Tetra-2,3-inoxidizability manganese as a thermo stabilizer of polyvinyl chloride

 

(57) Abstract:

Usage: as a thermo stabilizer of polyvinyl chloride. The inventive product of Tetra-2,3-inoxidizability manganese. B. F. C40H16N16Nn, yield 8% (nitrile), black with a metallic sheen crystalline powder, not melting up to 500oAnd not soluble in concentrated mineral acids, DMF, DMSO. Reagent 1: 2,3-dicyanobenzoquinone. Reagent: anhydrous manganese chloride. Reaction conditions: when heated to 200oC for 6 h 2 Il., table 1.

The invention relates to the synthesis of new macrocyclic complex compounds of some Tetra-2,3-Hino - clinophobia manganese, which can be used as a thermo stabilizer of polyvinyl chloride in the production of plastics, artificial leather, film materials.

A new chemical compound Tetra-2,3-inoxidizability manganese (2,3-Q) (1).

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On the structure of the inventive compound is a complex of Tetra-2,3-inoxidizability with ions of Mn2+.

The closest analogue of the claimed compounds on the structure and applied the Torah PVC plastics are not high enough "oven" properties.

The basis of the invention is consisting in the search for a new connection, which is the stabilizer in PVC plastics, which would improve their thermal stability.

For this task synthesized a new compound, namely Tetra-2,3-inoxidizability manganese (2,3-Q).

The proposed connection allows you to increase thermostability of PVC plastics more efficiently than its counterpart.

The difference in the structure of the claimed compounds and is similar in nature condensed with piperazinonyl cycle of aromatic fragments: cinoxacin in the case of the claimed compounds and benzene in the case of compounds similar [1] Such structural differences, namely: the presence of four hinoksalinovym cycles, condensed with porphyrazines provide the claimed connection "oven" best properties in comparison with the similar [2]

The structure of the claimed compounds proved elemental analysis and data electronic and vibrational spectroscopy (Fig.1 and 2).

Tetra-2, 3-inoxidizability manganese.

Calculated for C40H16N16Mn, C, 62.02; H To 2.06; N 28,94; Mn 6,98.

Found, C 63,01; H azinovic character, that confirms the presence in the structure of the molecule porphyrazines, extension tubes, condensed with four hinokio - new rings.

The parameters of the policy of the claimed compounds 2,3-Q: Solvent DMSO. Absorption band, nm: I: 718; II 670.

According to literature data [3] ESP metal-Tetra-2,3-inoxidizability find an intensive absorption in DMSO in the field 600-769 nm.

It is known that the IR spectra of porphyrinoid compounds is very complex and many absorption bands in them lose their characteristic property due to strong coupling to macrocells and currently almost not identified. However, the type of spectrum is very characteristic and can be used for identification of newly synthesized compounds of this class.

The IR spectra of 2,3-Q (Fig. 2) have a high degree of analogy with the IR spectra of other tetrahydrocannabivarin that can serve as a convincing proof of their structure.

The synthesis of the claimed compounds and measure their "oven" properties was carried out according to the given examples.

P R I m e R 1. Obtaining Tetra-2,3-inoxidizability manganese.

1.8 g (0.01 mol) of 2,3-dicionaries the>TheC for 6 hours, the Obtained melt was ground, washed with 5% hydrochloric acid, was extracted with hot acetone. The product was dried under vacuum at 100aboutC. Obtained Tetra-K2,3-inoxidizability manganese black with a metallic sheen crystalline powder, not melting up to 500aboutWith and insoluble in most organic solvents. Soluble in concentrated mineral acids, DMF and DMSO in quantities of up to 10-5mol per liter. Yield 1.52 g (80% nitrile).

P R I m m e R 2. Sample preparation of polyvinyl chloride.

100 g of polyvinyl chloride C-70 was thoroughly mixed with 55 g of di(2-ethylhexyl)phthalate (DOP) and 0.2 g (0,13%) Tetra-2,3-inoxidizability manganese kept for 1 h at a temperature of 100aboutFor swelling. The swollen mixture was valavala when the temperature of the rolls 150aboutWith and frictions 1:1,25 within 10 minutes, the resulting film of polyvinyl chloride thickness 0,150,03 mm warmed up in the press at a temperature of 150aboutC for 2 min, and extruded at this temperature under a pressure of 10 MPa for 2 min and cooled to 20 minutes Similarly prepared samples containing 0.2 g (0,13%) of manganese phthalocyanine (analog) and contains no additives. Samples of Ispytateley "oven" properties of the sample, 0.5 g of a film of polyvinyl chloride (obtained according to example 2), containing of 0.13 g of Tetra-2,3-inoxidizability manganese, was placed in the crucible of derivatograph system R. Pawlik, N. Paulik, L. Erdei and experienced in dynamic temperature regime with the speed of temperature rise of 3.2aboutWith in a minute in an argon atmosphere (flow rate of argon gas of 3 ml/min) sample comparison of Al2O3. "Oven" properties of the additive was estimated to increase the temperature of the beginning of decomposition (TN. p. determined by the point of intersection of the tangents constructed to the two branches of the curve TG, and the effective activation energy of thermal decomposition of (EEF.calculated according to the method Meshcheryakova [4]

Similarly performed derivatographic tests unstabilized films and polyvinyl chloride containing 0.2 g (0,13%) manganese phthalocyanine.

The obtained data were compared with those for unstabilized films and for films containing 0.2 g (0,13%) manganese phthalocyanine.

The results are given in the table.

Thus, Tetra-2,3-inoxidizability manganese is a thermo stabilizer of polyvinyl chloride in its "oven" properties, superior to similar manganese phthalocyanine.

Tetra-2,3-hinoksolinov the

 

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FIELD: organic chemistry, medicine, physiology.

SUBSTANCE: invention relates to agents for regulation (maintaining or suppression) of physical working ability and/or adaptation to different variants represented by solvated complex compounds of the general formula (I): Katm+[L1qEL2]Ann- x p.Solv (I) wherein L1 means aminothiols of the formula: R1NHCH(R2)(CH2)1-2SR3 wherein R1 means hydrogen atom (H), (C1-C20)-alkyl or RCO; R means (C1-C19)-alkyl; R2 means H or carboxyl; R3 means H, (C1-C20)-alkyl, (C2-C20)-alkenyl or benzyl; q = 1, 2 or 3; L2 means halogen atom, water and/or organic ligand. For example, bis-(N-acetyl-L-cysteinato)aquozinc (II) diheptahydrate suppresses physical working ability and in the dose 50 mg/kg increases reviving time of mice by 6 times and cats - by 2.8fold under conditions of acute hypoxia with hypercapnia, and increases reviving time of mice by 4 times under conditions of acute hypobaric hypoxia. Under the same conditions the known antihypoxic agents amtizol, acizol or mexidol are inactive or less active significantly by their activity. Bis-(N-acetyl-L-cysteinato)-ferrous (II) pentahydrate is more active as compared with the known antihypoxic agents and protects experimental animals in 4 variants of hypoxia. Bis-(N-acetyl-L-cysteinato)zinc (II) sulfate octahydrate is similar to enumerated compounds by its antihypoxic activity.

EFFECT: valuable medicinal properties of compounds.

4 cl, 1 dwg, 11 tbl, 33 ex

FIELD: catalyst preparation methods.

SUBSTANCE: invention relates to preparation of manganese (III) acetylacetonate, which can be used as catalyst as well as vinyl monomer polymerization initiator. Method is implemented in aqueous medium with ammonium acetylacetonate freshly prepared by mixing acetylacetone with aqueous ammonia solution. Hydrogen peroxide is used as oxidant and sodium bicarbonate is additionally introduced into reaction mixture. Following consecutive operations are carried out: reaction of manganese (II) chloride tetrahydraye with sodium bicarbonate; separating thus formed manganese (II) bicarbonate in the form of paste; adding ammonia acetylacetonate and then hydrogen peroxide aqueous solution to the paste; and recovering manganese (III) acetylacetonate with yield 95%.

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FIELD: chemical technology.

SUBSTANCE: invention relates to technology for synthesis of acetic acid inorganic salts. Method involves interaction of metallic manganese or its dioxide with acetic acid in the presence of oxidizing agent. Process is carried out in beaded mill of vertical type fitted with reflux cooling-condenser, high-speed blade mixer and glass beads as grinding agent loaded in the mass ratio to liquid phase = 1.5:1. Liquid phase represents glacial acid solution in ethylcellosolve, ethylene glycol, 1,4-dioxane, isoamyl alcohol and n-butyl alcohol as a solvent. The concentration of acid in liquid phase is 3.4-4 mole/kg. Then method involves loading iodine in the amount 0.025-0.070 mole/kg of liquid phase, metallic manganese and manganese dioxide in the mole ratio = 2:1 and taken in the amount 11.8% of liquid phase mass. The process starts at room temperature and carries out under self-heating condition to 30-38°C to practically complete consumption of manganese dioxide. Prepared salt suspension is separated from beads and unreacted manganese and filtered off. Filtrate is recovered to the repeated process and prepared precipitate is purified by recrystallization. Invention provides simplifying method using available raw and in low waste of the process.

EFFECT: improved method of synthesis.

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EFFECT: the invention ensures the increased output of the product, the reduced amount of the wastes, the insignificant consumption of the catalyst.

3 ex, 1 tbl

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to an improved solid-phase method for synthesis of radioisotope indicators, in particular, for synthesis of compounds labeled with 18F that can be used as radioactive indicators for positron- emission tomography (PET). In particular, invention relates to a method for synthesis of indicator labeled with 18F that involves treatment of a precursor fixed on resin if the formula (I): SOLID CARRIER-LINKER-X-INDICATOR wherein X means a group promoting to nucleophilic substitution by a definite center of a fixed INDICATOR with 18F- ion for preparing a labeled indicator of the formula (II): 18F-INDICATOR; to compound of the formula (Ib):

and compound of the formula (Ih): ;

to radiopharmaceutical set of reagents for preparing indicator labeled with 18F for using in PET; to a cartridge for radiopharmaceutical set of reagents for preparing indicator labeled with 18F for using in positron-emission tomography.

EFFECT: improved method of synthesis.

13 cl, 1 sch, 3 ex

FIELD: chemical industry; methods of production of the manganese salts with the organic acids.

SUBSTANCE: the invention is pertaining to production of the manganese salts with the organic acids in particular, to the salt of the divalent manganese and formic acid. The method is exercised by interaction of manganese, its oxides in the state of the highest valence with the formic acid solution in the organic solvent in the presence of iodine as the stimulating additive. The production process is conducted in the bead grinder of the vertical type having the revertive cooler-condenser, the high-speed paddle stirrer and the glass beads of in the capacity of the grinding agent loaded in the mass ratio to the loading of the liquid phase as (1÷2): 1. The liquid phase consists of the formic acid solution in the organic solvent. The concentration of the acid is taken within the range of 3.5÷10.8 mole/kg. In the loaded liquid phase they dissolve the stimulating additive of iodine in the amount of 0.025-0.100 mole/kg of the liquid phase. The ratio of the masses of the liquid phase and the total of the metallic manganese and the manganese oxide are as(4.9÷11):1. The molar ratio of the metal and the oxide in the loading is as (1.8÷2.,2):1. The metal and the oxide are loaded the last. It is preferable in the capacity of the dissolvent to use the butyl alcohol, ethyl acetate, ethylene glycol, 1.4-dioxane, dimethyl formamide. The production process is started and conducted at the indoor temperature up to practically complete(consumption of the whole loaded manganese oxide. Then the stirring is stopped, the suspension of the salt is separated from the beads and the nonreacted manganese and after that conduct filtration. The filtrate and the nonreacted manganese are returned into the repeated production process, and the filtered out settling of the manganese salt is exposed to purification by recrystallization. The technical result of the invention is - simplification of the method at usage of accessible reactants.

EFFECT: the invention ensures simplification of the method at usage of accessible reactants.

16 ex, 2 tbl

FIELD: chemistry.

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2 cl, 13 ex, 2 tbl

FIELD: medicine.

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EFFECT: production of new chelating agents applicable for making the technetium complexes.

22 cl, 12 ex, 3 dwg, 2 tbl

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