Method of producing manganese alcoholates

FIELD: chemistry.

SUBSTANCE: invention relates to method of producing manganese (II) alcoholates which can be used in different syntheses, in purification of complex multicomponent mixtures from alcohols, in analytical control and in scientific research. The method involves direct reaction of metal with alcohol in a vertical bead mill. The liquid phase used is the corresponding alcohol taken in mass ratio to glass beads of 1:1.5. Manganese is taken in amount of 5.81-43.3 % of the mass of the liquid phase. The process is initiated at room temperature and is carried out while controlling by taking samples and determination of content of manganese (II) compounds until all the loaded metal is virtually exhausted, after which stirring in the glass bead is stopped. The suspension of the reaction mixture is separated from the glass beads and taken for filtering. The alcoholate residue is washed with a liquid phase solvent and taken for purification by recrystallisation, and the filtrate and washing liquid phase with traces of dissolved alcoholate are returned for a repeated process. As a rule, the alcohol used is C1-C5-alcohol with normal and isomeric structure, cyclohexanol, ethyl cellosolve and ethylene glycol.

EFFECT: method allows for reaction of manganese with alcohol in conditions where the reaction could have been quantitatively insufficient with respect to the reagent, could have taken place at technically acceptable rates and led to accumulation the main mass of the product in solid phase, which can be easily separated by simple filtering.

2 cl, 2 tbl, 18 ex

 

The invention relates to a process for the preparation of organic compounds of manganese, which can be used in various fields of synthesis, purification complex multicomponent mixtures of alcohols, analytical control and scientific research.

A method of obtaining glycolate, calcium (Weng W.Y., Yang H., M. Ge // Mater.Chem. Phys. 1998, v.55, no. 2, p.102-107) by the interaction of metallic calcium with ethylene glycol. The process proceeds in accordance with the equation

4HOCH2CH2OH+Sa→Sa→(OCH2CH2OH)2·2HOCH2CH2OH+H2

The disadvantages of this method are:

1. The relatively high cost of the product associated with the use of metallic calcium.

2. Calcium - alkaline earth metal and manganese is in the 7th group of the Periodic system. Therefore, there is no reason to believe that both metals will react with a glycol of the same type and with similar speeds and outputs.

3. Ethylene glycol has two alcohol groups. It is not necessary that monohydroxy alcohols will interact similarly quickly and with good outputs.

Closest to the claimed is a method of producing formate, manganese (II) (patent RF №2316536), according to which a direct interaction of the metal, its oxide and formic acid are in the presence of liquid phases and stimulating supplements of iodine in the bead mill, vertical type, in the absence of an external supply of heat when the mass ratio of the liquid phase and beads 1:(1:2) and solid reagents (4,9÷11):1. As the liquid phase take a solution of formic acid in an organic solvent with a concentration of acid 3,5÷10,8 mol/kg and download the first or directly prepared from the components in the bead mill. Then it dissolved stimulating Supplement iodine in the amount of 0.025-0,100 mol/kg liquid phase and carry out the loading of the metal and its oxide in a molar ratio of 1.8÷2,2): 1. The process begins and is carried out at room temperature until almost fully exhausted just downloaded manganese oxide, after which the reaction mixture is separated from the glass beads and heavy particles of unreacted metal and filtered, the precipitate of manganese formate sent for recrystallization, and unreacted manganese and the filtrate is returned to repeat the process.

The manganese oxide is used MnO2, Mn2O3or Mn3O4and as an organic solvent - ethyl acetate, ethylene glycol, ethyl cellosolve, 1,4-dioxane, dimethylformamide, butyl alcohol.

The disadvantages of this method are:

1. In the known solution, we used a large excess of formic acid, which provides a relatively high selectivity to the salt of manganese (II) even when using alcohols as solvents liquid phase system. Not about evide absence of direct interaction of manganese with alcohols, if you carry out the process without excess acid, or the lack of it.

2. Of fatty acids formic considered to be relatively strong (PKand=3,8). Many other carboxylic acids have higher values PKandfor phenols PKand~10, and alcohols 14-18. However, these characteristics are found in aquatic environments. It is not certain that this proportion will remain in non-aqueous environments and at the same time will not depend on the nature of the non-aqueous environment, as well as the fact that the magnitude of the PKandwill strongly determine the competitive ability of the acid components of the reaction mixture in direct interaction with the metal. It is not excluded options when marked impact may not be too strong, and even missing completely.

3. In the known solution contains manganese oxides, which can also interact with acids and other components. Not predictable, as their presence will affect the direct interaction of the metal with alcohols and competitive ability of such interaction

The objective of the proposed solution is to find such conditions interaction of manganese with alcohols, so it was quantitative in respect of the reagent shortage, proceeded with technologically acceptable speeds and would lead to the accumulation of the main mass of the product predominantly in the solid phase, which could easily be separated by simple filtration.

This object is achieved in that the liquid phase take the appropriate alcohol in the weight ratio of glass beads of 1:1.5, manganese metered quantity of 5.81-43,3% by weight of the liquid phase, the process begins at room temperature and are in the control method of sampling and determination of the content of compounds of manganese (II) to almost quantitative stock-out loaded metal, after which the stirring agitator bead mill ceased, the suspension of the reaction mixture is separated from the beads and sent to the filtration, the precipitate of alcoholate washed with solvent liquid phase and is directed to purification by recrystallization, and the filtrate and the wash liquid phase with traces of dissolved alcoholate in return repeated the process.

At the same time as alcohol use1-C5fatty alcohols normal, isotrate, cyclohexanol, ethyl cellosolve and ethylene glycol.

Characteristics of the raw materials used

Manganese reactive GOST 6008-90.

Methanol technical GOST 2222-95.

Ethyl alcohol according to GOST 18300-87.

n-Propyl alcohol, GOST 9805-84.

ISO-Propyl alcohol according to GOST 9805-84.

n-Butyl alcohol according to GOST 6006-78.

ISO-Butyl alcohol according to GOST 9536-79.

Pentanol-1 on THE other 6-09-3467-79.

and what about the-Amyl alcohol according to GOST 5830-70.

The cyclohexanol in THE 3-03-358-83.

The ethyl cellosolve according to GOST 8313-88.

Ethylene glycol according to GOST 10164-75.

The process of the inventive method the following. In ball mill vertical type load rated amount of the glass beads, the corresponding alcohol as a liquid phase reaction mixture and at the same time reagent and manganese metal. Include mechanical mixing and the time taken for the beginning of the process. On his turn take samples of the reaction mixture, which determine the content of compounds of manganese (II). The solubility of the alcoholate of manganese in alcohols is very small, so the bulk of the product is accumulated in the solid phase. When the amount of accumulated product is close to the calculated value, the stirring agitator bead mill ceased, the suspension of the reaction mixture is separated from the glass beads, and then filtered. The precipitate product is washed to be used as the reagent and the liquid phase alcohol and shipped if necessary, at additional purification by recrystallization. And the filtrate and wash the alcohol back into the re-download process.

Example No. 1.

In ball mill vertical type with glass enclosure in the form of a thick-walled glass inner diameter of 55 mm and a height of 114 mm, equipped with Vysokoe orotol (1440 rpm) paddle stirrer made of durable fiberglass with a rectangular blade 52×40 mm, reflux-condenser and a liquid stabilizing the temperature of the bath, loaded sequentially 150 g of glass beads with the diameter of the balls in the range from 1.5 to 2.8 mm, 100 g of ISO-propyl alcohol and 13 g of manganese. The reactor is put into place in the frame the frame is properly connected to the cover and through it with reflux-condenser, bring water stabilizing bath, cooling water in a reflux-condenser, include mechanical mixing and the time taken for the beginning of the process. The temperature of the reaction mixture at this point was 19°C.

During the process, take samples of the reaction mixture, which control the content of compounds of manganese (II). This sampling is conducted without stopping the mechanical mixing. Made determination showed that 25, 50, 75 and >98%degree of conversion of the downloaded manganese achieved respectively for 25, 55, 105 and 165 minutes after reaching almost complete consumption of the loaded metal mixing in a bead mill ceased. The temperature of the reaction mixture at this point was 34°C. Stop the flow of water in a reflux-condenser, placing a stabilizing bath, disconnect the lid of the reactor and remove the reactor from its slot in the frame frame. The suspension of the reaction mixture is separated from clanlogo beads passing through the wall in a grid with a cell size of ~0.3×0.3 mm, and then filtered. The reactor is assembled, the stirrer and the beads when working stirring rinsed with 30 g of ISO-propyl alcohol. Resulting mixture is sent to the flushing of sediment on the filter. The filtrate and the washing solvent is directed to the re-download process, and the residue of the product on purification by recrystallization.

The product yield without taking into account losses during recrystallization was 0,235 mol. The degree of transformation of manganese in the product is more than 99%.

Examples No. 2-8.

The reactor, the nature of the reagents, the ratio of the mass download of glass beads and alcohol, order, load, start-up and maintenance process, as well as unloading of the reaction mixture, it is separated from the glass beads and the allocation of alcoholate product, as well as monitoring the progress of the process and the determination of the moment of termination is similar to that described in example 1.

Different initial dosage of manganese on interaction with alcohol. Load characteristics, the process and the results are shown in table 1.

Table 1
Load characteristics,
process and product yield
Example No.
2 345678
download manganese, mol/kg1,01,41,72,252,804,205,50
the temperature in the beginning of the process, °C19202218181820
the time to reach the degree of conversion of the downloaded manganese, min:
0,2560312721191316
0,5012890 7860352745
0,75192155135116684588
0,902312151781449085138
>9828726323319311595175
the temperature at the time of the termination process, °C23242632374844
the yield of the product (excluding
losses during recrystallization), mol0.104 g0,1490,1850,2540,3280,5410,764
the degree of transformation of manganese in the target product, %
98,098,598,599,0of 99.1of 99.197,0

Examples No. 9-18.

The reactor, the mass ratio of downloads glass beads and sleep is the one the initial content of manganese in the load, the operation of launch and implementation process, monitoring the progress of his passing, stopping, separating the reaction mixture from the beads and the selection of its product similar to that described in example 3. Different nature used alcohol. The nature of alcohol and the results are shown in table 2.

The positive effect of the proposed solution consists of:

1. In the proposed method there is no auxiliary reagents, catalysts and additives, which would not set its mass to the target product.

2. In the proposed solution, there is no wastewater and the need to use external supply of heat.

3. This process allows operation with a lot of alcohol on a single technology and in the same equipment.

4. Instrumentation the claimed process is simple and does not contain boiler-supervising devices.

5. The separation of the target product from the reaction mixture by filtration, returning the filtrate and the wash of alcohol in the re process. Recirculation of the product with the specified return is small, which is predetermined very poor solubility of the alcoholate in alcohol, from which he received.

1. The method of producing alcoholate of manganese (II) direct interaction of the metal with alcohol in a bead mill, vertical the social type, characterized in that the liquid phase take the appropriate alcohol in the weight ratio of glass beads of 1:1.5, manganese metered quantity of 5.81-43,3% by weight of the liquid phase, the process begins at room temperature and are in the control method of sampling and determination of the content of compounds of manganese (II) to almost quantitative stock-out loaded metal, after which the stirring agitator bead mill ceased, the suspension of the reaction mixture is separated from the beads and sent to the filtration, the precipitate of alcoholate washed with solvent liquid phase and is directed to purification by recrystallization, and the filtrate and wash the liquid phase with traces of dissolved alcoholate in return repeated the process.

2. The method according to claim 1, characterized in that as alcohol use1-C5fatty alcohols normal, isotrate, cyclohexanol, ethyl cellosolve and ethylene glycol.



 

Same patents:

FIELD: medicine.

SUBSTANCE: new pure syn-aminoacids of formulas I and II have ability of specific binding in biological system and may be used to produce image of tumor. II and I. In formulae I and II Y and Z are independently selected from group made of CH2 and (CR4R5)n, n=1, 2; R1-R3 are independently selected from group made of H and alkyl C1-C4; R4, R5 = H and R7 = 18F. Invention is related to method of synthesis of syn-aminoacids with formula II, which includes stages of ketone transformation into trans-spirit of formula I and transformation of produced trans-spirit into syn-aminoacid of formula II, and also to pharmaceutical composition for production of tumor image and method for production of tumor image.

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12 cl, 1 tbl, 3 dwg, 3 ex

FIELD: chemistry.

SUBSTANCE: method of synthesis of manganese (II) fumarate through direct reaction of metal with acid is presented. The process is carried out in a vertical type bead mill with mass ratio of beads to the reaction mixture equal to 1:1, and the liquid phase is a solution of fumaric acid in an organic solvent with content of acid of 0.70-1.80 mol/kg. Manganese is taken in stoichiometric amount with acid or in deficiency of up to 5%. The process is started by loading the liquid phase solvent and acid and preparation of the acid solution in a bead mill, after which metal is loaded and the process is carried out at temperature ranging from 25 to 35°C while preventing spontaneous increase of temperature through forced cooling and controlling through sample taking and determination of manganese salt in the samples and residual amount of acid until attaining values close to calculated values during quantitative conversion of the reagent in deficiency. After that stirring and cooling are stopped. The suspension of the reaction mixture is separated from the glass beads, cooled to temperature between 5.2 and 6.2°C and filtered. The filtering residue is washed with the liquid phase solvent, cooled to approximately the same temperature, and taken for purification by recrystallisation. The filtrate and the washing solvent are returned to the repeated process.

EFFECT: method is easy to implement, the end product can be easily separated and there are no auxiliary materials which contaminate the obtained product.

2 cl, 11 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an improved method of producing manganese (II) fumarate from manganese metal and its oxide (III) through direct reaction of the metal and its oxide Mn2O3 with an acid in the presence of a liquid phase and a stimulating iodine additive in a vertical type bead mill with glass beads as grinding agent. The metal and its oxide are loaded in molar ratio (2±0.1):1 in total amount of 7.87 to 10.93% of the mass of the load. Acid is added with 15 to 25% excess of the calculated value, equal to the number of moles of metal and twice the number of moles of metal oxide in the load. The base of the liquid phase is isoamyl alcohol, in which the iodine stimulating additive is dissolved in amount of 0.02 to 0.05 mol/kg. Glass beads are loaded first, in mass ratio to the reaction mixture of 1.35:1, and then later the liquid phase solvent, acid and stimulating additive, and after brief stirring, metal oxide and metal, stirring all the while. Taking this moment as the beginning of the process, forced cooling is introduced right away. Operating temperature is stabilised in the range 33 to 45°C and in this mode, the process is carried out until virtually quantitative conversion of metal and its oxide to the target salt, after which stirring and forced cooling are stopped. The reaction mixture is separated from the glass beads, cooled to temperature 5 to 6°C and kept at that temperature for 1 to 2 hours. The solid phase of the target salt is filtered off and washed with isoamyl on a filter cooled to approximately the same temperature, after which it is taken for purification by recrystallisation. The filtrate and the cleaning solvent, containing excess acid, the bulk of the stimulating additive and a certain amount of dissolved target salt, are returned for loading in the repeated process. The process is carried out in light temperature conditions. The target substance can be easily separated.

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9 ex

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22 cl, 12 ex, 3 dwg, 2 tbl

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2 cl, 13 ex, 2 tbl

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

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16 ex, 2 tbl

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3 ex, 1 tbl

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3 cl, 9 ex

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5 cl, 1 tbl, 5 ex

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1 tbl, 14 ex

FIELD: metallic coatings.

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7 cl, 2 ex

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EFFECT: obtaining desired product with high output and regioselectivity.

1 tbl, 5 ex

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