The method of obtaining acetic acid from ethyl alcohol

 

(57) Abstract:

The invention relates to an improved method for producing acetic acid, which is widely used in chemical, textile and food industries. The process of vapor-phase oxidation of ethanol to acetic acid by oxygen in the air at the Sn-Mo oxide catalyst is carried out with the aim of increasing the acetic acid concentration in the condenser in a reactor having two working zones (twin system), and the process is carried out at the optimum temperature in each zone: the first from 210 to 300oC and the second from 350 to 390oC, molar ratio of C2H5OH : H2O: air=1:(6,5-0,5):(11: 13) and flow rate of the process in the interval from 3849 up to 5070 (1/hour). table 1.

The invention relates to an improved method for producing acetic acid, which is widely used in chemical, textile and food industries.

A method of obtaining acetic acid vapor-phase oxidation of ethanol on the catalyst MOaVbNbcXewhere X is the number of metals: Li, Na, Be, Mg, Ca, Sr, Ba, Zn, Cd, Hg, Sc, Y, La, Ce, Al, Ti, Zr, Hf, Pb, Ta, As, Bi, Cr, W, Te, Fe, Co and Ni, with a=0.5 and 0.9, b=0.1 to 0.4, c=of 0.001 to 0.2, d= 0.001 to 0.1 and e= 0.001 to 1.0 in [1] Oxidation of SSA in acetic acid is approximately 60%, with virtually complete conversion (98% ) of ethyl alcohol. The concentration of the resulting acetic acid in the condensate reaches 20 to 25 wt.

The disadvantages of this method are: the process at relatively high pressures (up to 75 ATM.), the presence of the diluents (N2and He) in large quantities in the composition of the oxidizing gas mixture, which complicates the selection of the reaction products.

Also known is a method of obtaining acetic acid by oxidation of 20% ethyl alcohol for Sn-Mo oxide catalyst in the vapor phase in a single stage at a temperature of 220 240oC, flow rate 2070 (1/h) volumetric ratio C2H5OH:H2O:for air: N2=1:10:6:5 [2] When complete conversion of ethyl alcohol the yield of acetic acid is 60% of the Catalyst prepared by the method outlined in [3]

The disadvantages of this method include the application of nitrogen to dilute the vapor mixture of the alcohol-air-water, low concentration of the resulting acetic acid in the condensate, which is 10-11 wt.

According to our proposed method, the oxidation of ethyl alcohol kilogram air is carried out in a flow type reactor with two reaction zones (twin system) in the presence of Sn-Mo oxide catalyst. In each of reaction the 210 to 300oC and the second from 350 to 390oC and at a molar ratio of C2H5OH:H2O:air=1:(6,5-0,5): (11-13). A further increase in air leads to a substantial increase in products of deep oxidation, and reduction to the fall of the degree of conversion of ethyl alcohol. The optimum space velocity of the process ranges from 3849 up to 5070 (1/h).

The process in one technological stage in the two-zone reactor allows, in comparison with the prototype, to obtain a condensate containing 35 48% acetic acid with a selectivity for acetic acid is not lower than 60% and full conversion of ethyl alcohol.

The process described in example 1. Other examples are presented in the table.

Example 1. 4,2 ml 28,1% aqueous ethanol solution is supplied from the calibration of burette with Micronesian MA-62 in the upper part of the quartz evaporator, and in the lower part of the supplied air, free from impurities. Air consumption is 13.3 (l/h). Espares, alcohol vapor and air in a molar ratio of C2H5OH:H2O: air=1:6,5:13 directed into the reactor N1.

The reactor N1 is connected in series with the reactor N2 (two reaction zones), and both are to the and correspond to a fraction of 1 2 mm Total volume of active catalyst in both areas was 3.4 ml After reactor N2 has podkonicky refrigerator. The reactors are placed in the oven with electric heating, which is regulated by Latrom.

The reaction mixture from the evaporator enters the upper part of the reactor N1 and moves down through the layer of the first catalyst, and then goes to reactor # 2, after which immediately goes to the refrigerator, where hardening is rapid cooling of the mixture, to prevent further oxidation to CO and CO2. The volumetric rate of the process is 5070 (1/hour). The temperature in the reaction zones 210 in the first and 350oC second, measured chronicleby thermocouple along the entire length of each zone.

The reaction mixture is partially condensed in polcontact the refrigerator and enters the receiver. Neskondensirovannyh gases pass successively United scrubber containing 20 ml of 10% aqueous solution of hydrochloric acid hydroxylamine to capture residual quantities of acetaldehyde, which is followed by watches and gas released into the atmosphere.

The concentration obtained acetic acid was 19.5% with the selectivity of the process for acetic acid 64.4% and complete to the CFU determination of liquid reaction products is carried out by the method of internal standard. As a standard was used accurate canopy isopropanol, selected by retention time on the column PORAPAK q

Analysis of samples was carried out on the chromatograph LHM-80. Columns were filled with media PORAPAK Length of columns to 2 m, diameter 3 mm, the temperature of the evaporator 200oC, the detector temperature 200oC, the column temperature 175oC. the carrier Gas helium, the gas flow rate of 2.4 l/h In the products were determined: water, acetaldehyde, ethanol and acetic acid.

Acetaldehyde, caught in the scrubbers was titrated with 0.1 N. NaOH solution.

The method of gas analysis.

The analysis of gas products was carried out khromotograficheskie on the device coatings-MO.

Column N 1 - molecular sieve H, steel, length 3 m, diameter 3 mm Column N 2 Porarak Q, steel, length 3 m, diameter 3 mm column N of 1 was determined: H2O2N2, CO, on a column of N 2 - CO2. Analysis conditions: evaporator temperature 75oC, the detector temperature and columns 60oC. the carrier Gas argon. The gas flow rate of 1.5 l/H.

The method of obtaining acetic acid from ethyl alcohol vapor-phase oxidation with air oxygen at Sn-Mo oxide catalyst, characterized in that the used reactor with two reaktsionnymiAnd second 350 390oWith, the molar ratio of C2H5OH H2O air 1 (6,5 0,5) (11 13) and the flow rate of the process in the interval 3849 5070 h-1.

 

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1 tbl

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3 cl, 1 dwg, 3 ex, 3 tbl

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