Method of producing palladium trifluoroacetate

FIELD: chemistry.

SUBSTANCE: method includes dissolving palladium metal in concentrated nitric acid and evaporating the obtained solution. The palladium nitrate solution is evaporated at (40-80)°C until palladium nitrate begins to crystallise. The formed solution at (30-80)°C is mixed with trifluoroacetic acid in amount of (600-800)% of the molar amount of palladium in the starting palladium nitrate solution or trifluoroacetic acid anhydride in amount of (350-450)% of the molar amount of palladium in the starting palladium nitrate solution until the end of crystallisation of polymeric palladium trifluoroacetate. The method also includes filtering the formed compound and conversion thereof into the end product by adding acetonitrile at (10-30)°C with weight ratio of the compound to acetonitrile of 1:(0.5-2).

EFFECT: invention improves the method of producing palladium trifluoroacetate in a crystalline monophase state, improves synthesis stability and enables to achieve high output of the desired compound.

2 cl, 2 tbl, 2 ex

 

The invention relates to the field of chemistry of the platinum metals, in particular the synthesis of the palladium compounds, namely, getting trifenatate palladium (II), used as a reagent for organic synthesis, a constituent of the catalysts precursors of other compounds of palladium, preparation of various palladium-containing materials and for the deposition of palladium metal by the method of gas-phase pyrolysis.

A known method of producing trifenatate palladium interaction of palladium acetate with triperoxonane acid by evaporation of excess triperoxonane acid and substituted acetic acid, and curing the obtained residue under vacuum at 40°C (N.A. Stephenson, Morehous S.M., A.R. Powell, Heffer.J.P., Wilkinson G.//J. Chem. Soc. 1965. No. 6. p.3632-3640). The disadvantage of this method is to obtain the substance in the polymer crystalline modification - Catena-[Pd(CP3COO)2]nthat has no volatility, in contrast to molecular crystalline form [Pd3(CF3COO)6] (with volatility). Obtaining source material, palladium acetate requires its scheme, that leads to the expenditure of additional reagents and increases the duration of the whole process. For the almost complete substitution of acetate groups by trifurcation use a large excess of triflorus the Noah acid (more than 150 times higher than the stoichiometric value), that increases the cost of obtaining the target product.

A known method of producing trifenatate palladium by voshon product interaction, obtained by the previous method, when heated to 190-200°C in vacuum of 1.33-0.133 PA and its dual sublimation (Gerbeleu NV, Timko GA, Indican K.M., Popovich GA // Theoretical and experimental chemistry. 1986. No. 3. s-330). The disadvantage of this method is incomplete Vashon substances because of the difficulty of transition in the crystalline state of polymer modification trifenatate palladium in molecular and, respectively, low yield (25%).

A method of obtaining palladium propionate, consisting in processing one stripped off solution of palladium nitrate anhydride propionovoi acid (Murahaleen Russia, having got, S.D. Kirik, // RF Patent №2430926 dated 10.10.2011. Bull. No. 28.). One stripped off the solution of palladium nitrate, before the introduction of the anhydride propionic acid, may be a precursor of triptoreline palladium. This method is adopted for the prototype.

The disadvantage of this method is the lack of stability of the ethyl group in propionic acid or its anhydride to nitrouse and oxidative capacity of nitronium cation generated in the system nitric acid - anhydride propionic acid. Triperoxonane acid or its anhydride are more resistant to such interactions.

The technical result, which directed the alleged invention is an improved method of producing trifenatate palladium(II) in the crystal monophase state [Pd3(CF3COO)6], the stability of the synthesis, as well as achieving a high yield of the target compound.

The specified technical result is achieved by the fact that the original solution of palladium nitrate, which was prepared by dissolving palladium mobile in concentrated nitric acid, evaporated at a temperature (40-80°C)prior to the crystallization of palladium nitrate, and the resulting solution at a temperature (30-80)°C add triperoxonane acid number (600-800) % of the molar amount of palladium in the original solution of palladium nitrate or anhydride triperoxonane acid number (350-450) % of the molar amount of palladium in the original solution of palladium nitrate to stop the crystallization of polymer trifenatate palladium, filtering the resulting compound and its translation in the target product by adding acetonitrile at a temperature (10-30°C)at a mass ratio connection: acetonitrile - 1:(0.5-2). After transfer of the polymer trifenatate palladium target product acetonitrile is evaporated at a temperature (10 to 30)°C.

The essence of the method consists in t is m, what education target trifenatate palladium in molecular tricyclic form [Pd3(CF3COO)6] precedes the selection of the polymer modification - catena-[Pd(CF3COO)2]nthat is partially soluble in the reaction medium and can be translated in molecular form by recrystallization. To highlight the polymer forms trifenatate palladium used the interaction of a solution of palladium nitrate with triperoxonane acid or its anhydride. With the substitution of nitrate groups on trifenatate processes of ionization of nitric acid with the formation of the nitronium cation and the anhydride of nitric acid. Since N2O5thermally unstable and decomposes to form nitrogen dioxide and oxygen, which, for the most part, removed from the reaction system, and it allows you to reduce the amount of nitrate compounds. The appearance in the system of oxygen compounds of nitrogen (IV) is a condition for the manifestation nitrogenous agents that, apparently, promotes reversible coordination interactions of palladium and nitrosyl group, and is the key in choosing the path of crystallization in polymer carboxylate.

Recrystallization catena-[Pd(CF3COO)2]nin [Pd3(CF3COO)2] due to the greater thermodynamic Usto the strains trinuclear molecular forms (which exists in the gas phase). To implement such a transition with a high yield of the target compounds is important to select a solvent, since triptorelin palladium in solution is a reactive compound and is capable of activate, for example, such solvents as acetone, ethers, esters or toluene. The author's research showed that of the available solvents may be used acetonitrile. But at the same time, quantitative transition (without side activation processes acetonitrile) can only happen without a lot of excess solvent, its high purity and at relatively moderate temperatures.

In the course of the research it was established that the process of obtaining trifenatate palladium (II) from a solution of palladium nitrate and triperoxonane acid or its anhydride, the optimal parameters are:

- temperature evaporation of a solution of palladium nitrate - (40-80°C);

- evaporation of a solution of palladium nitrate prior to the crystallization of palladium nitrate;

the temperature in the interaction of a solution of palladium nitrate with triperoxonane acid or its anhydride (30-80)°C;

- the number of added triperoxonane acid (600-800) % of the molar amount of palladium in the original solution of palladium nitrate;

- the number of added anhydride is referencesee acid (350-450) % of the molar amount of palladium in the original solution of palladium nitrate:

- the temperature of the intermediate transfer polymer trifenatate palladium in the target product (10-30°C);

- mass ratio connection: acetonitrile when recrystallization is 1:(0.5-2);

- temperature evaporation of acetonitrile after the formation of the target compound (10 to 30)°C.

The increase in the temperature of the evaporation source solution of palladium nitrate above 80°C can lead to partial decomposition of the crystallizing palladium nitrate to oxide, because of its insolubility in nitrogen and triperoxonane acids leads to contamination of the product with palladium oxide or requires additional operations - filtering one stripped off solution. This, in turn, requires an increase in the duration of the process. Reducing the temperature of the evaporation source solution of palladium nitrate below 40°C leads to slower evaporation, which increases the duration of the process.

Evaporation of a solution of palladium nitrate, not reaching the crystallization of palladium nitrate, leads to an increase in the content of nitric acid and water in the reaction solution, which further leads to increase spending triperoxonane acid or its anhydride.

The temperature increase interaction solution isotonik the th palladium with triperoxonane acid or its anhydride above 80°C leads to a decrease in the solubility triperoxonane acid or its anhydride because of their evaporation and removal from the zone of interaction, that increases the consumption of reagents. The increase in temperature can lead to boiling of the solution, which may be the reason for the partial removal of substances from the reactor. Reducing the temperature of the interaction of a solution of palladium nitrate with triperoxonane acid or its anhydride below 30°C leads to the insufficient decomposition of nitrogen dioxide, which is not sufficiently reduces the content of nitrate compounds and increases the solubility of the intermediate product - polymer trifenatate palladium.

The increase in the number of added triperoxonane acid more than 800% of the molar amount of palladium in the original solution of palladium nitrate leads to the excessive consumption of reagent. Reducing added triperoxonane acid of less than 600% of the molar amount of palladium in the original solution of palladium nitrate leads to its disadvantage in the formation of the intermediate product and reduces its output and the target connection.

The increase in the number of the added anhydride triperoxonane acid more than 450% of the molar amount of palladium in the original solution of palladium nitrate leads to the excessive consumption of reagent. Reducing added anhydride triperoxonane acid less than 350% of the molar amount of palladium in the original solution and atomiclog palladium leads to its disadvantage in the formation of the intermediate product, that reduces the output of the whole process.

The increase in the temperature of the intermediate transfer polymer trifenatate palladium target product above 30°C can lead to development of adverse chemical processes involving solvent (acetonitrile), which is a cause of contamination of the target product or neobrazovana. Reducing the temperature of the intermediate transfer polymer trifenatate palladium target product below 10°C requires additional cooling, which complicates the process.

To increase the mass ratio connection: acetonitrile by recrystallization of the intermediate polymer trifenatate palladium target product more than 1:0.5 leads to the lack of solvent for dissolving catena-[Pd(CF3COO)2]nthat leads to incomplete recrystallization and contamination of the target compounds. The mass reduction ratio connection: acetonitrile by recrystallization of the intermediate polymer trifenatate palladium target product less than 1:2 leads to the excess solvent, which leads to excessive dissolution of the target product, thereby reducing its output, or increases the time required for partial or complete evaporation of the solvent.

The increase in the temperature of evaporation of the acetonitrile in the Le of formation of the target compounds above 30°C can lead to activation of the side-chemical processes involving solvent (acetonitrile), what is the cause of the contamination of the target product or translation in an unauthorized connection. Reducing the temperature of evaporation of acetonitrile after the formation of the target compounds below 10°C leads to slower evaporation, which increases the duration of the whole process.

Examples of the method

Example 1

In one stripped off the solution of palladium nitrate at a given temperature and stirring portions was added the calculated amount triperoxonane acid or its anhydride to stop the formation of brown precipitate. The resulting suspension was cooled to room temperature, the precipitate was filtered, washed with triperoxonane acid and was dried on the filter in the flow of dry and clean air. These experiments are shown in table 1. Experiments No. 1 to 6; 13-14 conducted using triperoxonane acid, experiments No. 7-12; 15-16 - using anhydride triperoxonane acid.

The precipitated polymer trifenatate palladium was loaded into the reactor and at a given temperature and stirring was added the required amount of acetonitrile. Dissolving the precipitate of the intermediate occurs almost instantaneously, and then crystallizes the target compound in the form of yellow crystals. The product was separated by filtration and dried on the filter in the flow of ugogo and clean air, then, under reduced or normal pressure in air atmosphere at 20-25°C. these experiments are shown in table 2 (experiments 1-6).

Example 2

The process was carried out according to example 1, but recrystallized target product has not been filtered, and the solvent is evaporated at a predetermined temperature. This has increased the product yield, but increased the duration of the process. These experiments are shown in table 2 (experiments 7-10).

Notes to tables:

I - temperature evaporation source solution of palladium nitrate (°C);

II - the temperature of the solution of palladium nitrate in the interaction with triperoxonane acid or its anhydride (°C);

III - the number of added triperoxonane acid (%) on the molar amount of palladium in the original solution of palladium nitrate;

IV - the number of added anhydride triperoxonane acid (%) on the molar amount of palladium in the original solution of palladium nitrate;

V - output intermediate catena-[Pd(CF3COO)2]n(%) of the amount of palladium in the original solution of palladium nitrate;

VI - data x-ray phase analysis of the intermediate product. The quality of the obtained substances were identified by means of x-ray phase analysis when comparing radiographs with reference to the powder base ICDD;

VII - temperature transfer sub the full-catena-[Pd(CF 3COO)2]nin the target [Pd3(CF3COO)6] (°C);

VIII - mass ratio catena-[Pd(CF3COO)2]n:CH3CN;

IX - temperature evaporation of acetonitrile after the formation of the target compound (°C);

X - exit target [Pd3(CF3COO)6] (%) of the amount of palladium in the intermediate catena-[Pd(CF3COO)2]n;

XI - data x-ray phase analysis of the target product. The quality of the obtained substances were identified by means of x-ray phase analysis when comparing radiographs with reference (unpublished) and dissolved in acetonitrile (if applicable insoluble residue was determined by its mass content).

As shown in the examples, the use of the proposed method can improve the way of obtaining trifenatate palladium (II) in the crystal monophase state [Pd3(CF3COO)6]to increase the stability of the synthesis, as well as to achieve a high yield of the target compound.

Table 1
The method of producing trifenatate palladium (getting catena-[Pd(CF3COO)2]n)
No.IIIIII IVVVI
13060600-78catena-[Pd(CF3COO)2]nwithout impurities
29080700-76catena-[Pd(CF3COO)2]nmixed with PdO
35020700-72catena-[Pd(CF3COO)2]nwithout impurities
46090800-77the same
58030500-70the same
67550 900-77the same
78050-30076the same
88070-50087the same
98020-40083the same
107590-40088the same
113040-35085the same
129050-45088catena-[Pd(CF3COO)2 nmixed with PdO
137570700-76catena-[Pd(CF3COO)2]nwithout impurities
148080700-78the same
158040-40088the same
168050-42088the same

Table 2
The method of producing trifenatate palladium (receive [Pd3(CF3COO)6])
No.VIIVIM*IXXXI
1 51:1-92[Pd3(CF3COO)6] without additives
2401:0.5-90the same
3301:0.25-92[Pd3(CF3COO)6] mixed with catena-[Pd(CF3COO)2]n
4201:3-85[Pd3(CF3COO)6without impurities
5151:2-92the same
6201:1-90the same
7101:0.75quantitative adapter is d the same
8251:140the samesame, but the matter worse kristallizovannye; insoluble residue is less than 0.5%
9201:1.530the same[Pd3(CF3COO)6without impurities
10201:120the samethe same
* Was used acetonitrile brand “reagent grade.”, for additional purification was distilled twice under vacuum over sodium sulfate and P2O5and again without reagents.

1. The method of producing trifenatate by dissolving palladium palladium metal in concentrated nitric acid, concentrating the resulting solution, wherein the solution of palladium nitrate evaporated at a temperature (40-80°C)prior to the crystallization of palladium nitrate, the resulting solution at a temperature (30-80)°C add triperoxonane acid number (600-800) % of Molino what about the amount of palladium in the original solution of palladium nitrate or anhydride triperoxonane acid number (350-450) % of the molar amount of palladium in the original solution of palladium nitrate until the termination of the crystallization polymer trifenatate palladium, filtering the resulting compound and its translation in the target product by adding acetonitrile at a temperature (10-30°C)at a mass ratio connection : acetonitrile - 1:(0.5-2).

2. The method according to claim 1, characterized in that after the transfer of the polymer trifenatate palladium target product acetonitrile is evaporated at a temperature (10 to 30)°C.



 

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5 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: method involves reaction of a metal oxide with an acid in a bead mill in the presence of a stimulant. The process takes place in the presence of a liquid phase, the solvent of which is distilled water. Copper oxide is added in amount of 1.8-3.3 mol/kg in molar ratio to acetic acid equal to (1:1.7)-(1:2.1). The stimulant is added in amount of 0.05 mol/kg. Addition is performed in the following sequence: glass beads, liquid phase solvent, acetic acid, stimulant and copper (II) oxide, in molar ratio of the glass beads to the rest of the material equal to (1:1)-(1.5:1). Further, the material undergoes mechanical mixing and the process is carried out while constantly cooling in temperature range of 20-45°C until almost complete conversion of the loaded copper (II) oxide into a salt. Mixing and cooling are then stopped. The suspension of the reaction mixture is then separated from the glass beads. This suspension is mixed with washing water with reaction mixture residue, left for 1-2.5 hours and filtered. The product residue is thoroughly squeezed and taken for purification via recrystallisation, and the filtrate is returned to repeated process.

EFFECT: invention increases output and selectivity of the method of producing copper acetate.

2 cl, 9 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing tetrahydrate of manganese acetate, relating to chemical engineering of manganese compounds and can be used in producing pure manganese salts used in electronic industry as raw material for making solid-electrolyte capacitors. The method of producing tetrahydrate of manganese acetate involves leaching manganese carbonate with dilute chemically pure nitric acid, followed by filtration, dissolution of manganese carbonate in glacial acetic acid solution, alkalisation of the obtained product manganese acetate solution with aqueous ammonia solution, filtration of manganese acetate solution clarified by settling with separation of a precipitate of impurities from the solution, and evaporation of the solution to concentration 32-32.5 wt %, and addition acetic acid and crystallisation of manganese acetate from the solution by cooling at temperature 50-15°C, and adding into the solution nucleating agents from crystals of the tetrahydrate of manganese acetate in amount of 0.05 wt %, holding the suspension the crystalline manganese acetate precipitate obtained after crystallisation at final crystallisation temperature while stirring constantly, separating the crystalline manganese acetate precipitate followed by washing the crystalline precipitate with a saturated solution of pure manganese acetate and/or acetone at temperature equal to final crystallisation temperature.

EFFECT: obtaining highly pure powdered tetrahydrate of manganese acetate.

8 cl, 2 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an improved method for synthesis of lead (II) acetate through direct reaction of a metal, its dioxide with a carboxylic acid in the presence of an organic liquid phase and a stimulating iodine additive in a vertical bead mill, where the oxidising agent and the reagent in deficit are lead dioxide taken in amount of 0.4-0.6 mol/kg, metal and acetic acid are taken in amount of 0.6-1.5 mol/kg and respectively so as to obtain mol/kg of a salt product, where nPbO2 is amount of lead dioxide in mol/kg. The stimulating additive used is iodine taken in amount of 0.01-0.05 mol/kg liquid phase, the base of which is initially composed of an organic solvent and acetic acid and iodine dissolved in the said solvent. Components of the reaction mixture are loaded in the following sequence: liquid phase solvent, acetic acid, metal, its dioxide, molecular iodine. Mass ratio of the components and glass beads is at least 1:1.5; the process starts at room temperature and is carried out at maximum temperature of 30-50°C under forced cooling conditions and while controlling using a sampling method and determining content of accumulated salt and unreacted lead dioxide and acetic acid in the said samples until the oxidising agent is virtually exhausted, after which the process is stopped. The suspension of the reaction mixture is separated from the glass beads and thin films of unreacted metal by passing through netting with cell size of 0.3×0.3 mm as a filter partition. The beads and unreacted metal are returned to the reactor where together with the housing, mixer and other components of the reactor are washed with the liquid phase solvent from reaction mixture remaining after discharge thereby obtaining a washing solvent; the suspension of the reaction mixture is filtered, the residue on the filter is treated with the washing solvent, pressed well and taken for cleaning through recrystallisation, and the obtained filtrate in a mixture with the washing solvent is returned to the repeated process. Output the filtered off product is 93-98% of the theoretical output.

EFFECT: design of an improved method of obtaining lead acetate.

2 cl, 15 ex

FIELD: chemistry.

SUBSTANCE: method of obtaining palladium acetate involves dissolving palladium metal in concentrated nitric acid, evaporation of the obtained solution and reaction with acetic acid, where the palladium nitrate solution after evaporation, before crystallisation of palladium (II) nitrate salt, is treated with nitrogen (II) oxide or a mixture of nitrogen (II) and (IV) oxides containing not more than 30% nitrogen (IV) oxide and acetic acid at temperature of the solution of 40-90°C with glacial acetic acid consumption of 1.5-2.5 l per kg of palladium in the solution and nitrogen (II) oxide or mixture of nitrogen (II) and (IV) oxides consumption of 1.0-2.0 m3 at normal conditions per 1 l of the initial palladium nitrate solution for 0.5-1.5 hours and the formed solution is heated in a nitrogen atmosphere at 110-140°C for not less than 2 hours with consumption of elementary nitrogen of approximately 30 m3 per 1 m3 of the formed solution.

EFFECT: obtaining palladium acetate in monophase state and avoding formation of impurities of insoluble palladium catena-poly-acetate.

3 cl, 35 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: method of producing zinc stearate involves reacting stearic acid and zinc hydroxide with heating and intense stirring, followed by heat treatment, filtration, drying and packaging. When reacting stearic acid and zinc hydroxide, hydrochloric acid is further added to the mixture as a catalyst. The reaction is carried out in an aqueous medium which is heated to 96-98°C. Circulation is carried out for 2.0 hours. The zinc stearate suspension is then turned into a stable emulsion state and held at that temperature for 30-45 minutes. Further, heat treatment is carried out to aggregate particles, which are then held for 20-25 minutes to solution pH 4.5-5.0, acid number of 5.0 mg and basic substance content of 10-11%. Water is added, followed by stirring and filtering. The precipitate is dried with hot air at temperature of 80-90°C.

EFFECT: invention simplifies production of zinc stearate.

1 tbl, 1 ex

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