ol ^yglyk vistozitou s at 50 ° C of about 6 ° E.

^P rocedure ^{dl p} o ^p e personal identification přftladu Roveda is analogous to that of Example 1, except that in this embodiment replace ^says minerálrn oil microcapsules ^h motnostním same amount of synthetic liquid lubricants ^Ba zi oiktylseMtotu and olktyíipátu.

The main characteristics of the resulting solid lubricant are as follows:

initial penetration 200 dmm penetration after 60 double strokes 200dmm penetration pa 100 030 double strokes 230dmm drop point ASTM 250 ° C

Example 10

The procedure for preparing the lubricating fat in this example is similar to that described in Example 1, except that the calcium monosulfonate from the α-olefinic C 15 -C 18 mixture is replaced by the same amount of the corresponding disulfonate, and also in this example embodiment is applied ^to a synthetic apaln ^eh mazwa on the MZI and oktylsebakátu oktyladipátu.

The main characteristics of the obtained grease are as follows:

initial penetration 240 dmm penetration after 60 dvojzdvizích 250 dmm penetration of 100,000 dvojzdvizích 285 dmm drop point ASTM 245 Noc: 2 ° C

Example 1 a d 11

According to this exemplary embodiment, the post ^P U is such that ^{80 g} IxysličnPku calcium powder mixed with vigorous stirring with 300 ml of methanol was bubbled with carbon dioxide. A geothermal product is formed upon e.othermic reaction.

Separately, 40 g of calcium monosulfonate derived from an α-olefinic mixture containing 15 to 18 carbon atoms is dispersed in 600 ml of toluene. Increased alkalinity vyjá ^d REN ^and řebytkem and ^{p! Alice to} ACTIVE ions ^b y ^l, and in this case 80 (measured in milligrams h ^yd drasehteho butyl hydroperoxide per ^g ram s ^u l t ^{u fon).}

220300

The dispersion is then heated under reflux for 30 minutes, then cooled and the entire contents are placed in a container containing calcium oxide. The mixture was homogenized and bubbled through carbon dioxide for 30 minutes. At the end of this interval, the solvent (methanol and toluene) was distilled off and 200 g of mineral oil (naphthenic raffinate and solvent) were added to the mixture.

The mineral oil viscosity is 2.8 Έ at 50 ^° C and the viscosity index is 40.

After removal of the solvents, the product was homogenized 6 times in a colloid mill with a slow addition of an additional 600 g of said mineral oil.

The resulting grease had the appearance of short fibers and was almost transparent. The main characteristics obtained for the product were as follows:

initial penetration 280 dmm penetration after 60 dvojzdvizích 285 dmm penetration of 100,000 dvojzdvizích 340 dmm ASTM drop point greater than 250 C

Example 12 and a viscosity index of 95 and a naphthenic oil had a viscosity of 8.75 visk and a viscosity index of 60.

The main characteristics of the resulting grease were as follows:

initial penetration 270 dmm penetration after 60 double strokes 2 -5 dmm penetration after 100 003 double-stroke 295 dmm drop point ASTM greater than 250 ² C

Example 14

The procedure of this example is similar to the procedure for preparing the max fat according to Example 13 except that the disulfonate is used in place of the monosulfonate. The mineral oil in this example was the same as in Example 3; same as in the pre-chord example.

The main characteristics of the resulting grease were as follows:

initial penetration 290 dmm penetration after 60 double strokes 295 dmm penetration after 109 090 double strokes 350 dmm drop point ASTM greater than 250 ^? C

The process for preparing the lubricating grease of the present invention is similar to that of Example 11, except that the same amount of calcium disulphonate is used in place of the monosulphonate in this example.

The mineral oil used was the same oil as in Example 11, i.e. naphthenic raffinate with a viscosity solvent

3.8 ° E at temperature and viscosity index 40.

The main characteristics of the grease according to this example were as follows:

initial penetration 300 dmm penetration after 60 double strokes 310 dmm penetration after 100 000 double strokes 360 dmm ASTM drop point greater than 250 ° C

Example 13

The procedure of this example is similar to that of Example 3, except that other quantitative amounts of ingredients are used in this example. In this process, 70 g of calcium oxide, 60 g of calcium monosulfonate (increased alkalinity in this case 70 mg of potassium hydroxide per gram of sulfonate), and 800 g of mineral oil, which in this embodiment was the same as in Example 3, were used. means a mixture containing 25% paraffin oil and 75% naphthenic oil, the paraffin oil having a viscosity of 30 ° E at 50 ° C

Example 15

The procedure of this example is similar to that of Example 13 except that the same amount of dimethylpolysiloane is used instead of mineral oil. The main characteristics of the obtained grease are as follows:

initial penetration 280 dmm penetration after 60 dvojzdvizích 285 dmm penetration of 100,000 dvojzdvizích 350 dmm

ASTM drop point greater than 250 ° C

Example 1 a d 16

The procedure of this example was similar to that of Example 11. except that the mineral oil was replaced with phenylmethylpolysiloan.

The main characteristics of the obtained grease are as follows:

initial penetration 300 dmm penetration after 60 dvojzdvizích 310 dmm penetration of 100,000 dvojzdvizích 380 dmm

ASTM drop point greater than 250 ° C

Example 17

The procedure of this embodiment is

14 was similar to that of Example 14, except that the mineral oil was replaced with an equal amount of polyethylene glycol in this case.

The main characteristics of the resulting grease are as follows:

initial penetration 300 dmm penetration after 60 dvojzdvizích 310 dmm penetration of 100,000 dvojzdvizích 380 dmm

ASTM drop point greater than 250 ° C

Example 18

The procedure of this example is similar to that of Example 14, except that in this case the mineral oil is replaced with an equal amount of polyglycol polyoxyethylene.

The main characteristics of the resulting grease were as follows:

initial penetration 280 dmm penetration after 60 dvojzdvizích 320 dmm penetration of 100,000 dvojzdvizích 390 dmm

ASTM drop point greater than 250 ° C

Example 19

The procedure of this example is similar to that of Example 13, except that the mineral oil is replaced by an equal amount of dioctyl sebacate in this example.

The main characteristics of the obtained grease are as follows:

initial penetration 230 dmm penetration after 60 dvojzdvizích 320 dmm penetration of 100,000 dvojzdvizích 395 dmm

ASTM drop point greater than 230 ° C

Example 20

The procedure of this example is the same as that of Example 14, except that the mineral oil was replaced with diisobutyl adipate as a liquid lubricant in this case.

The main characteristics of the obtained grease were as follows:

initial penetration 310 dmm penetration after 60 dvojzdvizích 320 dmm penetration of 100,000 dvojzdvizích 395 dmm

ASTM drop point greater than 200 ^° C

Example 21

120 g of barium hydroxide octahydrate Ba (OH) 2 are used. . 8 H 2 O dispersed in 300 ml of anhydrous methanol in crushed form. Carbon dioxide was bubbled through the mixture for 30 minutes. To this barium hydroxide dispersion is added a mixture consisting of 80 g of barium monosulfonate with an olefinic mixture of 14 to 18 carbon atoms in 400 ml of toluene. The increased basicity in this case is 30 (basicity in milligrams of potassium hydroxide per gram of sulfonate). Carbon dioxide was then bubbled through the mixture. Subsequently, solvents (methanol and toluene) were removed from the mixture. 300 g of naphthenic mineral oil having a viscosity of 8 ^{DEG C.} at 50 ^DEG C. were then added to the mixture with stirring. The mixture was stirred and the solvents were distilled off. After multiple grinding in a colloid mill, a homogeneous paste was obtained, with an additional 300 grams of mineral naphthenic oil (specified above) being added gradually.

The main characteristics of the resulting grease are as follows:

initial penetration 280 dmm penetration after 60 double strokes 290 dmm penetration after 100 000 double strokes 340 dmm drop point ASTM greater than 250 ° C

Example 1 a d 22

200 g of magnesium monosulfonate from an a-olefinic mixture of 14 to 16 carbon atoms are mixed with 500 ml of toluene. The resulting mixture was heated to reflux for 30 minutes.

A dispersion of 30 g of magnesium oxide in 200 ml of anhydrous methanol is then added to the refluxing mixture. This dispersion was obtained by vigorously mixing the 200 mesh screen. The resulting mixture is then heated to boiling with bubbling carbon dioxide. After one hour, evaporation of the solvents was started.

When about half of the solvents were distilled off, 200 g of naphthenic oil having a viscosity of 8 ° at 50 ° C was added, and the solvent mixture was distilled off completely. After the solvents have been distilled off, the product is ground in a colloid mill, 200 g of naphthenic mineral oil is added gradually.

This procedure produces a grease that is translucent and has a penetration value of 290 to 300 dmm. The drop point in this case is approximately 240 ° C.

The lubricating grease prepared in this way has excellent anti-corrosive characteristics.

Example 23

According to this exemplary embodiment, 200 grams of zinc oxide disulfonate α-olefin SMe ^about bsahuj ^I or ^the 15 and the 18 ^F atoms ^at SMTA shutting up with 300 ml of toluene under reflux to obtain a dispersion. Increased alkalinity expressed excess alkaHc ^to YC шпШ ^H in this beta ^Rip ad ^E 30 ^(N UMBER mihgramů sultonátu KOH per gram). Do this ^for the processing ^e mixture can then ^{in di- p} ersion with zinc oxide in methanol, which had been bubbled through for half an hour at kysličn ^CART em ^hliči team. Outlet mixture. ^p Otom is heated ^to boiling under vigorous stirring and bubbling carbon dioxide. After evaporating half of the solvents, 200 g of a mineral oil having a viscosity of approximately 8 DEG C. at 50 ^DEG C. are added.

The mixture is then vigorously stirred to evaporate all solvent used. Then 200 g of mineral oil (naphthenic oil as in the previous example) is added to this mixture and the resulting product is homogenized in a colloid mill to obtain products of the desired consistency. wear and drop point around 200 ° C.

Example 24

According to this embodiment is allowed to react 100 g of aluminum isopropoxide with 200 g of alumina monosulfonate wolefimc obsahujp ^to a mixture of ¹⁵ to ¹⁸ atom ^of carbon, and the mixture is dissolved in 500 ml of toluene.

This mixture was heated for the next probubfévám ^alkyl sHčn ^Cart uMféhým em. ^p oo ^d pa em half the amount ^of solvent was added 250 g of mineral oil (naphthenic oil as well as in the previous example, having a viscosity in the range of ^7-8 ° ^E pn toptoto ⁵⁰ ° ^C].

The solvent is then distilled off with vigorous stirring. The resulting paste is tomogenized several times with an additional 200 g of the same oil.

The so obtained grease has a density vyjá ^{f p} enou enetram ^{290 further} exhibits e ^{d b} of drilled and ^dh ^ ezní sctopno and hair dryer ^for about ou ^d olnost ^teaches the load

Example 25

In this example, 30 g is suspended in anhydrous metoylate. ^Z and vigorous stirring, the suspension leaving ^{the P} ro ^b u ^{t bl} juice of ^{half an hour} in ^{d y} ^ sběrákem ^no carbon dioxide. ^When the exothermic reaction is carried out, a gelatinous product is formed. Do this for ^the u ^{d p} is the Otom for neustMého mícMní ргШа ^D is ^p ersion monosultonMu weighing ^{140 g p} ENAT ^eh oz α-olefin mixture containing 20 to 24 carbon in ³⁰⁰ ml uMfau tohienu. ^From increased to substantial excess alkalinity expressed alkaline Tonti. in this ice ^{comm 2} 0 (m eno ^measured in milligrams of potassium hydroxide per gram sultonátu). Be mícMní b ^{h em-yl,} and the mixture ^P ro ^b ublávána carbon dioxide. The mixture was then heated to give a white powder after evaporation of the solvent. Then, 20 ^parts by weight ^of a ^{p h} oto r ^ASK uv ^h omo ^g enizovaném state mixed with 80 parts of a naphthenic mineral oil having a viscosity in the range of 7 to ⁸ ° ^{E p} n ^t e ^{pl I} of ⁵⁰ ° C. ^Those of ^P MTO Úsobí grease is obtained with a good consistency, which becomes a semiliquid during mixing and thickens when the stirring was continued. This phenomenon was repeated many times. This lubricant ^to herein could najft ^ atóctou usage in devices with a central lubrication.

Example 26

According to this example, 120 g of calcium monosuhonate from an α-olefinic C 12 -C 14 mixture is dispersed in 300 ml of toluene while heating under reflux.

Then, 40 g of anhydrous calcium oxide dispersed in 300 ml of anhydrous methyl ^{ethyl ta} and ^h o u ^{l d p} is the ^p erzí Otom half ^hour Odin bubbled carbon dioxide.

The two dispersions are then mixed, and the mixture is heated while bubbling another portion of carbon dioxide. After removing the solvent then bui ^{l d} e r Nu ^{P and} Se ^to tomogenizuje. The PR ^and check the ^p Otom in Fifejdy City Hospital ^25% by weight, homogenized with mineral oil (naphthenic) of viskozltě in the range of 7 to ⁸ ° ^{E p} ri te ^pl OTE ^{50 C} C ^BC and ^no EMZ gains ^and grease consistency expressed penetration 270 dmm and drop point 220 ° C.

Example 27

According to this embodiment, 80 g of calcium monosulfonate are in the form of a mixture of assemblies. ^ bhžně ^50% monosultonMu phosphate from α-olefin mixture containing ¹² to 14 atoms ^at uMíh and ^p nbližně of ⁵ 0% monosuhonMu ^AP enoate ^h oz alpha ^olefin MC ^to Star mixture ^of about ^B sahuj ^I C ^{s 20} to ²⁴ atom ^at uW ^ u, ^{P di} of ³⁰⁰ ergs of milHitre ^ pn toluene refluxing.

Separately dispersed 60 g of calcium oxide powder in anhydrous ^{methylcarbazole} and ^{ta h} o u ^{l d p} is erzí for mtonzwntoo ^p ROMs ^and c ^{ha ck p} robub ^la weighing ^P UL hours ^{ky y} sličník dioxide.

The two dispersions are then mixed and the resulting mixture is heated and bubbled through with carbon dioxide. After removal of the extended ^P Oust ^EDL and the obtained ^P r ^and SEQ ^h omo emzuje ^{g. In d} and ^LSI m with ²⁵ parts of ^H motnostníc ^h personal identification imask ^h a homogenized with ^{75 parts} minerMntoo oil (naphthenic oil) having a viscosity in the range of 7 to 8 Έ at 50 ° C to give a grease with the following characteristics:

Initial Penetration Penetration after 60 Double Penetrations Penetration after 100,000 Double Penetration Drop Point ASTM

Example 28

300 dmm

305 dmm

350 dmm

220 DEG

According to this example, the following basic mixture is homogenized (in percent by weight):

white zinc (zinc oxide5 yellow zinc (zinc chromate) 11 red lead (lead) 38 red iron oxide (iron oxide) 0.61 asbestos 5.3 "long oil" glycerophthal resin (contains 60% non-volatile substances) 27 pulp [25 % of basic sulfonate in mineral resin] 2 dehydrating agents1,72 mineral resin9,37

After 10 days, no settling was observed in this mixture. This mixture is suitable for a colored substrate. Further tests were performed using the same components but at a different percentage. These mixtures were compared to a sulphonate-free mixture. It is noted that the sulfonate-free compositions had significant amounts of deposits after the same time, while 0.5% of the sulfonate reduced the amount of deposits to one fifth.

Claims (4)

Lubricating grease, characterized in that it consists of a liquid lubricant in an amount ranging from 60% to 95% by weight, selected from the group consisting of mineral oils, polyglycols, said polyglycol being preferably polyglycol polyoxypropylene esters, said ester is preferably dioctyl sebacate, Silicones, wherein said silicone is preferably dimethylpolysiloxane, and of metal sulfonate II. or III. said sulfonate being a 12 to 24 carbon atom sulfonate, said sulfonates having an increased alkalinity in excess of alkali ions corresponding to 20 to 90 milligrams of potassium hydroxide per gram of said sulfonate; sulfonate. 2. The grease of claim 1 wherein said metal from which the sulfonate is derived is selected from the group consisting of alkaline earth metals, zinc, and aluminum. 3. The grease of claim 1, wherein said mineral oil has a viscosity in the range of viscosity grades characterized by a viscosity of at most 1300 mm ^{< 1 > * *} / s at a temperature of -17.8 ° C to viscosity grades of viscosity. in the range of 25 to 43 mm ² / s at 98 ° C, the freezing point is less than 30 ^° C and the flash point is at least 150 ° C. 4. The grease of claim 1, wherein said polyglycols, esters and silicones have a viscosity ranging from 6.3x10 ⁶ m ² / s to 1.52x10 ^-4 m ² / s at 50 ^{° C.} C while remaining liquid at temperatures below -20 ° C, while exhibiting a high oxidation resistance according to ASTM D 942, which means that the pressure drop during the 100 hour test is less than 20.7 kPa.