The method of obtaining metal salts of diesters dithiophosphoric acids

 

(57) Abstract:

The invention relates to a method for Organoelement compounds, which can be used as additives to lubricating oils. Object of the invention is the simplification of the method of producing metal salts of diesters dithiophosphoric acids. The technical problem is solved by a method of obtaining metal salts of diesters dithiophosphoric acids by the interaction of the reactants by heating in a solvent in the presence of a catalyst, in which the reagents are taking elemental phosphorus, and elemental sulfur, aliphatic alcohol, or a mixture of aliphatic alcohols, or a mixture of the substituted phenol and an aliphatic alcohol and an oxide or hydroxide of the metal in a molar ratio 1:(2 - 2,5) : (2 - 3):(0,5 - 0,75) accordingly, the interactions lead to a full conserve phosphorus and upon reaching the pH of the reaction mass is 5.5 to 7.0. As the catalyst used aliphatic, aromatic or cyclic primary, secondary or tertiary amines, amides, thioamides coal or carboxylic acid, or turangalila, or xanthates, or dithiocarbamate, or metal salts of diesters dithiophosphoric acids. As the oxide or hydroxide of the metal barometre diesters dithiophosphoric acids by reducing the labor intensity, environmental pollution, and reduce economic costs. 1 S. and 3 C.p. f-crystals.

The invention relates to a method for elementarnykh compounds which can be used as lubricating oil additives, flotation agents, light stabilizers, accelerators of vulcanization.

A method of obtaining metal salts of diesters dithiophosphoric acids when heated in a solvent in the presence of a catalyst of the main character by the interaction of pentasulfide phosphorus with aliphatic alcohol or with a mixture of aliphatic alcohols or phenol, or substituted phenol, or a mixture of the substituted phenol and alcohol and oxide or hydroxide or hydroxide of the metal in the presence of catalytic amounts of nitrogen-containing compounds C1 group of the formula C(X)-N=, where X is oxygen or sulfur; as catalyst using N - vinyl pyrrolidone, pyrrolidone, caprolactam, urea, thiourea, atlantiscasino, ndimethylacetamide, benzamide, N,N-dimethylformamide and mixtures thereof, preferably using 5, 6 and 7-membered lactams (UK, application N 1422037, CL 07 F 9/165, publ. 21.01.76; R j "Inventions abroad", No. 2, vol. 24, 1976).

The process proceeds according to the scheme

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the houtem interaction of white (yellow) phosphorus with elemental sulfur at 640 - 650K, to obtain an active pentasulfide phosphorus is necessary to observe the mode of synthesis and cooling of the melt, which is associated with greater technological difficulties. The original components of the phosphorus and sulfur to obtain pentasulfide phosphorus should not contain incidental impurities. To increase the activity of the obtained pentasulfide phosphorus his purified by extraction or sublimation. Cleaning pentasulfide phosphorus requires additional energy consumption and leads to trudnookislyaemymi waste (the book, the authors A. A. Brodsky, W. A. Blankstein, C. A. Ershov, N. D. Talanov "Recycling of phosphorus", Leningrad, Khimiya, Leningrad branch, 1985, S. 171).

A method of obtaining metal salts of diesters dithiophosphoric acids selected as a prototype.

The disadvantage of this method is that it is laborious. In addition, in the process of interaction of the reagents produces a large quantity of hydrogen sulfide, which must be disposed of, therefore, the method is not environmentally safe and is associated with high economic costs.

Object of the invention is the simplification of the method of producing metal salts of diesters dithiophosphoric acids.

The reaction products are a thick liquid. The structure of the products is proved by the data of elemental analysis, IR and NMR31P spectroscopy. In the IR spectra of products watch bandP=Sin the area of 645 to 700 cm-1in NMR31P products see the signals in the fieldP100 - 105 M. D.

Primary execution method, when as a catalyst (the main character) use aliphatic, aromatic or cyclic primary, secondary or tertiary amines, amides, thioamides coal or carboxylic acid, or turangalila, or xanthates, or dithiocarbamate, or metal salts of diesters dithiophosphoric acids.

Primary execution method, when the metal oxide or hydroxide take Ca, Zn, Ni.

Primary execution method, when were the major examples of specific performance.

Example 1. Obtaining zinc salts diisobutylphthalate acid.

Take the elemental yellow phosphorus (P4) in the amount of 62 g of elemental sulfur (S8) in an amount of 140 g, butyl alcohol - 325 and the oxide Zinkov - 105 g in a molar ratio of 1:2,2:2,2:0,65 respectively. The interaction of these reagents are in 500 ml of solvent ethylbenzene in the presence of 0.2 g of catalyst a tertiary amine - tributylamine under stirring at a temperature of 90 - 125oC until complete conversion of the phosphorus and to achieve a pH environment of 5.5.

The reaction mixture is centrifuged, separating the liquid part from which the solvent is distilled off and the unreacted reagents.

Get 495 g (90,5%) of the desired product, which is a thick liquid light yellow color.

Elemental analysis data:

Found, % P 10,8; S 24,2; Zn 10,2.

Brutto-formula of the target product: C16H36O4P2S4Zn

Calculated, % P 11,3; S 23,4; Zn 11,8.

Example 2. Getting the calcium salt diisobutylphthalate acid.

Take the elemental yellow phosphorus (P4) in the amount of 62 g of elemental sulfur (S8) in an amount of 140 g, isobutyl alcohol - 300 g and the oxide of callories toluene in the presence of 0.2 g of the tertiary amine catalyst is of triethylamine with stirring, and the temperature of 90 - 120oC until complete conversion of the phosphorus and to achieve the pH of the medium to 7.0.

The reaction mixture is centrifuged, separating the liquid part from which the solvent is distilled off and the unreacted reagents.

Receive 428 g (82%) of the desired product, which is a thick liquid cream color.

Elemental analysis data:

Found, % P 11,2; S 24,9;

Brutto-formula of the target product: C16H36O4P2S4Ca

Calculated, % P 11,8; S 24,5;

Example 3. Getting Nickel salt diisobutylphthalate acid.

Take the elemental yellow phosphorus (P4) in the amount of 62 g of elemental sulfur (S8) in the amount of 147 g, isobutyl alcohol - 370 g and Nickel oxide 112 g in a molar ratio of 1:2,3:2,5:0.75 respectively.

The interaction of these reagents are in 500 ml of solvent xylene in the presence of 0.5 g of catalyst thioamide carbonic acid thiourea under stirring at a temperature of 100 - 130oC until complete conversion of the phosphorus and to achieve a pH environment of 5.5.

The reaction mixture is centrifuged, separating the liquid part from which the solvent is distilled off and not the liquid lilac.

Elemental analysis data:

Found, % P 11,50; S 24,0;

Brutto-formula of the target product: C16H36O4P2S4Ni

Calculated, % P 11,46; S 23,7;

Example 4. Obtaining zinc salts diisooctylphthalate acid.

Take elemental red phosphorus in the amount of 62 g of elemental sulfur in the amount of 155 g, isooctyl alcohol - 550 g and zinc oxide - 82 g in a molar ratio of 1: 2,4: 2,1: 0,5 respectively. The interaction of lead in 700 ml of solvent xylene in the presence of 3 g of the catalyst is a zinc salt diisooctylphthalate acid with stirring and the temperature of 90 - 140oC to achieve the pH of the medium 6.

The reaction mixture is centrifuged, separating the liquid part from which the solvent is distilled off and the unreacted reagents.

Get 385 g (50%) of the desired product, which is a thick liquid light yellow color.

Elemental analysis data:

Found, %: P 8,5; S 17,4

Brutto-formula: C32H68O4P2S4Zn

Calculated, %: P 8,04; S 16,8.

Example 5. Obtaining zinc salts dietaryguidelines acid.

The target product is obtained analogously to example 1.

Ber is the solution of the reactants is 1:2,2:2,2:0,65 respectively.

The interaction is carried out in the presence of 0.3 g of the catalyst of the primary amine is monoethanolamine in 500 ml of solvent toluene.

Get 536 g (89%) of the desired product, which is a thick liquid cream color.

Elemental analysis data:

Found, %: P 9,8; S 21,7; Zn 10,2

Brutto-formula of the target product: C20H44O4P2S4Zn

Calculated, %: P 10,3; S 21,2; Zn 10,8.

Example 6. Getting Nickel salt dietaryguidelines acid.

The target product is obtained analogously to example 3.

Take:

Phosphorus - 62 g

Sulfur - 130g

Isoamyl alcohol - 440 g

Nickel oxide - 80 g

The molar ratio of reactants is 1:2,04:2,5:0.53 per share, respectively.

The interaction is carried out in the presence of 0.2 g of catalyst turangalila - tetramethylthiuramdisulphide in 500 ml of solvent xylene.

Get 417 g (70%) of the desired product, which is a thick liquid lilac.

Elemental analysis data:

Found, %: P 9,8; S 21,7;

Brutto-formula of the target product: C20H44O4P2S4Ni

Calculated, %: P 10,4; S 21,4.

Example 7. Obtaining zinc Take:

Phosphorus - 62 g

Sulfur - 160 g

n-Hexyl alcohol - 450 g

Zinc oxide - 121 g

the molar ratio of reactants is 1:2,5:2,2:0.75 respectively.

The interaction is carried out in the presence of 0.5 g of the catalyst of the secondary amine - diethylamine in 500 ml of solvent is ethylbenzene.

Get 560 g (85%) of the desired product, which is a viscous yellow liquid.

Elemental analysis data:

Found, %: P 8,9; S 19,1;

Brutto-formula of the target product: C24H52O4P2S4Zn

Calculated, %: P 9,4; S 19,42.

Example 8. Getting the calcium salt vexillationes acid

The target product is obtained analogously to example 2.

Take:

Phosphorus - 62 g

Sulfur - 135 grams

n-Hexyl alcohol - 450 g

Calcium oxide - 80 g

the molar ratio of reactants is 1:2,1:2,2:0,71 respectively.

The interaction is carried out in the presence of 0.2 g of catalyst cyclic primary amine - cyclohexylamine in 1000 ml of solvent is ethylbenzene.

Receive 494 g(78%) of the desired product, which is a viscous yellow liquid.

Elemental analysis data:

Found, %: P 9,2; S 200,2.

Example 9. Obtaining zinc salts diisooctylphthalate acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 155 g

Isooctyl alcohol - 550 g

Zinc oxide - 82 g

the molar ratio of reactants is 1:2,4:2,1:0,5 respectively.

The interaction is carried out in the presence of 1 g of the catalyst is a zinc salt diisooctylphthalate acid in 700 ml of xylene.

Receive 678 g (88%) of the desired product, which is a thick yellow liquid.

Elemental analysis data:

Found, %: P 8,1; S 17,2

Brutto-formula of the target product: C32H68O4P2S4Zn

Calculated, % P 8,05; S 16,6.

Example 10. Getting the calcium salt diisooctylphthalate acid.

The target product is obtained analogously to example 2.

Take:

Phosphorus - 62 g

Sulfur - 160 g

Isooctyl alcohol - 560 g

Calcium oxide - 80 g

the molar ratio of reactants is 1:2,5:2,2:0,71 respectively.

The interaction is carried out in the presence of 0.5 g of catalyst amide carboxylic acid - ndimethylacetamide in 800 ml of ethylbenzene.

Receive 595 (80%) target 8,00

Brutto-formula: C32H68O4P2S4Ca

Calculated, %: P 8,3; S 17,2.

Example 11. Getting Nickel salt diisooctylphthalate acid.

The target product is obtained analogously to example 3.

Take:

Phosphorus - 62 g

Sulfur - 160 g

Isooctyl alcohol - 780 g

Nickel oxide - 80 g

the molar ratio of reactants is 1:2,5:3:0,53 respectively.

The interaction is carried out in the presence of 1 g of the catalyst thioamide carbonic acid - thiourea 700 g ml xylene.

Receive 507 g (66%) of the desired product as a thick liquid lilac.

Elemental analysis data:

Found, %: P 8,5; S 20,5.

Brutto-formula: C32H68O4P2S4Ni

Calculated, %: P 8,3; S 19,9.

Example 12. Obtaining zinc salts didodecyldimethylammonium acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 153 g

Dodecyloxy alcohol - 860

Zinc oxide - 90 g

the molar ratio of reactants is 1:2,4:2,3:0,55 respectively.

The interaction is carried out in the presence of 1 g of the catalyst xanthate - butylxanthine in 1000 ml of this.

Elemental analysis data:

Found, %: P 6,5; S 13,6.

Brutto-formula: C48H100O4P2S4Zn

Calculated, %: P 6,23; S 12,8.

Example 13. Getting the calcium salt didodecyldimethylammonium acid.

The target product was prepared as in example 2.

Take:

Phosphorus - 62 g

Sulfur - 160 g

Dodecyloxy alcohol - 1000 grams

Calcium oxide - 84 g

the molar ratio of reactants is 1:2,5:2,7:0.75 respectively.

The interaction is carried out in the presence of 1 g of the catalyst of the tertiary amine is triethylamine in 2000 ml of ethylbenzene.

Get 708 g (73%) of the desired product in the form of a pasty mass of dark yellow color.

Elemental analysis data:

Found, %: P 6,5; S 13,2.

Brutto-formula: C48H100O4P2S4Ca.

Calculated, %: P 6,23; S 12,8.

Example 14. Obtaining zinc salt of O,O,O-isobutyl, - O-isooctylphenol acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 160 g

Isobutyl alcohol - 240 g

Isooctyl alcohol - 140 g

Zinc oxide - 82 g,

the molar ratio of the reactants is 1:2,5:(1,6+0,5):0,5 accordingly the benzene.

Receive 548 g (91%) of the desired product as a thick liquid light cream color.

Elemental analysis data:

Found, %: P 10,1; S 20,8; Zn 10,3

Brutto-formula: C20H44O4P2S4Zn.

Calculated, %: P 10,3; S 21,2; Zn 10,8.

Example 15. Obtaining zinc salts O-O-O-isobutyl, - O-isooctylphenol acid.

The target product is obtained analogously to example 4.

Take:

Red phosphorus - 62 g

Sulfur - 160 g

Isobutyl alcohol - 240 g

Isooctyl alcohol - 140 g

Zinc oxide - 82 g

the molar ratio of the reactants is 1: 2,5:(1,6+0,53):0,5 respectively. The interaction is carried out in the presence of 1 g of the catalyst of the primary amine is dodecylamine in 760 ml of xylene.

Get 361 g (60%) of the desired product as a thick liquid light yellow color.

Elemental analysis data:

Found, %: P 10,8; S 21,8; Zn 10,0

Brutto-formula: C20H44O4P2S4Zn

Calculated, %: P 10,3; S 21,2; Zn 10,8.

Example 16. Getting Nickel salts O-O-O-isobutyl, - O-isooctylphenol acid.

The target product is obtained analogously to example 3.

Take:

Phosphorus - 62 g

Sulfur - 135 grams

The interaction is carried out in the presence of 0.5 g of catalyst dithiocarbamate - dimethyldithiocarbamate zinc in 500 ml of toluene.

Get 447,5 g (75%) of the desired product, which is a thick liquid lilac.

Elemental analysis data:

Found, %: P 9,85; S 22,1.

Brutto-formula: C20H44O4P2S4Ni

Calculated, %: P 10,3; S 21,45.

Example 17. Obtaining zinc salt of O,O-isobutyl -, O -, O-isooctylphenol acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 153 g

Isobutyl alcohol - 170 g

Isooctyl alcohol - 275 g

Zinc oxide - 85 grams

The molar ratio of reagents 1:2,4:(1,15+1,05):0,52 respectively.

The interaction is carried out in the presence of 1 g of the catalyst of zinc salts diisopropylethylamine acid in 700 ml of xylene.

Receive 612 g (93%) of the desired product, which is a thick liquid light cream color.

Elemental analysis data:

Found, %: P 9,6; S 19,8

Brutto-formula: C24H52O4P2S4Zn

Calculated, %: P 9,4; S 19,4.

Example 18. Getting the calcium salt of O,O-the tx2">

Take:

Phosphorus - 62 g

Sulfur - 148 g

Isobutyl alcohol - 162 g

Isooctyl alcohol - 280g

Calcium hydroxide - 74 g

the molar ratio of reagents 1:2,3:(1,1+1,07):1 respectively.

The interaction is carried out in the presence of 0.5 g of catalyst amide carboxylic acid - ndimethylacetamide in 500 ml of toluene.

Receive 494 g (78%) of the desired product, which is a thick liquid cream color:

Elemental analysis data:

Found, %: P 10,2; S 21,5.

Brutto-formula: C24H52O4P2S4Ca.

Calculated, %: P 9,8; S 20,2

Example 19. Getting Nickel salt of O,O-isobutyl -, O -, O-isooctylphenol acid.

The target product is obtained analogously to example 3.

Take:

Phosphorus - 62 g

Sulfur - 142 g

Isobutylic alcohol - 175 g

Isooctyl alcohol - 325

Nickel oxide - 112 g

the molar ratio of the reactants is 1:2,2:(1,2+1,25):0,75 respectively. The interaction is carried out in the presence of 0.2 g of catalyst a tertiary amine is triethanolamine in 500 ml of toluene.

Receive 457 l (70%) of the desired product as a thick liquid lilac.

Elemental analysis data:

Found, %: P 9,8; S2">

Example 20. Obtaining zinc salt of O,O-isobutyl -, O -, O-solidityturning acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 150 grams

Isobutyl alcohol is 155 g

Isoamyl alcohol is 185 g

Zinc oxide - 90 g

The molar ratio of reagents 1: 2,3:(1,05+1,05):0,55 respectively. The interaction is carried out in the presence of 0.5 g of the tertiary aromatic amine - dimethylaniline in 500 ml of toluene.

Receive 517 g (90%) of the desired product as a thick bright liquid.

Elemental analysis data:

Found, %: P 10,2; S 22,9.

Brutto-formula: C18H40O4P2S4Zn

Calculated, %: P 10,8; S 22,3.

Example 21. Getting the calcium salt of O,O-isobutyl -, O -, O-solidityturning acid.

The target product is obtained analogously to example 2.

Take:

Phosphorus - 62 g

Sulfur - 160 g

Isobutyl alcohol - 170 g

Isoamyl alcohol - 264 g

Calcium hydroxide - 96 g

The molar ratio of reagents 1:2,5:(1,15:1,5):0,65 respectively.

The interaction is carried out in the presence of 1 g of the catalyst of timid carbonic acid - thiourea in 500 ml of toluene.

Receive 451 (82%) of the whole is 3,9.

Brutto-formula: C18H40O4P2S4Ca

Calculated, %: P 11,3; S 22,3.

Example 22. Getting Nickel salt of O,O-isobutyl -, O -, O-solidityturning acid.

The target product is obtained analogously to example 3.

Take:

Phosphorus - 62 g

Sulfur - 150 grams

Isobutyl alcohol - 165 g

Isoamyl alcohol is 200 grams

Nickel oxide - 95 g

the molar ratio of the reactants is 1:2,34:(1,1+1,13):0,63 respectively. The interaction is carried out in the presence of 1 g of the catalyst of the tertiary amine is 2,6-getrebacktranslation in 500 ml of ethylbenzene.

Get 398 g (70%) of the desired product, which is a thick liquid lilac.

Elemental analysis data:

Found, %: P 10,2; S 23,1.

Brutto-formula: C18H40O4P2S4Ni

Calculated, %: P 10,9; S 22,5.

Example 23. Getting the calcium salt of O-isopropyl, O,O,O-solidityturning acid.

The target product is obtained analogously to example 2.

Take:

Phosphorus - 62 g

Sulfur - 142 g

Isopropyl alcohol and 90 g

Isoamyl alcohol - 280g

Calcium oxide - 67 g

the molar ratio of reactants is 1:2,2:(0,75+disulfide in 500 ml of toluene.

Receive 489 g (89%) of the desired product as a thick pale cream-colored liquid.

Elemental analysis data:

Found, %: P 10,8; S 24,01.

Brutto-formula: C18H40O4P2S4Ca

Calculated, %: P 11,3; S 23,3.

Example 24. Obtaining zinc salt of O-isopropyl, O,O,O-isobutylacetophenone acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 128 g

Isopropyl alcohol - 65 g

Isobutyl alcohol - 225 g

Zinc oxide - g

the molar ratio of the reactants is 1:2:(0,54+1,52):0,5 respectively. The interaction is carried out in the presence of 1 g of the catalyst of the secondary amine is diethanolamine in 400 ml of toluene.

Receive 426 g (80%) of the desired product as a thick bright liquid.

Elemental analysis data:

Found, %: P 11,5; S 24,5.

Brutto-formula: C15H34O4P2S4Zn

Calculated, %: P 11,6; S 24,0.

Example 25. Obtaining zinc salts diapir dithiophosphoric acid based on the fraction of C9-C13synthetic fatty alcohols.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Get 750 g (80%) of the desired product in the form of a pasty mass brown.

Elemental analysis data:

Found, %: P 6,4; S 13,8.

Example 26. Obtaining zinc salt of O,O-isobutyl -, O -, O-isoenergetically acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 145g

Isobutyl alcohol - 160 g

n-Isononylphenol - 440 g

Zinc oxide - 85 grams

the molar ratio of the reactants is 1:2,3:(1,08+1):0,52 respectively.

The interaction is carried out in the presence of 2 g of catalyst amide of carbonic acid - urea in 700 ml of xylene at 90 - 160 oC.

Receive 771 g (92%) of the desired product as a thick liquid cream color.

Elemental analysis data:

Found, %: P 7,1; S 15,9;

Brutto-formula: C38H64O4P2S4Zn

Calculated, %: P 7,4; S 15,3.

Example 27. Getting Nickel salt of O,O-isobutyl -, O -, O-isononylphenol dithiophosphoric acid.

The target product is obtained analogously to example 3.

Take:

THE

the molar ratio of the reactants is 1: 2,26:(1,35+1):0,53 respectively.

The interaction is carried out in the presence of 0.2 g of catalyst turangalila - tetramethylthiuramdisuphide in 700 ml of benzene at 90 - 160oC.

Receive 433 g (52%) of the desired product as a thick liquid dark purple color.

Elemental analysis data:

Found, %: P 6,9; S 14,9.

Brutto-formula: C38H64O4P2S4Ni

Calculated, %: P 7,44; S 15,4.

Example 28. Obtaining zinc salt of O,O,O-isobutyl-O-isoenergetically acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 160 g

Isobutyl alcohol - 280g

n-Isononylphenol 220 g

Zinc oxide - 121 g

the molar ratio of the reactants is 1:2,5:(1,9+0,5):0,75 respectively.

The interaction is carried out in the presence of 1 g of the catalyst a tertiary amine - tributylamine in 1000 ml of xylene at 90 - 140oC.

Receive 609 g (88%) of the desired product as a thick liquid cream color.

Elemental analysis data:

Found, %: P 9,4; S 19,2

Brutto-formula: C27H50O4P2S4Zn

the slots.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 145g

Isobutyl alcohol - 160 g

n-Tertbutylphenol - 300 grams

Zinc oxide - 85 grams

the molar ratio is 1:2,26:(1,08:1):0,52 respectively.

The interaction is carried out in the presence of 1 g of the catalyst a tertiary amine 2,6-getrebacktranslation in 500 ml of benzene at 90 - 140oC.

Receive 573 (82%) of the desired product as a thick liquid brown.

Elemental analysis data:

Found, %: P 9,2; S 19,00.

Brutto-formula: C28H44O4P2S4Zn

Calculated, %: P 8,9; S 18,3.

Example 30. Obtaining zinc salt of O,O-isooctyl, O-O-n-tertbutylbenzothiazole acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 145g

Isooctyl alcohol - 300 grams

n-Tertbutylphenol - 300 grams

Zinc oxide - 84 g

the molar ratio is 1:2,26:(1,15:1):0,51 respectively.The interaction is carried out in the presence of 1 g of the catalyst - Nickel salt diisobutylphthalate acid in 700 ml of xylene at 100 - 150oC.

Receive 552 g (79%) of the desired product in the form of the RM-formula: C28H44O4P2S4Zn

Calculated, %: P 8,86; S 18,3.

Example 31. Obtaining zinc salt of O,O-isobutyl -, O -, O-2,6-directbuylighting.com acid.

The target product is obtained analogously to example 1.

Take:

Phosphorus - 62 g

Sulfur - 160 g

Isobutyl alcohol - 200g

2,6-Ditertbutyl - 412 g

Zinc oxide - 88 g

the molar ratio of the reactants is 1:2,5:(1,35+1):0,54 respectively.

The interaction is carried out in the presence of 2 g of the catalyst is a zinc salt diisobutylphthalate acid in 700 ml of xylene at 100 - 160oC.

Get 405 g (50%) of the desired product as a thick brown liquid.

Elemental analysis data:

Found, %: P 7,00; S 15,9;

Brutto-formula: C36H60O4P2S4Zn

Calculated, %: P 7.62mm; S 15,8.

Example 32. Obtaining zinc salt of O,O,O-isooctyl, O-2,6 - directbuylighting.com acid.

Target product as in example 1.

Take:

Phosphorus - 62 g

Sulfur - 160 g

Isooctyl alcohol - 430 g

2,6-Ditertbutyl - 206 g

Zinc oxide - 90 g

The molar ratio of the reactants is 1:2,5:(1,65+0,5):0,55 respectively.

oC.

Receive 584 (69%) of the desired product as a thick brown liquid.

Elemental analysis data:

Found, %: P 7,8; S 15,9.

Brutto-formula: C38H72O4P2S4Zn

Calculated, %: P 7,3; S 15,1.

Example 33. Getting Nickel salt of O,O-isobutyl -, O -, O-solidityturning acid.

The target product is obtained analogously to example 4.

Take:

Red phosphorus - 62 g

Sulfur - 150 grams

Isobutyl alcohol - 165 g

Isoamyl alcohol is 200 grams

Nickel oxide - 95 g

The molar ratio of the reactants is 1:2,33:(1,4+1,15):0,63 respectively. The interaction is carried out in the presence of 0.5 g of catalyst turangalila - tetramethylthiuramdisuphide in 500 ml of o-xylene at 120 - 140oC.

Get 325 g (62%) of the desired product, which is a thick liquid lilac.

Elemental analysis data:

Found, %: P 10,5; S 22,8

Brutto-formula: C18H40O4P2S4Ni

Calculated, %: P 10,9; S 22,5.

Example 34. Obtaining zinc salt of O,O,O-isobutyl, - O-n - isoenergetically acid.

The target product is obtained analogously to example 4.

/BR> Zinc oxide - 121 g

The molar ratio of the reactants is 1:2,5:(1,9+0,5):0,75 respectively.

The interaction is carried out in the presence of a catalyst is a zinc salt of O,O,O-isobutyl, - O-isooctylphenol acid in 600 ml of xylene at 120 - 140oC.

Receive 423 g (61%) of the desired product as a thick liquid cream color.

Elemental analysis data:

Found, %: P 9,2; S 18,8

Brutto-formula: C27H50O4P2S4Zn

Calculated, %: P 8,9; S 18,5.

Example 35. Obtaining zinc salt of O,O-isobutyl -, O -, O-2,6-directbuylighting.com acid.

The target product is obtained analogously to example 4.

Take:

Red phosphorus - 62 g

Sulfur - 160 g

Isobutyl alcohol - 200g

2,6-Ditertbutyl - 412 g

Zinc oxide - 88 g

The molar ratio of the reactants is 1:2,5:(1,35+1):0,54 respectively.

The interaction is carried out in the presence of 1 g of the catalyst of the tertiary amine is triethanolamine in 700 ml of xylene at 120 - 160oC.

Get 650 g (80%) of the desired product as a thick liquid dark color.

Elemental analysis data:

Found, %: P 7,8; S 16,2.

Brutto-formula: C36H60

1. The method of obtaining metal salts of diesters dithiophosphoric acids by the interaction of the reactants by heating in a solvent in the presence of a catalyst, characterized in that as reagents take elemental phosphorus, and elemental sulfur, aliphatic alcohol, or a mixture of aliphatic alcohols, or a mixture of the substituted phenol and an aliphatic alcohol and an oxide or hydroxide of the metal in a molar ratio 1: (2 - 2,5) : (2 - 3) : (0,5 - 0,75) accordingly, the interaction leads to complete conversion of the phosphorus and to achieve a pH of the reaction mass 5,5 - 7,0.

2. The method according to p. 1, characterized in that the catalyst used aliphatic, aromatic or cyclic primary, secondary or tertiary amines, amides, thioamides coal or carboxylic acid, or turangalila, or xanthates, or dithiocarbamate, or metal salts of diesters dithiophosphoric acids.

3. The method according to p. 1, characterized in that the metal oxide or hydroxide take Ca, Zn, Ni.

4. The method according to PP.1 to 3, characterized in that the interaction of these reagents is carried out at 90 - 140oC.

 

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