SU950732A1 - Arylsulfonato-bis-acetylacetonates of manganese (iii) as initiators of (co)polymerization of compounds exhibiting surface-active properties - Google Patents

Description

In a 50 ml beaker, dissolve 2 g of TAM in 10 ml of benzene. Separately, dissolve 1 g of benzenesulfonic acid in 10 ml of acetone and add with stirring to a TAM solution at 20 ° C. The crystalline green precipitate formed after 1-2 minutes is filtered off, washed with the indicated solvents from the starting products, dried to constant weight and analyze. The yield of benzenesulfonate bis-acetylacetonate Mn (lll) is 2.15 g W7I 93%. PRI mme R 2. p-Toluensulfonate bis-acetylacetonate Mn (| 1). In a 50 ml beaker, 2 g of TAM is dissolved in 10 ml of tetrahydrofuran. Separately, 1.1 g of p-toluenesulfonic acid is dissolved in 10 ml of tetrahydrofuran and added with stirring to a solution of TAM at 20 ° C. The crystalline green precipitate formed after 1-2 minutes is filtered off, washed with tetrahydrofuran from the starting materials, dried to constant weight and analyze. The yield of p-toluensulfonato-bis-acetyl-acetonate (111) is 2.1 or 90%. PRI me R 3. p-Styrene sulfonato bis-acetylacetonate (111). In a 50 ml beaker, 2 g of TAM is dissolved in 10 ml of acetone. Separately, dissolve 1 g of p-styrene sulfonic acid in 10 ml of acetone and add with stirring to a TAM solution at 20 ° C. The green crystalline precipitate formed after 3-4 min is filtered off, washed with acetone from the starting products, dried to constant weight and analyze. The output of p-styrene sulfonato bis-acetylacetonate Mn (lll) 1.24 g or 50%. Example 4. p-Sulfosalicylate bis-acetylacetonate Mn (lll). In a 50 ml beaker, dissolve 2 g of TAM in 10 ml of acetone. Separately, dissolve 1.6 ml of sulfosalicic acid in 10 ml of acetone and add with stirring to the TAM solution at 20 ° C. After 1-2 minutes, the crystalline precipitate of the green brush is filtered off, washed with acetone from the starting products, dried to a constant mass and analyzed. The output of the p-sulfosalicyst to bis bis-acetylacetonate Mn () 2.14 g or 80% Example. p-Phenolsulfonato bis-acetylacetonate Mn (). In a 50 ml beaker, dissolve 2 g of TAM in 10 ml of acetone. Separately, dissolve 1 g of p-phenolsulphonic acid in 10 ml of acetone and add with stirring to the TAM solution at 20 ° C. The green crystalline precipitate formed after 1-2 minutes is screened off, washed with acetone from the starting products, dried to a constant mass and anaize. Exit p-phenolsulfonato bis-acety. Mn (lll) cetonate 1.96 g or 81%. PRI me R 6. Decyl benzenesulfonate bis-acetylacetonate (111). In a 50 ml beaker, 1.3 g of TAM is dissolved in 20 ml of diethyl ether. Separately, dissolve 1 g of decylbenzenesulfonic acid in 10 ml of diethyl ether and add, under stirring, to a TAM solution of 10 ° C. The green precipitates formed after 1-2 minutes are filtered off, washed off from the original products with distillate ether, dried to flow. and analyze. The output of alkylenediamine sulfonate bis-acetylacetonate Mn (lll) 1.32 g or 72%. The study of the surface activity of the obtained Mn (lll) compounds by determining the surface tension of their aqueous solutions and stability during long-term storage shows that the introduction of the sulfo-aromatic ligand into the metal chelate produces compounds with surface-active properties and storage stability. Win (III) sulfocomplexes, in contrast to the usual radical initiators in the process of bezomulgatornoy (co) polymerization of vinyl compounds. Surface-active properties of Mn (lll) sulfocomplexes at 20 ° С, Сз 10n / m. B-benzosulfonato-bis-acetylacetonate Mn (lll) 54.6 p-toluensulfonato-bis-acetylacetonate Mn (111) 52.5 p-Decyl benzenesulfonatobis-acetylacetonate Mn (111) 31.4 n-Phenolsulfonato-bys-acetylacetone Mn (lll ) 51.3 p-Sulfosalicylate-bis-acetylacetonate Mn (lll) 52.5 p-Styrene sulfonato-bis-acetylacetonate Mn (111) 40.2 Manganese chloride-bis-aceclaacetonate (1) 68.1 In a table. 2 shows the technological parameters and conditions (co) polymerization of vinyl compounds (20% solution of acrylamide in water) in the presence of manganese (III) sulfocomplexes. A study of the initiating activity of Mn (| 11) sulfocomplexes over time allows us to establish that the synthesized compounds are highly active initiators and, unlike the prototype, have a time-initiating initiating activity, which may be due to the stabilizing effect of the aromatic ring.

The proposed Mn (lll) sulfocomplexes, obtained from tris-acetylacetone in manganese and aromatic sulfonic acids and used for (co) polymerization of wine compounds, provide, in comparison with the known MP (III) metal chelates, a wide range of new highly efficient catalytic systems based on Mn (111) with mixed ligands of different structure, with high stability and surface-active properties.

The use of Mn (lll) sutpocomplexes as inspectors for (co) polymerization provides oxidation and bending in the polymerization of vinyl monomers and the flow of (co) polymerization in the presence of air oxygen at 10–30 ° C at high rates (100% The yield of polymers at 2P ° С and the concentration of sulfonic complexes Mn (lll) equal to 0.5% of the mass of monomers is reached in 510 missions.

(Table 2

By offering-. Benzene sulphonate-ghbis-acetylmode Mn (lll) acetonate

Toluensulfonato bis acetyl acetonate Mn (lll)

Styrene sulfonato-bis-acetylacetonate Mn (lll)

Decyl-benzylsulfonato-bis-acetylacetonate, Mn (111)

Sulfosalicylate Bis-acetylacetonate Mp (111)

Phenolsulfonato bis-acetylacetonate Mn (lll)

Claims (1)

Known Hlorvd bis-acetyl acetonate Mn (111) Claims of the invention Mar (II) arilsulfonato bis-acetylacetonates of the general formula b - c - oo with HC with I CHi X, o thirty 0 80 12 0 20 70 12 60 0.5 20 12 0 63 20 12 58 0 20 12 60 0.5 20 12 32 0.5 20 where R Н, CHj, ОН, СООH, СН CHj, СюНгз as initiators of (co) polymerization of cherish compounds with surface active properties. Sources of information taken into account in examination 1, USSR Author's Certificate N 691460, WI. C 07 F 13/00, 1979.