The method of obtaining isovalerianic acid

 

(57) Abstract:

The inventive product is isovalerianic acid, C5H10O2so Kip. 176-177°C. ; n1D5=1,4064, -0,9331 g/cm3(18°C). Reagent 1: isoamyl alcohol. Reagent 2: oxygen-containing gas. Reaction conditions: at 50-130°C and 0 to 10 MPa at a stationary layer of the catalyst is palladium on charcoal in an aqueous-alkaline medium.

The invention relates to an improved method for producing a isovalerianic acid, which is used as intermediate for synthesis of medicines (sedatives, Corvalol) and odoriferous substances.

A method of obtaining isovalerianic acid oxidation by oxygen isoamyl alcohol to aldehyde in the presence of a catalyst - silver on the pumice, and oxidation of the resulting aldehyde to isovalerianic acid air at 10-30aboutIn the presence of acetate of lead or manganese [1].

The main disadvantages of this method is the explosion process and multi-stage.

A method of obtaining isovalerianic acid oxidation isoamyl alcohol in an alkaline medium at 30-65aboutC and current density 3-13 A/DM2in electroche the Main disadvantages of this method are the complexity of the hardware design process, energy consumption and relatively low yield of isovalerianic acid. The closest in technical essence is a method of obtaining isovalerianic acid (CPI) oxidation isoamyl alcohol (IAS) in aqueous-alkaline solution of potassium permanganate at a temperature of not more than 21aboutWith subsequent acidification of the reaction mass and the release of the CPI by distillation. The output of the CPI is 68-72 mol.% [2].

The main disadvantages of this method are the low yield of the CPI and the formation of equimolar quantities of waste production of oxides of manganese.

Technical solution to the problem is the increase in the output of the CPI and the elimination of waste oxides of manganese.

This task is solved by the oxidation of IAS in aqueous-alkaline medium with subsequent acidification of the reaction mass and the release of the CPI by distillation, the distinguishing feature of which is the execution of the process at 50-130aboutWith and 0-10 MPa at the stationary layer of the catalyst is palladium on charcoal and used as the oxygen-containing oxidant gas.

P R I m e R 1. The oxidation process of the IAS carried out in a vertical tubular flow type reactor equipped with thermostatically part of the reactor continuously at a rate of 0.6 kg/h serves mixture composition, wt.%: water 87,0; IAS 8,8; NaOH 4,2, and air at a rate of 140 l/h Temperature in the reactor is maintained at 60aboutC. a pressure of 2 MPa. The gas-liquid mixture leaving the reactor is cooled to room temperature, is sent to the separator type gas-liquid, where the separated water and the organic phase composition, wt.%: water 87,8; IAS 0,3; NaOH 0.3; the sodium salt of the CPI to 11.6. Water and the organic phase is acidified with sulfuric acid to pH 3, separating the upper organic layer and expose its distillation. For 8 hours of continuous operation filed 0,422 kg (4.8 mol) of IAS. After separation obtained 0,464 kg (4,55 mol) isovalerianic acid, having the following characteristics: tKip= 176-177aboutS; nD15= = 1,4064; = 0,9331 g/cm3(if 18aboutC). The output of isovalerianic acid was 95,0 mol.%.

P R I m m e R 2. The oxidation process is carried out analogously to example 1, the feeding to the reactor inlet, filled heterogeneous catalyst -1% PD on charcoal AR-3, mixture composition, wt.%: water 80,5; IAS 13,2; Paon 6,3, at a rate of 0.5 kg/h as the oxidant used technical oxygen content of the main substance of 94%. The feed rate of oxygen of 25 l/h Temperature in the reactor is maintained at level 80aboutWith the pressure to 0.5 MPa. For 8 h some, with the following parameters: tKip= 176-177oS; nD15= 1,4063; = 0,9333 g/cm3(18 deg.C). The output of the CPI - 90,4 mol.%.

P R I m e R 3. The process is carried out analogously to example 1 at a temperature of 110aboutC and a pressure of 7 MPa. The output of the CPI 0,429 kg (4,21 mol) - 87,8 mol.%. Quality acid analogous to example 1.

P R I m e R 4. The process is carried out analogously to example 1, using as catalyst (5% Pd on charcoal brand ARB and implementing the process at 130 deg. C and 10 MPa. After highlighting receive the CPI with the following characteristics: tKip.= 176-177aboutS; nD15= 1,4062; = =0,9331 g/cm3(if 18aboutC) and the output 0,405 kg (3,98 mol) 83,0 mol.%.

P R I m e R 5. The process is carried out analogously to example 2 at 50aboutAnd atmospheric pressure. The output of the CPI amounted to 0,391 kg (3,83 mol) - 85,1 mol.%. Qualitative characteristics of acid analogous to example 2.

The process in this way allows to increase the output of the CPI with 68-72 up 83-95 mol.% in the absence of waste production of oxides of manganese.

The METHOD of OBTAINING ISOVALERIANIC ACID interaction isoamyl alcohol with an oxidizing agent in an aqueous-alkaline medium, characterized in that oxidize the lyst - palladium on charcoal.

 

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2 tbl, 2 dwg, 1 ex

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1 tbl,1 ex

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