Method of producing isopropyl benzene hydroperoxide

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing isopropyl benzene hydroperoxide (IPB HP) which is then used to produce phenol and acetone using what is known as industrial cumol method. According to the invention, isopropyl benzene hydroperoxide is obtained by oxidising isopropyl benzene with molecular oxygen. The catalyst used is iron nanopowder with specific surface area of 6.9 m2/g, obtained through electrical explosion of a conductor in a nitrogen atomsphere. The process is carried out at 50-60C.

EFFECT: increased output of isopropyl benzene hydroperoxide.

1 cl, 3 ex

 

The invention relates to a method for the gidroperekisi of cumene (SE IPA), which are further used for production of phenol and acetone and industry, the so-called komorny, method for production of phenol and acetone [Lebedev N.N. Chemistry and technology of basic organic and petrochemical synthesis. M.: Chemistry, 1981. - S].

Known industrial method of obtaining gidroperekisi of cumene, which SE IPA is produced by oxidation of isopropylbenzene (cumene) by atmospheric oxygen at a temperature of 100-120C, the oxygen of the air supplied under pressure [Lebedev N.N. Chemistry and technology of basic organic and petrochemical synthesis. M.: Chemistry, 1981. - S]. The disadvantages of this method are the high temperature and oxygen flow of air under pressure.

Also known is a method of obtaining GP IPA in the oxidation of cumene with the use of salts of metals of variable valence (salts of vanadium, cobalt, molybdenum) [Blumberg E.A., Mayzus Z.K., Norika UD, Skibina I.P. // DAN USSR. - 1978. - T. No. 2. - S]. The disadvantage of this method is the decomposition of gidroperekisi during the response to acetophenone and dimethylphenylcarbinol.

Also known is a method of obtaining SE cumene in the presence of metallic copper in the form of shavings (Shalya CENTURIES, Colatura B. I., Yampolskaya F.A., Gorohovatsky AB //Kinetics and catalysis. - 1972. - TH 111. - V.2. - S). However, fault the mi method are the high temperature process of obtaining GP IPA and the lack of selectivity of the process.

Closest to the proposed invention is a method for SE IPA using nanopowder iron (Fe) with a specific surface area of 4.6 m2/g, obtained by the method of electrical explosion of the conductor in a nitrogen atmosphere at a temperature of 60C and atmospheric pressure (message Tosorontio, Neskorodeeva, ADN at the International conference "Chemistry, chemical engineering and biotechnology at the turn of the Millennium", Tomsk, 11-16 September 2006, the Disadvantage of this invention is not a high yield of SE IPA. The task of the invention is to develop a method of producing cumene, which allows to increase the output SE of the IPA.

The technical result is achieved by the fact that hydropeaking of cumene is produced by oxidation of cumene with molecular oxygen in the presence of a catalyst - nanopowder iron with a specific surface area of from 4.7 to 6.9 m2/g, obtained by electrical explosion of the conductor in a nitrogen atmosphere at a temperature of 50-60C.

To get SE IPA carry out the oxidation of cumene to gasometrical installation (Emanuel N.M., Gladyshev G.P., Denisov ET, Zaalov V.F., V.V. Kharitonov, Piotrovsky K.B. Procedure for testing chemical compounds as stabilizers for polymeric materials. Chernogolovka: Izd-vo oihf the USSR Academy of Sciences, 1976. - P.35).

The reactor is placed IPA and nanopowder glands is, obtained by electrical explosion of a conductor in an atmosphere of nitrogen, with a specific surface area of 4.7 m2/g or 6.9 m2/, the resulting mixture is Heated to 50-60C, passed through the reaction mixture of oxygen and record the absorption rate and the amount of absorbed oxygen. After absorption 5,0; 10,0; 20,0; 30,0; 40,0; 50,0; 60,0 ml oxygen deprived of the sample (~1,4-1,45 ml) and define the number of the resulting SE IPA iodometrically by well-known methods (General workshop on organic chemistry. Moscow: Mir, 1965. - P.153). The reaction by-products (acetophenone and dimethylphenylcarbinol) analyze by gas chromatography (GC) on the chromatograph Perkin Elmer Sigma 2B with a flame ionization detector column SE-52 33 m in programming mode temperature: initial temperature of thermostat 80C, the temperature increase of 3C/min to 150C. the carrier Gas - helium.

Example 1. The reactor is placed 8.6 g of IPA and 0,0198 g nanopowder iron with a specific surface area of 4.7 m2/g, obtained by electrical explosion of the conductor in a nitrogen atmosphere. Heat the mixture to 50C, passed through the reaction mass of oxygen and fix the rate of absorption of oxygen and the amount of absorbed oxygen. After absorption 5,0; 10,0; 20,0; 30,0; 40,0; 50,0; 60,0 ml oxygen deprived of the sample (~1,4-1,45 ml) and define the number of the resulting SE IPA iodometrically.

1. After absorption of 5.0 ml of m is molecular oxygen in the reaction mixture contains 0,50% wt. SE IPA.

2. After absorbing 10.0 ml of molecular oxygen in the reaction mixture contains 1,09% wt. SE IPA.

3. After absorption of 20.0 ml of molecular oxygen in the reaction mixture contains at 2.45% wt. SE IPA.

4. After absorption of 30.0 ml of molecular oxygen in the reaction mixture contains 3,60% wt. SE IPA.

5. After absorption of 40.0 ml of molecular oxygen in the reaction mixture contains 4,80% wt. SE IPA.

6. After absorption of 50.0 ml of molecular oxygen in the reaction mixture contains 6,05% wt. SE IPA.

7. After absorption by 60.0 ml of molecular oxygen in the reaction mixture contains 7,06% wt. SE IPA.

In the reaction mixture contains trace amounts of acetophenone and dimethylphenylcarbinol.

Example 2. The reactor is placed 8.6 g of IPA and 0,0198 g nanopowder iron with a specific surface area of 6.9 m2/g, obtained by electrical explosion of the conductor in a nitrogen atmosphere. Heat the mixture to 60C, passed through the reaction mass of oxygen and fix the rate of absorption of oxygen and the amount of absorbed oxygen. After absorption 5,0; 10,0; 20,0; 30,0; 40,0; 50,0; 60,0 ml oxygen deprived of the sample (~1,4-1,45 ml) and define the number of the resulting SE IPA iodometrically.

1. After absorption of 5.0 ml of molecular oxygen in the reaction mixture containing 0.5% wt. SE IPA.

2. After absorbing 10.0 ml molecular to the of Sloboda in the reaction mixture contains 1,09% wt. SE IPA.

3. After absorption of 20.0 ml of molecular oxygen in the reaction mixture contains at 2.45% wt. SE IPA.

4. After absorption of 30.0 ml of molecular oxygen in the reaction mixture contains 3,60% wt. SE IPA.

5. After absorption of 40.0 ml of molecular oxygen in the reaction mixture contains 4,90% wt. SE IPA.

6. After absorption of 50.0 ml of molecular oxygen in the reaction mixture contains 6,21% wt. SE IPA.

7. After absorption by 60.0 ml of molecular oxygen in the reaction mixture contains 7,28% wt. SE IPA.

In the reaction mixture contains trace amounts of acetophenone and dimethylphenylcarbinol.

Example 3. The reactor is placed 8.6 g of IPA and 0,0198 g nanopowder iron with a specific surface area of 6.9 m2/g, obtained by electrical explosion of the conductor in a nitrogen atmosphere. Heat the mixture to 80C., is passed through the reaction mass of oxygen and fix the rate of absorption of oxygen and the amount of absorbed oxygen. After absorption 5,0; 10,0; 20,0; 30,0; 40,0; 50,0; 60,0 ml oxygen deprived of the sample (~1,4-1,45 ml) and define the number of the resulting SE IPA iodometrically.

1. After absorption of 5.0 ml of molecular oxygen in the reaction mixture contains 0,49% wt. SE IPA and trace amounts of acetophenone and dimethylphenylcarbinol.

2. After absorbing 10.0 ml of molecular oxygen in the reaction mixture, siderits the 0,92% wt. SE IPA and trace amounts of acetophenone and dimethylphenylcarbinol.

3. After absorption of 20.0 ml of molecular oxygen in the reaction mixture contains 1,87% wt. SE IPA and trace amounts of acetophenone and dimethylphenylcarbinol.

4. After absorption of 30.0 ml of molecular oxygen in the reaction mixture contains 2,84% wt. SE IPA and trace amounts of acetophenone and dimethylphenylcarbinol.

5. After absorption of 40.0 ml of molecular oxygen in the reaction mixture contains 3,75% wt. SE IPA, 0, 75% wt. dimethylphenylcarbinol and 0.04 wt.%. of acetophenone.

6. After absorption of 50.0 ml of molecular oxygen in the reaction mixture contains 4,01% wt. SE IPA, 1.5% wt. dimethylphenylcarbinol and 0.07 wt.%. of acetophenone.

7. After absorption by 60.0 ml of molecular oxygen in the reaction mixture contains 3.8% of wt. SE IPA, and 2.0% wt. dimethylphenylcarbinol and 1% wt. of acetophenone.

Thus, the technical result - selective education SE IPA is achieved by using nanopowder iron with a specific surface area of 4.7-6.9 m2/g and a temperature of 50-60C.

The way to get gidroperekisi of cumene oxidation of cumene with molecular oxygen in the presence as catalyst of the iron nanopowder obtained by electrical explosion of the conductor in a nitrogen atmosphere, characterized in that the use of nanopowder jelly is a, having a specific surface area of 6.9 m2/g, and the process is conducted at a temperature of 50-60C.



 

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