SU992508A1 - Process for preparing phenol and acetone - Google Patents

Description

(5) METHOD FOR PRODUCING PENOL

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The invention relates to an improved process for the production of phenol and acetone used in the chemical, petrochemical and pharmaceutical industries.

A known method of producing phenol and acetone by decomposing isopropylbenzene hydroperoxide (GPIPB) in isopropylbenzene (IPB) when heated in the presence of silicon, zirconium. go catalyst tl,

The disadvantage of this method is the lack of complete (100) conversion on the GCPP catalysts. The incompleteness of decomposition of IPB hydroperoxide, leading under production conditions to accumulation in the system of undecomposed isopropylbenzene hydroperoxide, which is an unstable substance and under favorable conditions instantaneously 20 decomposes with an explosion.

There is also known a method of producing phenol and acetone by decomposition of isopropyl benzene hydroperoxide in ace and acetone.

tones at 0-70 ° C in the presence of sulfonic cation exchangers KU-23 bulk flow rate of the raw material h 2.

The disadvantage of this method is the synthesis under the conditions of the decomposition of mesityl oxide from acetone. In the decomposition reaction mass, the content of mesityl oxide as a result of the condensation reaction reaches 0.9-1.2 wt.%, Which does not allow the production of using KU-2-8 hC cationite as a catalyst for the fine purification of phenol. I The closest to the present invention is a method for producing phenol and acetone by decomposing GPPB 3.

Water is added to a solution of isopropylbenzene hydroperoxide with a concentration of 0-30 masd in acetone in the amount of 0.6-5 May. . This mixture is passed upwards through a tubular type reactor filled with KU-23 sulfonic cation exchanger at 5–60 ° C and a space velocity of Conversion of hydroperoxide 100. The yield of phenol (from theory) is 98.199, 1 mas. The oxide content of mesityl in the reaction mass 0, 0.12 masch. The disadvantage of this method is the presence of a large amount of mesityl oxide, which degrades the quality of the target product, causes a sharp decrease in the operating time of the reactor with the KU-2-8-8 C ion, intended for fine purification of phenol from carbonyl-containing compounds, including mesityl oxide, contained in the industrial reaction mass of decomposition, using isopropyl benzene hydroperoxide as a catalyst for decomposition, and concentrated H2SOE reaches 0.02 mas p. The purpose of the invention is to improve the quality of the target product. This goal is achieved by the fact that, according to the method of producing phenol and acetone by decomposing isopropylbenzene hydroperoxide in an organic solvent in the presence of a heterogeneous catalyst at an elevated temperature, the catalyst composition is used as a heterogeneous catalyst, mas: AInO10,1-11,7, 1-0 , 12 CaO0.2-0.55, 1-0.28 Si0289.28-87.35 and having a particle size of 0.5-2 mm, acetone or an equimolecular mixture of phenol and acetone are used as the organic solvent, the process is carried out at 50-70 ° C and a space velocity of 2-10 h at the initial end n radios equal isopropylbenzene hydroperoxide -20 wt .. The inventive method is carried out as follows. A solution of isopropylbenzene hydroperoxide with a concentration of -20 masD in acetone or in an equimolecular mixture of phenol and acetone is passed through the tubular reactor from bottom to top, filled with catalyst (fraction O, 52 mm). This catalyst is preliminarily calcined in a stream of air at 600-650 ° C. The decomposition of isopropylbenzene hydroperoxide is carried out at 50-70 ° C. The volumetric feed rate of the solution is 2–10. Under these conditions, mesityl oxide is completely absent in the reaction mass of decomposition. Conversion of isopropyl benzene hydroperoxide 100. The phenol yield is 97.8-99.3 wt.% Of the theoretically possible. Carrying out the decomposition reaction of hydroperoxide, isopropyl benzene under other conditions leads to the fact that at temperatures less decomposition takes place at a very low speed, the temperature rises above 70 ° C, which favors the increased resin formation, which also takes place at a decrease in the feed rate of the initial mixture below 2 hours. An increase in the space velocity of more than 10 parts leads to incomplete decomposition of isopropyl benzene hydroperoxide (up to 0.2 wt. At a volumetric rate of 12 hours). A decrease in the concentration of isopropyl benzene hydroperoxide in the initial mixture fed to decomposition below k wt is not technological, since it leads to an increase in the volume of circulating solvent under the conditions of the existing production, and an increase in the concentration of isopropyl benzene hydroperoxide makes it difficult to remove heat. Example 1 A stock solution containing 5.2% by weight of isopropylbenzene hydroperoxide in acetone is continuously fed into a reactor filled with a lithium nitrite-containing catalyst of composition,% in May: A120311.7 ResOZ 0.12 CaO0.55 Na200.28 SiOn87.35 at 50 c, the flow rate of the mixture is 2 hours. The conversion of the hydroperoxide reaches 100, the yield of phenol is 99.3 May, mesityl oxide is absent. Example 2. A stock solution containing 5736 Ma.I hydroperoxide in an equimolecular mixture of phenol and acetone is continuously fed to a reactor filled with a sylmanite-containing catalyst containing composition shown in Example 1 at 62 ° C and a space velocity 4, conversion of hydroperoxide 100%, mesityl oxide missing. Example 3. Decomposition is carried out under conditions of example 2 at 70 ° C and a space velocity of 10 hours. Conversion of hydroperoxide 100, mesityl oxide is absent.

Example i. A stock solution containing 8% by weight of isopropylbenzene hydroperoxide in an equimolecular mixture of phenol and acetone is continuously fed to a reactor filled with silli-5 manitoseolyte-containing catalyst of the composition shown in Example 1 at 70 ° C and a space velocity of C h-. Conversion of hydroperoxide 100, mesityl oxide is absent .. in

Example 5 Decomposition is carried out under the conditions of example, but on decomposition -. The solution serves 19.2 wt.%. hydroperoxides in an equimolar mixture of phenol and acetone. Converse hydroperoxide 100, mesityl oxide is absent. 6. A 5% solution of those of exemplary isopropylbenzene hydroperoxide in acetone is loaded into a flask containing a catalyst containing as described in Example 1, its content is 10% by weight, based on the weight of the initial mixture. The mixture with the catalyst is vigorously stirred at 56 ° C for 2 hours. Mesityl oxide is completely absent in the reaction mixture. Example 7. The original solution containing C, S may. isopropylbenzene hydroperoxide in an equimolecular mixture of phenol and acetone, is continuously fed to a reactor filled with sillimanitolol with a catalyst containing the following composition, wt .: ACO.10.1 RegOz0.1 CaO0, i «2 NaoO0.1 Si 0289.28

at and the volumetric rate C h. Conversion of hydroperoxide is 100%, mesityl oxide is absent.

Example 8. The initial solution, containing k wt.% HPA in an equimolar mixture of phenol and acetone, is continuously fed to a reactor filled with sillimanitseolite with a retention catalyst of the composition specified in Example 7 | at 55 ° C and flow rate 6.

Conversion of the CCP 100. Mesityl oxide is absent. The phenol yield is 99.25 mas.

Example 9. The original solution. containing 20 May.% HPA in an equimolecular mixture of phenol and acetone, is continuously fed to a reactor filled with a sillimanitzeolite-containing catalyst of the composition indicated in Example 7 at 70 ° C and a space velocity of 2 hours. HPP 100 conversion. Mesityl oxide is absent. The phenol yield is 97.8 wt. In the table. Tables 1 and 2 show the data on the comparison of the decomposition of a solution of isopropylbenzene technical hydroperoxide in the presence of heterogeneous catalysts according to the proposed method (Table 1) and the known methods (Table 2.). Comparison of these tables shows that in all experiments carried out in the presence of a sillimanite zeolite-containing catalyst (fraction 0.5–2 mm), mesityl was absent, and in the presence of sulfonic cation exchanger, the average content of mesityl oxide was 0.097 May L. 3 shows experimental data confirming the possibility of repeated use of sillimanitse-containing catalysts in the decomposition reaction of GPIPB.

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 At the first breakthrough of the CCP (up to 0.1 mAb) in the reaction mass, the catalyst is regenerated for k-6 h at air flow.

Claims (3)

1. USSR author's certificate number 188985, cl. C 07 C 39/04, published 1966. 2. Author's certificate. USSR № 379559, cl. C 07 C 39/04, published 1973. 3. USSR author's certificate number 537066, cl. C 07 C 39/04, published 1977 (prototype).