RU1836411C - Method for obtaining the concentrate of an additive to lubricating oils - Google Patents

Description

metal cyclates, wherein the metal is an alkaline earth metal, e.g. calcium, magnesium or barium. Both normal and superbasic alkaline earth metal bicarbonate sadicylates were used. The term "superbasic" is used to denote such a hydrocarbon radical substituted alkaline earth metal salicylate in which the ratio of the number of alkaline earth metal equivalents to the number of equivalents of the salicylate residue is greater than one, usually greater than 1.2. and can reach 4.5 or more. On the contrary, the ratio of equivalents of alkaline earth metal and salicylate residue to normal hydrocarbon radical-substituted salicylates is equal to one. Thus, an overbased compound typically contains more than 20% excess alkaline earth metal compared to the corresponding normal compound. As a result, overbased alkaline earth metal salicylates substituted with a hydrocarbon radical have an increased ability to neutralize acidic compounds compared with the corresponding normal alkaline earth metal salicylates substituted with a hydrocarbon radical.

The state of the art provides a number of methods for the preparation of both normal and overbased metal salicylates substituted with hydrocarbon radicals,

The use of carboxylic acids in the preparation of hydrocarbon-substituted alkaline earth metal salicylates and their sulfur-containing derivatives is not new.

A known method of producing salicylate of a base metal, which includes a reaction at a temperature of from 25 ° C to a boiling point between: (A) a hydrocarbon radical substituted with salicylic acid, a substituent of which contains at least 6 carbon atoms, a mixture of the specified salicylic acid with no more than equivalent the amount of succinic acid substituted by a hydrocarbon radical or its anhydride having a substituent with at least 6 carbon atoms, or a completely neutral salt of an alkali or alkaline earth metal one of the above acids; (B) 1-10 equivalents per equivalent (A) of calcium or strontium base; and (C) carbon dioxide, in the presence of 0.002-0.2

equivalents, per equivalent of said base of calcium or strontium, a carboxylic acid containing up to 100 carbon atoms, or a salt thereof with an alkali metal, alkaline earth metal, zinc or lead. Preferred carboxylic acids of the latter are those with up to 10 carbon atoms: of which, particular attention is paid to acetic acid. The only carboxylic acid exemplified is acetic acid.

A known method of producing a detergent additive for lubricating oils, which is the main sulphide alkaline earth metal alkyl salicylate by reacting at an elevated temperature a component that is a mineral oil, which is

0 alkyl substituted salicylic acid or its salt, sulfur, alkaline earth metal base, component representing one of the following compounds or a mixture thereof: a compound of general formula R (QRi) xOH, where R is hydrogen, () is alkyl, RI is alkylene, x is at least 1; alcohols, esters, ketones, and calcium chlorides, followed by distillation and filtration steps,

0 The current level of technology in which carboxylic acids are used does not concern the problem of producing concentrated additives containing overbased hydrocarbon substituted

5 by alkaline earth metal salicylates having a TBN of more than 300 and an acceptable viscosity.

From the foregoing, it is clear that it would be desirable to obtain a concentrated

0 additive containing alkaline earth metal salicylates substituted by a hydrocarbon radical or their sulfur-containing derivatives having high TBN, namely more than 300, preferably more

5,350, while retaining acceptable viscosity.

Accordingly, the present invention provides a method for producing a concentrated lubricant additive,

0 having a TBN of more than 300, which includes a reaction at an elevated temperature between: °.

component (A), which is at least one of the following 5 compounds: () a hydrocarbon radical substituted alkaline earth metal salicylate, (II) a hydrocarbon radical substituted salicylic acid, (III) a hydrocarbon radical substituted alkaline earth metal salicylate and a sulfur source,

(IV) a hydrocarbon radical substituted salicylic acid and a sulfur source,

(V) a sulfur-containing derivative of a hydrocarbon radical substituted with an alkaline earth metal salicylate, (VI) a sulfur-containing derivative of a substituted hydrocarbon radical of salicylic acid;

component (B), which is an alkaline earth metal base, added either once or in portions during the reaction;

component (C), which is at least one compound of the following: (I) water, (II) a polyhydric alcohol with a number of carbon atoms from 2 to 4, (III) -di- (C3 or Gi) glycol, (/ ) three (C2-CO glycol, (V) ether of a monohydric alcohol and mono- or polyalkylene glycol of the formula

R (ORi) xOR2,

(ABOUT

where R is an alkyl group with carbon atoms from 6 to 6, RI is an alkylene group, R2 is hydrogen or an alkyl group with carbon atoms from 1 to 6, x is an integer from 1 to 6, (VI) a monohydric alcohol with a number of atoms carbon from 1 to 20, (VJt) ketone with the number of carbon atoms from 1 to 20, (VIII). an ester of a carboxylic acid having from 1 to 10 carbon atoms, or (IX) an ether with a number of carbon atoms from 1 to 20;

component (D), which is a lubricating oil;

component (E). which is carbon dioxide added after the addition (of a single or each of the portions) of component (B);

component (F), capable of providing from 2 to 40% by weight of the concentrate and representing at least one of the following: (I) a carboxylic acid or its anhydride, chlorohydride or ester, wherein said acid has the formula

R3-CH-COOH, RC

(YU

where Ra is an alkyl or alkenyl group with a carbon number of 10 to 24, R4 is hydrogen, an alkyl group with a carbon number of 1 to 4, or a CH2COOH group, or (P) a di- or poly-carboxylic acid with a number carbon atoms from 36 to 100, or anhydride,

the acid chloride or ester of the specified acid;

components (G), which is at least one of the following compounds: (I) an inorganic halide. or (II) ammonium alkanoate or mono-, di-, tri- or tetraalkylammonium formate or alkonoate, provided that when component (G) is (II), component (F) is not an acid chloride;

the weight ratios of all components are such as to obtain a concentrate having a TBN of more than 300.

5 Component (A) of the reaction mixture is (I) a hydrocarbon radical-substituted alkaline earth metal salicylate, (II) a hydrocarbon-radical-substituted salicylic acid,

0 (III) a hydrocarbon radical-substituted alkaline earth metal salicylate and a sulfur source, (IV) a hydrocarbon-radical-substituted salicylic acid and a sulfur source, (V) a sulfur-containing derivative of an alkaline earth metal-substituted salicylate, (VI) a sulfur-containing derivative of a substituted hydrocarbon radical of salicylic acid, or a mixture of at least two compounds (A (l) - A (VI)).

When using component A () or component A (P), the final product contains an alkaline earth salicylate substituted with a hydrocarbon radical

5 metal, and when using components A (W). A (lV), A (V) or A (VI) the final product contains a sulfur-containing derivative of an alkaline earth metal salicylate substituted with a hydrocarbon radical.

0 Typically, the alkaline earth metal may be strontium, calcium, magnesium or barium, preferably calcium, barium or magnesium, more preferably calcium, although it is possible to use as

5 of the initial component A (P) -salicylic acid substituted with a hydrocarbon radical. (A) (Y) -substituted with a hydrocarbon radical, salicylic acid and a sulfur source, for example elemental sulfur,

0 sulfur monohalide or sulfur dihalide, or (A) (Y1) -sulfur derivative substituted by a hydrocarbon radical of salicylic acid, it is preferable to use (A) (I), (A) (III) or (A) (V), i.e.

5 to increase the initial content of an alkaline earth metal salicylate substituted by a hydrocarbon radical or a sulfur-containing salicylate derivative. In this way, you can increase the content of both neutral and

superbasic salicylates. It is also possible to increase the content of a mixture of neutral salicylates and salicylic acids. In this case, salicylates and / or salicylic acids may contain sulfur or may be mixed with a sulfur source.

A hydrocarbon substituent of a salicylate substituted with a hydrocarbon radical and a salicylic acid substituted with a hydrocarbon radical and their sulfur-containing derivatives may contain up to 125 aliphatic carbon atoms. Examples of common substituents are cerebral radicals, for example hexyl, cyclohexy, octyl, isooctyl, decyl, tridecyl, hexadecyl, eicosyl and tricosyl; radicals obtained by the polymerization of olefins with both terminal and internal double bonds, for example ethylene, propylene, butene-1, isobutylene, hexene-1-octene-1, butene-2, pentene-2, pentene-3 and octene- 4. A preferred hydrocarbon substituent is a substituent derived from a monoolefin, more preferably from the following monoolefins: propylene, butene-1 or isobutylene.

The alkaline earth metal base (component B) may typically be an alkaline earth metal oxide or hydroxide, preferably hydroxide. For example, calcium can be added as quicklime (CaO) or as quicklime (Ca (OH) a). Preferred alkaline earth metals are calcium, magnesium, strontium and barium, preferably calcium. The alkaline earth metal base should be added in such an amount with respect to component (A) that is sufficient to obtain a product with TBN greater than 300, preferably more than 350. This amount depends on a number of factors, including the following: contains or not component (A ) any amount of alkaline earth metal base, the nature of the hydrocarbon substituent, and exceeds the amounts used in the methods of the state of the art. Typically, the mass ratio of component. {B} to component (A) may range from 0.2 to 50, preferably from 0.4 to Yu.

Component (B) can be added entirely to the starting reagents at the beginning of the reaction, or a part can be added to the starting reagents, and the remaining amount can be added in one or several portions in a subsequent stage or stages of the process.

It is preferable to add component (B) by a single addition.

As component (C), one or more polar organic compounds or water, or mixtures thereof can be used; it is preferable to use a polar organic compound.

Suitable compounds of formula (1) include monomethyl or dimethyl ethers (a) ethylene glycol, (b) diethylene glycol, (c) triethylene glycol or (d) tetraethylene glycol. A particularly suitable compound is methyl diglycol (CH3COCH2CH20CH2CH20H). Mixtures of glycol ethers of the formula (I) and glycols may also be used. When a glycol of formula (I) or glycol is used as component (C) of an ether, it is preferable to use an inorganic halogen, for example ammonium chloride, and a lower carboxylic acid, for example acetic acid, with 1 to 4 carbon atoms . The polyhydric alcohol can usually be either a diatomic alcohol, for example ethylene glycol or propylene glycol, or a trihydric alcohol, for example glycerin. A suitable di- (C3 or CA) glycol may be dipropylene glycol, a suitable tri- (C2-C4) glycol may be triethylene glycol. Preferably component (C) is ethylene glycol or methyldiglycol, the latter in combination with ammonium chloride and acetic acid.

A suitable component (C) may also be a monohydric alcohol with a number of carbon atoms from 1 to 20, a ketone with a number of carbon atoms from 1 to 20, an ester of a carboxylic acid having from 1 to 10, carbon atoms, or an ether with the number of atoms carbon from 1 to 20, and the above compounds may be aliphatic. al-acyclic or

aromatic. Examples are methanol, acetone, 2-ethylhexSanol, cyclohexanol, cyclohexanone, benzyl alcohol, ethyl acetate, acetophenone, preferably 2-ethylhexanol. In a preferred embodiment of the claimed method for producing the concentrate, a combination of (I) component (C) as defined above and (I) a solvent can be used.

An inert hydrocarbon, which can be aliphatic or aromatic, can usually be used as solvent (I). Examples of suitable solvents are toluene, xylene, lacquer gasoline and aliphatic saturated hydrocarbons, e.g. hexane, as well as cycloaliphatic saturated hydrocarbons.

A particularly preferred combination of (I) and (II) is a combination of methanol with toluene. The advantage of using a combination of (I) with (II) is that ethylene glycol can be avoided. Residual ethylene glycol in the lubricating oil additive can cause corrosion of the engine in which the concentrated additive is used.

Component (D) is a lubricating oil. Typically, the lubricating oil is an animal, vegetable or mineral oil. A suitable lubricating oil is a lubricating oil derived from petroleum, for example a naphthenic base, a paraffin base or a mixed base oil. Neutral solvent oils are particularly suitable. Alternatively, the lubricating oil may be a synthetic lubricating oil. Suitable synthetic lubricating oils include synthetic ester lubricating oils, which in turn include double esters, for example dioctyl adicinate, dioctyl sebacinate and tridecyl adipate, or polymeric hydrocarbon lubricating oils, for example liquid polyisobutylene or polyalpha olefins. Lubricating oils can typically comprise from 10 to 90%, preferably from 10 to 70%, by weight of the concentrate.

Component (E) is carbon dioxide that can be added in gaseous: or in solid form, preferably in gaseous form. When supplied in gaseous form, it is convenient to purge it through the reaction mixture. We found that, as a rule, the amount of carbon dioxide introduced increases with increasing concentration of component (F).

Typically, carbon dioxide may be present in the concentrate in combined form in an amount of from 5 to 20, preferably from 9 to 15% by weight of the concentrate.

Component (F) is either (I) a carboxylic acid of formula (II), or (I) di- or polycarboxylic acid with 36 to 100 carbon atoms, or anhydride, acid chloride or ester (1) or (U) . As regards (I), (I) is a carboxylic acid of formula (II) or its anhydride, acid chloride or ester. Preferably Ra is a straight chain alkyl or alkenyl group. Preferred acids of formula (II) are those in

of which R4 represents a hydrogen atom and H3 represents a straight chain alkyl group with carbon numbers from 10 to 24, preferably from 18 to 24. Examples of suitable saturated carboxylic acids of formula (II) include, caproic, lauronic, miri - stonic, palmitic, stearic, isostearic. arachidic, beginic and lignoceric acids. Examples of suitable unsaturated acids of the formula (II) include lauroleic, myristoleic, palmitoleic, oleic, gadoleic, eruschinic. ricinoleic acid, linoleic and linolenic acids. Mixtures of acids can also be used, for example rapeseed higher fatty acids. Particularly suitable mixtures of acids are those produced

0 industry acids, which contain a set of acids, both saturated and unsaturated. Such mixtures can be obtained synthetically or isolated from natural products, for example, from cotton. coconut, peanut, flaxseed, olive, corn, palm, castor, soybean, sunflower, herring, sardine oil, from palm kernel oil and from lard. Sulfur-containing acids and mixtures thereof may also be used. Instead of, or with carboxylic acid, acid anhydride, acid chloride or ester derivatives of the Acid can be used, preferably 5 acid anhydride. However, it is preferable to use a carboxylic acid or a mixture of carboxylic acids. A preferred carboxylic acid of formula (li) is stearic acid.

0 Instead of (I), or in addition to (I), component (F) may be (II) di- or polycarboxylic acid containing from 36 to 100 carbon atoms or its anhydride, x acid hydride or ester, preferably its anhydride; (I.I) is preferably polyisobutylene succinic acid or polyisobutylene succinic anhydride.

Typically, the concentrate may have

0 100 ° C with a viscosity of less than 1000 cSt, preferably less than 750 cSt, more preferably less than 500 cSt,

The amount of component (F) required to obtain from 2 to 40% by weight of the mass

5 of the concentrate, to a first approximation, is the amount whose presence in the concentrate is desired. When calculating this amount, it is necessary to take into account the loss of water, for example from a carboxylic acid.

The reaction is carried out in the presence of component (G). As component (G), it is possible to use (I) an inorganic halide, which can usually be a hydrogen, ammonium or metal halide. Typically, the metal halide moiety may be zinc, aluminum or an alkaline earth metal, preferably calcium. Of the above halides, chloride is preferred. Suitable chlorides include hydrogen chloride, calcium chloride, ammonium chloride, aluminum chloride and zinc chloride, preferably calcium chloride.

Alternatively, component (G) may be (II) ammonium alkanoate or mono-, di-, tri- or tetraalkylammonium formate or alkanoate, preferably ammonium alkanoate, more preferably ammonium acetate.

Component (G) may be a mixture of 0) and (I). However, when component (G) is the above compound (I), component (F) is not an acid chloride.

Typically, the amount of component (G) used can be up to 2.0% by weight of the sum of the concentrate,

Typically, the total amount of alkaline earth metal present in the concentrate is from 10 to 20% by weight of the concentrate.

In the final product, the alkaline earth metal salicylate substituted with a hydrocarbon radical may either contain sulfur or not contain sulfur, preferably not contain sulfur. When it contains sulfur, it may be present in the concentrate in amounts of from 1 to 6%, preferably from 1.5 to 3% by weight of the concentrate.

Preferably, the concentrate has a TBN greater than 350, more preferably more than 400.

Typically, the reaction between components (A) to (G) can be carried out at temperatures from 15 to 200, preferably from 60 to 150 ° C, although the actual temperatures selected for the various stages of the reaction may, if desired, vary. The pressure may be atmospheric below atmospheric or above atmospheric.

The concentrate can be isolated by conventional means, for example by distillation of component (C) or a solvent (if any).

Finally, it is preferable to filter the concentrate thus obtained. As a rule, the method according to

The present invention provides a concentrate having an acceptable viscosity, namely a viscosity of less than 1000 cSt at 100 ° C, and also allows concentrates with a viscosity of less than 750 or 500 cSt at 100 ° C. Such viscosity characteristics of the concentrate represent its advantage, since they facilitate the use (including filtration) of the concentrate. However, it is also possible to obtain concentrates with a viscosity greater than 1000 cSt at 100 ° C, usually at higher TBN levels. Filtering concentrates with such viscosities is a problem that can be solved by adding diluent before removing the filter and removing it after filtration. On the other hand, highly viscous concentrates, such as concentrates,

having a viscosity at 100 ° C of more than 1000 cSt, and also having a high TBN value of, for example, more than 350, can be diluted by the addition of lubricating oil, maintaining TBN at a level of more than 300, and

facilitate filtering in this way.

Alternatively, the concentrate can be centrifuged in the presence of a diluent.

Last distinctive feature

The present invention is that it provides a final lubricating oil composition that includes a lubricating oil and a concentrated lubricating oil additive formulated as

described above.

Preferably, the final lubricating oil composition contains an amount of concentrated additive sufficient to obtain TB N from 0.5 to 120.

The amount of concentrated additive present in the final lubricating oil depends on the nature of its use. Thus, for marine lubricants, the amount of concentrated additive present can usually be sufficient to produce TBNs of 9 to 100, and for lubricants used in automotive engines, the amount of additive can usually be sufficient for

producing TBN from 4 to 20.

The final lubricating oil composition may also include effective amounts of one or more commonly used lubricating oil additives belonging to other types of additives, for example, viscosity index improvers, wear agents, antioxidants, dispersants, corrosion inhibitors and lubricating oil or directly or through a concentrated composition.

In addition to being used as a lubricant additive, a declared concentrated additive may also find application as a fuel additive.

The present invention is further illustrated by the following examples. In all examples, the term TBN (Total Base Number) is used. TBN is expressed in mg KOH / g. measured by ASTMP 2896. In the examples where lime is used, it is present in the form of slaked lime Ca (OH) 2. Viscosities were measured by ASTMP445.

PRI me R 1.

Loading, g:

OSCA 420 (Superbased

industrially produced salicylate):

270 TBN, ex. OSCA Chemical

With. Japan) 230

Lubricating oil

(100 SN) 26

Calcium Chloride 3

Method:

(a) the mixture was heated to 100 ° C and stearic acid (63 g) was added at this temperature,

(b) 2-ethylhexanol (190 g) was added at 100 ° C.

(c) at 120 ° C 7,760 mmHg added lime (66 g),

(d) the mixture was heated to 145 ° C / 500 mm Hg; at these temperatures and pressures ethylene glycol (32 g) was added over 20 minutes,

(e) kept the mixture for 5 min at 145 ° C / 500 mm Hg,

(f) carbon dioxide (56 g) was added at 145 ° C / 1 bar,

(d) the product was distilled at 200 ° C / 10 mm Hg.

(h) the product was filtered. Product mass, g: Crude product 369

Distill T235

The composition of the product after filtration: Calcium 14.22 wt.%

CO211-1 wt.%

TBN .407mg KOH / g

Viscosity at 100 ° C 880 cSt Viscosity at 40 ° C 18 950 cSt

IV236

Stearic acid 17.1 wt.% PRI me R 2 Download, g:

OSCA 405 (industrially produced superbasic salicylate:

175 TBN; ex. OSCA Chemical Co. Japan) 230

Lubricating oil (100 SN) O

Calcium Chloride 4.0

Method:

Steps (a) - (e) of Example 1 were repeated, except for the following: in step (c) instead of 66 g of lime, 76 g was used, in step (d) instead of 32 g of ethylene glycol, 37 g was used and added to for 5 minutes instead of 20 minutes, in step (f), instead of 56 g of carbon dioxide, 76 g was used, and an additional step was added:

(d) added lubricating oil {100 SN) 5 (20 g)

Product masses:

Crude product Not determined

Distill t222 g

The composition of the product after filtration:

0 Calcium 13.3 wt.%

СОа13.4 wt.%

TBN372mg KOH / g

Viscosity at 100 ° C 414 cSt at 40 ° C6625 cSt

5IV220

PRI me R 3. Download, g: OSCA 420 (280 TBN, ex OSCA Chemical Co.) 236

0 Lubricating oil (100 SN) 27

Calcium Chloride 3

Method:

(a) the mixture was heated to 100 ° C and stearic acid was added at this temperature

5 (65 g).

(b) 2-ethylhexanol (299 g) was added at 100 ° C.

(c) at 120 ° C / 700 mmHg, lime (68 g) was added,

0 (d) the mixture was heated to 135 ° C / 500 mm Hg: Ethylene glycol (33 g) was added at these temperatures and pressure over 5 minutes,

(e) the mixture was kept for 5 min 5 at 135 ° C / 500 mm Hg,

(f) carbon dioxide (56 g) was added at 135 ° C / 1 bar,

(d) the product was distilled at 200 ° C / 10 mm Hg.

0 (h) added lubricating oil (SN 100) (20 g),

(I) the product was filtered.

Product masses, g:

Raw Product395

5 Distill T238

The composition of the product after filtration: Calcium 13.6 wt.%

COa 10.5 wt.%

TBN395mg KOH / g

Viscosity at 100 ° C 205 cSt

4012 cSt

163

May 16.5%

230

26 3

at 40 ° C

Willow

Stearic acid

Example 4

Loading, g:

OSCA 420 (280 TBN, ex.

OSCA Chemical Co. Japan)

Lubricating Oil (100 SN)

Ammonium chloride

Method:

(a) the mixture was heated to 100 ° C and stearic acid (63 g) was added at this temperature,

(b) methylene glycol (130 g) and acetic acid (2.0 g) were added at 100 ° C;

(c) at 120 ° C / 700 mmHg, lime (60 g) was added,

(d) heated the mixture to 135 ° C / 500 mm Hg,

(e) the mixture was kept for 5 min at 135 ° C / 500 mm Hg,

(f) carbon dioxide (56 g) was added at 135 ° C / 1 bar,

(d) the product was distilled at 200 ° C / 10 mm Hg,

(h) the product was filtered.

Product masses, g:

Raw Product443

Distill T132

The composition of the product after filtration:

Calcium 13.4 wt.%

C0214.1 wt.%

. TBN 339 mg KOH / g

Viscosity at 100 ° C 315 cSt at 40 ° C 5329 cSt

Willow. 199

Stearic acid 14.2 wt.%

PRI me R 5.

Loading, g:

Shell AC 606 (commercially available overbased salicylate: ex. Shell Chemical Ltd.) 174 TBN; 5.9 wt.% Ca; 0.4 wt.% S:

Viscosity at 100 ° C 24 cSt at 40 ° C 208 cSt

Lime49

Stearic Acid 70

Calcium Chloride 4

2-Ethylhexanol112

Method:

(a) in the process of adding ethylene glycol (36 g), the mixture was heated from 145 ° C to 165 ° C / 700 mm Hg,

(b) the mixture was kept for 1 h at 165 ° C / 700 mm Hg,

(c) carbon dioxide (50 g) was added at 165 ° C / 1 bar,

(d) the mixture was cooled to 135 ° C / 700 mm Hg. and lime (33 g) was added.

(e) a reaction was carried out at 165 ° C / 700 mm Hg. within 1 h

(f) carbon dioxide (25 g) was added; (e) the product was distilled at

210 ° C / 10mmHg,

(p) the product was filtered to obtain 473 g of the product.

The composition of the product after filtration: Calcium 12.0 wt.%

0 S0.3 wt.%

C0211.8 wt.%

TBN335mg KOH / g

Viscosity at 100 ° C 154 cSt at 40 ° C 2008 cSt

5 IV186

Stearic acid 14.8 wt.%

Example

Loading, g:

OSCA 420 (see example 1} 230.0

0 stearic acid

(70% purity) 63.0

Lubricating oil (SB 130) 26.0

Calcium Chloride 3.0

Toluene 240.0

5 Methanol 20.0

Method:

(a) the mixture was heated to 60 ° C and carried out the reaction at this temperature,

(b) at 60 ° C / 700 mmHg added from - 0 news (66.0 g),

(c) carbon dioxide (35 g) was added at 60 ° C,

(d) the mixture was distilled at 130 ° C / 10 mm Hg. for 60 minutes

5 (e) the mixture was filtered. Product mass, g: Crude product 350.5

Distill T185.3

The composition of the product after filtration:

0 Calcium 14.6 wt.%

Carbon dioxide 13.9 wt.%

TBN408 mg KOH / g

Viscosity at 100 ° C 678 cSt

at 40 ° C Not determined

5 Stearic acid 18.0 wt.% Example. Loading, g:

OSCA 420 (industrially produced overbased salicylate):

0 280 TBN230

Lubricating oil26

Ammonium Acetate 3

Method:

(a) the loaded mixture was heated to 100 ° C 5 and stearic acid (63 g) was added at this temperature,

(b) 2-ethylhexanol (190 g) was added at 100 ° C.

(c) at 120 ° C / 700 mmHg lime was added (66 g).

(d) the mixture was heated to 145 ° C / 500 mm Hg; at these temperatures and bouts. ethylene glycol (32 g) was added over 20 minutes,

(e) the mixture was kept at 145 ° C / 500 mm Hg. within 5 minutes

{f) carbon dioxide (56 g) was added at 145 ° C / 1 bar,

(d) the product was distilled at 200 ° C / 10 mm Hg,

(h) the product was filtered.

Product masses:

Crude product443 g

The composition of the product after filtration:

Calcium 13.4 wt.%

TBN339mg KOH / g

Viscosity at 100 ° C 315 cSt

LRI40 ° C5329 cSt

Claims (8)

Stearic acid 14.2 wt.% The claims 1. A method of obtaining a concentrate additives for lubricating oils by reacting at elevated temperatures component (A), which is a derivative of silicic acid, component (B), which is an alkaline earth base metal, component (C), which is an oxo-containing organic compound, and component (D), which is a lubricating oil, characterized in that, in order to increase the alkalinity of the additive concentrate and improve its viscosity properties, as component A, salicylic acid or an alkaline earth metal substituted with a hydrocarbon radical, sulfur containing an alkaline earth metal substituted with a hydrocarbon radical, an alkaline earth metal substituted with a hydrocarbon radical and elemental sulfur or sulfur halide substituted with a hydrocarbon radical substituted with a hydrocarbon radical and elemental sulfur, or sulfur halide, or a mixture of at least two of these compounds, as Ve component (C) uses a C2 C4 polyhydric alcohol, di-C3-C3-glycol. tri- (C2-C4) glycol, mono- or polyalkylene glycol alkyl ether of the general formula R (ORi) xOR2, where R-Ci-Ce is alkyl; Rt is alkylene; Ra is hydrogen or (C1-Cb) alkyl:.  a monohydric alcohol or a mixture of at least two of the listed compounds, component (B) is administered once or in several portions during the reaction in a mass ratio to component (A), equal to 0.2-50.0, and the interaction is carried out in the presence of component (E), which is introduced after component (B) and is carbon dioxide, taken in an amount providing the presence of 5-20 wt.% component (E) in concentrate additives, component (F), which is a carboxylic acid of the General formula RC-CH-COOH, "H where Rz-Syu-C24-zalkyl or alkylene; RA is hydrogen and Ci-Cj-alkyl, its anhydride, acid chloride or ester or a mixture of at least two of these compounds, taken in an amount ensuring the presence of 2 -40 wt.% Component (F) in the additive concentrate and component (G), which is an inorganic halide, ammonium alkanoate or mono-, di-, tri- or tetralkylammonium formate and alkanoate or a mixture of at least two of the listed compounds, provided that if component G is one of the listed alkanoates or formates, component F is not with a carboxylic acid chloride, with a mass ratio of all the above components, providing an additive concentrate with an alkaline number above 300. 2. A method according to claim 1, characterized in that component (A) is an alkaline earth metal salicylate substituted with a hydrocarbon radical, an alkaline earth metal salicylate substituted with a hydrocarbon radical, or a mixture thereof. 3. A method according to claim 1 or 2, characterized in that component (G) is a metal halide. 4. The method according to claim 3, wherein the metal halide is calcium chloride. 5. The method of claim 1, wherein component G is ammonium alkanoate or mono-, di-, tri- or tetraalkylammonium formate or alkanoate. 6. The method according to claim 5, wherein the ammonium alkanoate is ammonium acetate. 7. A method according to claim T. characterized in that component (C) is a mono- or polyalkylene glycol ether, component (G) is an inorganic halide and the reaction is carried out in the presence of a C1 C4 carboxylic acid, 183641120 8. The method according to claim 7, characterized in that the halide halide is that component (C) is ammonium chloride and (C 1 -O)) is a carboxylic acid monomethyl ether diethylene glycol, non-aorta is acetic acid.