Method for preparation of manganese oxalate (ii)

FIELD: chemistry.

SUBSTANCE: invention is related to improved method for preparation of manganese oxalate (II) by means of direct interaction of metal with acid in bead mill in presence of liquid phase, in which manganese and oxalic acid are loaded into bead mill in stoichiometric ratio in amount of 0.75-2.4 mole/kg of load at mass ratio of load and glass beads of 1:1.2, liquid phase dissolvent used is water or organic substance, or mixture of organic substances; loading is carried out in the following sequence: liquid phase dissolvent, acid, then metal; process is started at room temperature and is carried out under conditions of forced cooling in the temperature range of 18-39°C with control over procedure by sampling method to practically complete spend of loaded reagents for product making, afterwards mixing and cooling are terminated, suspension of reaction mixture is separated from glass beads and filtered, salt deposit is sent for product cleaning from traces of non-reacted metal, and filtrate is returned into repeated process.

EFFECT: method makes it possible to produce target product in absence of manganese dioxide and stimulating additive at temperatures close to room temperature.

2 cl, 13 ex, 2 tbl

 

The invention relates to the technology of producing oxalate, manganese (II) and can be used in various fields of chemical practice, analytical control and scientific research.

A known method of producing oxalate, manganese (II) (Remy, the Rate of inorganic chemistry. Vol.2. M.: Mir, 1966. 836 C.), whereby a hot solution of oxalic acid is poured to a hot dilute solution of salt of manganese (II) or suspension of manganese carbonate in hot water, the result is the oxalate dihydrate manganese (II) MnC2O4·2H2O. On cold formed trihydrate MnC2O4·3H2O, which is unstable and goes into dihydrate. By heating the dihydrate above 100°C it becomes anhydrous MnC2O4.

The disadvantages of this method are:

1. The need to have water-soluble salt of manganese (II) or carbonate of manganese (II), which must be obtained.

2. The process is energy-intensive, and the main amount of heat is wasted in heating the solvent - water, which is needed to obtain dilute solutions of the reactants. However, the water included in the composition of the product in the form of crystallization. But the latter is easily lost when heated product in excess of 100°C.

3. The use of dilute solutions inevitably leads to a significant amount of waste is od want to clear from the taken anion salts of manganese in the form of the corresponding acid.

A known method of producing oxalate, manganese (II) (Vasiliev SG, A.A. Granovsky, Tairova A.A. Laboratory work in General and inorganic chemistry. L., Chemistry, 1986, s), based on the stoichiometric equation

7H2C2O4+2KMnO4+2CH3COOH→2MnC2O4+2KOCOCH3+10CO2+8H2O

According to him it is heated to boiling saturated solution of oxalic acid, acidified with acetic acid and slowly poured with stirring to a hot solution of potassium permanganate until slightly pink color, then give the resulting solution was left standing. After coagulation of the precipitate, the liquid is poured, the precipitate washed twice by decantation, filtered, washed with water and dried in a Cabinet at 150°C to remove water of crystallization.

The disadvantages of this method are:

1. The use of expensive and generally scarce oxidant KMnO4.

2. Part of oxalic acid being wasted in carbon dioxide.

3. A large number of initial reagents and the accompanying product potassium acetate, which requires disposal.

4. Quite a diluted aqueous solutions and a large number of leaching predetermine a significant amount of waste in the.

5. Very energy intensive process.

Closest to the claimed is a method of producing manganese acetate (II) (patent RF №2294921), according to which salt is produced by direct interaction of the metal with acid in the presence of manganese dioxide, stimulating supplements of iodine and an organic solvent liquid phase system in a bead mill, vertical type with a reflux-condenser, a high-speed paddle stirrer and glass beads as pereirago agent. Load metal and dioxide taken in a molar ratio of 1:1 in the amount of 11.8% by weight of the liquid phase, the liquid phase comprises an organic solvent and acetic acid with a concentration of 3.4-5 mol/kg and dosed in a mass ratio of glass beads of 1:1.5. In the liquid phase dissolved iodine in the amount of 0.025-0,070 mol/kg liquid phase. Loading is carried out in sequence: liquid phase or its components separately, iodine, metal and oxide of the metal. And the process starting at room temperature and lead to the almost complete consumption of dioxide. The resulting suspension of the salt is separated from the main part of the unreacted metal and glass beads, and is directed to the filtering. The precipitated salt is cleaned from impurities of the metal and its oxide by recrystallization, and the filtrate is sent to the re process. The organic solvent used ethyl cellosolve, ethylene glycol, 1,4-dioxane, isoamyl and n-butyl alcohols, and the presence in the liquid phase system of water up to 4% does not affect the characteristics of the process. The disadvantages of this method are:

1. Acetic acid is monobasic and rather weak (pKa=4.8V). Oxalic acid is dibasic and much more strongNot necessarily and it's obviously not a favorable variant of the process of obtaining salts of acetic acid will be suitable for oxalic acid.

2. Oxalic acid is a strong reducing agent, and manganese dioxide is quite a strong oxidizer. Therefore, when their joint presence in the reaction mixture in a bead mill between them may direct redox interaction. From this point of view, the simultaneous presence of these reagents in the same reaction mixture is unlikely to be reasonable.

3. It is not excluded direct interaction of oxalic acid with manganese, if this interaction is carried out in a bead mill, to ensure effective destruction of the blocking of the protective film of the product on the metal surface.

4. No it is obvious that the interaction of manganese with oxalic acid iodine is p is havlat its stimulating properties and its presence is mandatory in the initial download.

5. There is no reason to expect a favorable solvents for the liquid phase upon receipt of manganese acetate will remain in the same process of obtaining manganese oxalate.

The objective of the proposed solution is to select such a solvent liquid phase system and process conditions in a bead mill, in which the manganese oxalate would be by direct interaction of the metal with an acid in the absence of manganese dioxide and stimulating supplements of iodine at close to room temperatures.

The problem is solved in that the manganese and oxalic acid load in the ball mill in the stoichiometric ratio in the amount of 0.75 to 2.4 mol/kg loading weight ratio of load and glass beads 1:1,2; as solvent liquid phase using water or an organic substance or a mixture of organic substances; loading lead to sequence the solvent liquid phase, acid, and then the metal; the process begins at room temperature and is carried out in conditions of forced cooling in the temperature range 18-39°C while monitoring the flow method of sampling to practically complete consumption of the loaded reagent to form a product, after stirring and cooling stops, the suspension of the reaction mixture is separated from the glass is of Ysera and filtered, the precipitated salt is directed to the purification of the product from traces of unreacted metal, and the filtrate is returned to repeat the process. As the organic solvent of the liquid phase take ethyl cellosolve, butyl acetate, n-propyl alcohol, n-butyl alcohol, toluene, xylene and white spirit.

Characteristics of the raw materials used

Manganese reactive GOST 6008-90

Oxalic acid according to GOST 22180-76

Distilled water according to GOST 6709-72

m-Xylene (TU 6-09-2438-77)

White spirit technical GOST 3134-78

Butyl acetate according to GOST 8981-78

n-Propyl alcohol, GOST 9805-84

n-Butyl alcohol according to GOST 6006-78

The ethyl cellosolve according to GOST 8313-88

The process of the inventive method the following. In ball mill vertical type that have a direct connection with a reflux-condenser and forced cooling load calculated number of glass beads, solvent, liquid phase, oxalic acid and manganese metal, down the cooling bath and include mechanical stirring, taking this moment as the beginning of the process. During the process, take samples of the reaction mixture, which determine the salt content of manganese (II) and the residual amounts of acid and also lead temperature control. The exothermic process that determines the growth rate is atory during the course. Therefore, the forced cooling of the injected effectively from the outset.

As soon as the current control shows the almost complete withdrawal of all loaded acids for salt formation, work bead mill ceased. The reaction mixture is in the form of a suspension of the product is separated from the glass beads by filtration through a grid as a filtering partition with cell sizes(0,3-0,4)×(0,3-0,4) mm, and then filtered. The precipitate is washed with a solvent liquid phase and sent to clean up the traces of unreacted metal and oxalic acid, and the filtrate and the washing solvent is returned to re-process

Example No. 1.

In a ball mill with glass enclosure and high-speed (1440 rpm) paddle stirrer, shaft and blade which is made of textolite, equipped with a reflux-condenser and the high inertia of the cooling bath, a load of 120 g of glass beads and 100 g of the initial reaction mixture containing 81,9 g of ethyl cellosolve as a solvent, of 12.6 g of oxalic acid with two molecules of water of crystallization and 5.5 g of manganese. The reactor is placed in a special slot in the frame frame, combined with a lid, which contains the agitator stuffing box, slot sampler and socket for thermocouple and the outlet on the back of holodilniktelevizor, fixed in the working position, is connected with a reflux-condenser, down the cooling bath so that the reactor vessel was immersed in it at least 70-80% of its height, include mechanical mixing and the time taken for the beginning of the process.

During the process, take samples of the reaction mixture, which determine the content of manganese oxalate and the residual content of acid. The process is exothermic. Therefore, when sampling is fixed and the temperature in the reaction zone. In this example, it ranged from 27°C at the beginning to 30°C at the point of maximum.

As soon as virtually all of the acid is spent on the education of salt (in this case through 116 min) stop stirring, the reaction mixture is separated from the glass beads by passing through the filter wall with cell sizes(0,3-0,4)×(0,3-0,4) mm, and then filtered. The precipitated salt is washed on the filter with a solvent and is directed to the purification of the remaining traces of metal, and the filtrate and the washing solvent in return repeated the process.

The output of manganese oxalate was 0,098 mol. The utilization of the acid to the target product was 98%.

Examples No. 2-8

The reaction apparatus, loading weight and the ratio by weight of glass beads, the mass ratio of the loaded reagents sequence operas the Nations download process for monitoring flow, separating the reaction mixture from the beads, the precipitate of the salt wash solvent, and further purification of salt, as well as the criterion for determining when termination process similar to that described in example 1. Different nature of the used solvent, time and temperature characteristics of the process. The results are shown in table. 1.

Table 1

Load characteristics and processExample No.
2345678
The nature of the used solvent liquid phasewaterBU-Tyl-ACE-tatn-propyl alcoholn-butyl alcoholtoluenem-xylenewhite spirit
The time to reach
degree
turning, min
50%
2655 3715334038
75%53867440476675
approaching 100%1011351369564120160
Operating temperature range, °C18-2418-2321-2621-2820-3019-2520-24
The output of manganese oxalate, mol0,0970,0990,0970,0990,0980,0980,097
The utilization of the acid to the target product, %9799 9799989897

Examples No. 9-13

The reaction apparatus, the weight of the load and its sequence, the solvent of the liquid phase, the sequence of loading operations, the process, the separation of the reaction mixture, the criterion of the date of termination of the process is similar to that described in example 1. Different mass ratio of the reagents and solvent loading, time and temperature characteristics of the process. The results are shown in table. 2.

Table 2

Load characteristics and processExample No.
910111213
Download:
the solvent, g86,479,771,063,856,6
the margana is C, mol/kg0,751,41,62,02,4
oxalic acid·2H2O, mol/kg0,751,41,62,02,4
The time to reach the degree of transformation, min:
50%3514161730
75%7427303465
approaching 100%140687583130
Operating temperature range, °C22-2818-3920-3918-39 19-36
The output of manganese oxalate, mol0,073was 0.138strength of 0.1590,1980,236
The utilization of the acid to the target product, %97,398,699,499,098,3

The positive effect of the proposed solution consists in the following:

1. The basis of this method is simpler chemical interaction with the formation of a salt and hydrogen as a co-product that accumulates in the reaction mixture in small quantities and from which you do not need to clear the target product.

2. For carrying out process does not require the use of a stimulating supplements, making the reaction mixture is simpler and does not require the allocation of products of transformation of stimulating additives, and cleaning away the last of the target product.

3. As a solvent of the liquid phase is allowed to use distilled water, and without serious complications in implementation stages and losses in a time consuming process.

4. The process is relatively fast and almost to depletion taken stechiometric the ski ratios of metal and acid, which greatly facilitates the selection of the target product and its cleanup.

5. Process low flows at close to room temperatures and can maintain the necessary thermal conditions due to its reaction heat.

1. The method of producing oxalate, manganese (II) by direct interaction of the metal with the acid in a bead mill in the presence of a liquid phase, characterized in that the manganese and oxalic acid load in the ball mill in the stoichiometric ratio in the amount of 0.75 to 2.4 mol/kg loading weight ratio of load and glass beads 1:1,2, as a solvent of the liquid phase using water or an organic substance, or a mixture of organic substances; loading are in order: solvent liquid phase, acid, and then the metal; the process begins at room temperature and is carried out in conditions of forced cooling in the temperature range 18-39°C while monitoring the flow method of sampling to practically complete consumption of the loaded reagents for the formation of the product, after which the stirring and cooling stops, the suspension of the reaction mixture is separated from the glass beads and filtered, the precipitated salt is directed to the purification of the product from traces of unreacted metal, and the filtrate is returned to repeat the process.

2 the Method according to claim 1, characterized in that the organic solvent liquid phase take ethyl cellosolve, butyl acetate, n-propyl alcohol, n-butyl alcohol, toluene, xylene and white spirit.



 

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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.

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16 ex, 2 tbl

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4 cl, 1 dwg, 11 tbl, 33 ex

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8 cl, 4 ex

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7 cl, 2 dwg, 3 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention refers to platinum metal salts synthesis, specifically palladium salts, namely palladium (II) acetate applied as catalyst or for production of initial salt for other palladium salts. Method of palladium acetate production includes as follows. Metal palladium is dissolved in concentrated nitric acid. Prepared solution is steamed prior to crystallisation of palladium nitrate salt, processed by ice acetic acid. Deposition is filtered and processed with ice acetic acid. Nitrate palladium solution is processed with ice acetic acid with sodium acetate additive in amount 1.5 - 2 kg per 1 kg of palladium in solution. Deposition is processed and dissolved in ice acetic acid in ratio 19-21 l per 1 kg of deposition with acetamide added in amount 0.1 - 0.2 kg per 1 kg of deposition. Solution is warmed at temperature 80 - 90 °C within at least 5 h and steams until salt is formed.

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2 cl, 2 tbl, 4 ex

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EFFECT: improved method of production of formic acid formates.

10 cl, 4 ex

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