SU372903A1 - - Google Patents

Description

(54) METHOD FOR OBTAINING SECONDARY BUTYLBENZENE

one

The invention relates to methods for producing alkyl aromatic compounds, in particular butyl benzene, which is used as an additive to motor fuel and mainly as a raw material for production, and phenol and methyl ethyl ketone, the most important products of organic synthesis.

A known method for producing butylbonzol is by treating benzene with ethyl gum in the presence of zeolite catalysts containing rare earth cations. The catalysts prepared on the basis of rare-earth elements and a: mmonium, quite quickly deza. Are activated during the experiment due to coke formation. In addition, after the operation of the catalyst for 200 hours, their “aging occurs — the initial activation is lost irreversibly.

In order to increase the yield of the target product and increase the service life of the catalyst according to the proposed method, the process is carried out on a zeolite catalyst containing calcium and nickel cations. At this, the yield of butylbenzene increases to 60–70%, the catalyst operates under milder conditions (150–200 ° C per 200–250 ° C), and the stability of the catalyst increases dramatically. After operating for 200 hours, no signs of catalyst fatigue are observed, ion formation decreases.

Example 1. For the experiment, use was made of granulated in the form of cylinders (5x / mm) NaY zeolite without a binder component with a ratio of SiO2 to A12Oz equal to 3.6, and a mechanical strength of 2.5 kg / mm. 100 g of the sample is loaded into a flask and subjected to cationic exchange of calcium oxide for 1 equivalent of sodium in zeolite 10 equivalents of calcium. The cation exchange was carried out with a 10% solution of calcium chloride at 5 bays, 2 hours each. After the fifth treatment, the zeolite is washed with distilled water until there is no SG, then it is kept at 120 ° C and calcined for 6 hours at 500-600 ° C. After these operations, the zeolite contains 11.9% CaO, which corresponds to the degree of exchange for calcium 74%.

The second step in the preparation of the catalyst is the cation exchange for nickel. The obtained sample of CaY zeolite is treated in a flask with a 5% solution of nickel nitrate based on 1 equivalent of calcium or sodium 5 equivalents of nickel at pH 4.5. If the RP of the initial solution is lower, then it is necessary to add calcium oxide to it. Capacity is carried out when moving in 5 bays for 2 hours each at 60-70 ° C. At the end of the exchange, the zeolite is washed away from NOs, dried and calcined at 500-600 ° C for 5-6 hours. The weight of the obtained zeolite contains 15.1% NiO, which

corresponds to the degree of exchange of 76.3%. The strength of the granules of the obtained zeolite NiY is 1.9 kg1 mm, the sorption capacity for benzene at 20 ° С and atmospheric pressure of 31%, the acidity by titration with butyl amine 1.1 meq 1 g.

50 Si3 (35 g) of CaNiY zeolite catalyst is loaded into a flow reactor with a diameter of 20 L1M and a length of 1 m. After loading, the catalyst is activated by blowing air at a rate of 50 l / h at 500 ° C for 5 hours and then with nitrogen at the same temperature for 30 minutes . Through the catalyst thus activated, a mixture of benzene and ethylene is passed in a ratio of 3: 1 at a space velocity of 3 hours 30 atm and 150 ° C. The yield of secondary butylbnzol under these conditions is 60-70%, the productivity is 0.3-0.4 g / hour with 1 cm of catalyst. The yield of ethylbenzene does not exceed 4%. In the first 5 hours of catalyst operation, no more than 2.7 g of coke was deposited on it.

PRE | Meph -2. At the same sample of the catalyst under the conditions of measurer /, but at 200 ° C, the yield of secondary butylbenzene is 50-60%, and ethylbenzene is 6-7%. An increase in pressure (| over 30 atm) does not affect the yield of secondary butylbenzene, but increases the stability of the catalyst. After 200 hours of operation in the mode of food regeneration, there were no noticeable signs of catalyst fatigue, a decrease in its mechanical strength, or a loss in weight.

Subject invention

The method of producing secondary butylbenzene by treating benzene with ethylene with zeolite catalysts, characterized in that, in order to increase the yield of the target product and increase the service life of the catalyst, the process is carried out on a zeolithium catalyst containing calcium and nickel cations.