CS267240B1 - Process for producing 9,10-anthraquinone - Google Patents

Abstract

The method of producing 9,10-anthraquinone by selective catalytic oxidation of anthracene in the gas phase is discussed. Its essence is that liquid anthracene is evaporated under tension into a stream of steam and, after mixing with process air, is selectively oxidized to 9,10-anthraquinone on a fixed catalyst bed in an adiabatic controlled tubular reactor. The reaction gases are led to a recuperator, then the partially cooled reaction gases are mixed with fresh air and cooled in a controlled manner to a temperature that is at least 15 °C higher than the dew point of the resulting gas mixture and does not exceed 110 °C. The desubllinated 9,10-anthraquinone is separated on bag filters, the excess content of 9,10-anthraquinone vapors and by-products of organic reaction are washed into water and disposed of.

Description

The present invention provides a process for the production of 9,10-anthraquinone by the selective, catalytic gas phase oxidation of anthracene.

9,10 ~ Anthraquinone is an important semi-finished product for the production of anthraquin dyes. A number of processes are known for obtaining 9,10-anthraquinone from petrochemical and coke chemical raw materials. These include, in particular, the preparation of 9,10-anthraquinone by the Diels-Alder reaction of 1,4-naphthoquinone with 1,3-butadiene (U.S. Pat. No. 2938,913,43870,730, French Pat. No. 217,283, NSR Pat. No. 2,218,316; 180 806, No. 2,245,555, No. 2,532,387.4 2,532,365), FriedelSrafts by the reaction of benzene with phthalic anhydride (Japanese Patents No. 74-30,350, £ 74-95952, £ 74-95055), by oxidation of alkyl-substituted phenylindanes ( NSR Patents 2,500,166,419,344,043, USSR Patent & 410,585, French Patent No. 2,052,598, U.S. Pat. Processes based on the oxidation of anthracene of coke chemical origin are also known. The known processes use the total evaporation of anthracene into the air stream (patent ČSSRfc11O 142), selective catalytic oxidation takes place in a fluidized bed (US patent ξ 2 769 018), condensation chamber systems are used for desublimation and separation of 9,10-anthraquinone (British patent 173 723). The disadvantages of the processes used so far include, in particular, the disproportionate costs of production equipment and raw materials with low selectivity of reactions (synthetic processes from petrochemical raw materials). The hitherto used processes for the production of 9,10-anthraquinone by the oxidation of anthracene have a low yield with high demands on the purity of the processed anthracene, a considerable amount of generated waste with negative effects on the work and the environment.

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These disadvantages are considerably alleviated by the process for the preparation of 9,10-anthraquinone according to the invention. Its essence is that the liquid anthracene with minimal retention in the storage tank and in the evaporator is vigorously evaporated into a stream of water vapor and after mixing with process air is selectively oxidized to 9,10-anthraquino on a fixed catalyst bed in an adiobatically controlled tubular reactor. The reaction gases are passed to a recuperator, where part of the heat is transferred to fresh air, then the partially cooled reaction gases are mixed with fresh air and cooled in a controlled manner to a temperature at least 15 ° C higher than the dew point of the resulting gas mixture. ° C. Desublimed 9,10-anthraquinone is separated on bag filters, the remaining vapor content of 9> 10-anthraquinone and by-products of the organic reaction products is washed into water and disposed of.

The use of the process for the production of 9,10-anthraquinone according to the invention brings a significant increase in the production yield compared to the technologies used so far, it allows the use of anthracene with reduced active ingredient content, which was unusable by previous processes for the production of 9,10-anthraquinone. The amount of generated waste is significantly reduced, the negative effects of the technologies used so far on the working and environment are eliminated.

A practical operation of the process for the production of 9,10-anthraquinone according to the invention may be as follows. Molten anthracene in an amount of 418 kg per hour of vaporized into the stream of superheated steam and then flash mixed with 10 OOO / ^J Nm / hr of air at 285 ° C. The homogeneous mixture is passed over a fixed catalyst bed in the tubes of an adiabatically controlled reactor. mixed gases. The precipitated 9,10-anthraquinone is separated in a separation device, its desublimed residues are separated from the waste gases on a bag filter and are discharged at a rate of 362 kg / h from a finishing device, such as separation of ferromagnetic impurities, grinding and adjustment. The waste gas is freed of residual redesublimed 9,10-anthraquinone and organic by-products by washing with water.

Claims (1)

Process for the production of 9,10-anthraquinone by catalytic oxidation of anthracene, characterized in that the liquid anthracene and the minimum retention in the storage tank and in the evaporator are vigorously evaporated into a stream of water vapor and after mixing and fresh air on a fixed catalyst bed in an adiabatically controlled reactor is oxidized to 9,10-anbraquinone, after which the reaction gases, after heat recovery by mixing and fresh air, are cooled to a temperature which is at least 15 ° C higher than the dew point of the resulting gas mixture and which does not exceed 110 ° C, and by filtration on sleeve filters, the desublimed 9,10-anthraquinone is separated, the residual content of 9,10-anthraquinone and in particular other organic reaction products being washed into water and disposed of.