SU1182020A1 - Method of producing 2-(1-methylalkyl)-phenols - Google Patents

Abstract

METHOD OF OBTAINING 2-

Description

The invention relates to the production of o-substituted alkiphenols of the general formula

3-13, are used as origin η = which are the starting materials for the production of surfactants and herbicides.

And, the spruce of the invention is an increase in the yield of 2- (1-methylalkip) phenols and a simplification of the technology.

Example 1. The catalyst is obtained by hydrothermal treatment of alumina at 120-150 ° C for 3-5 hours in an aqueous solution containing silver ions. After that, the catalyst is dried at 100-120 ° C for 3 hours and calcined at for 3-4 hours,

In a flow reactor, a thermally treated alumina promoted with Ag ions. The catalyst is dehydrated for 1-3 hours in a stream of inert gas at 500 ° C. Then the temperature is reduced to 200-210 ° C and phenol vapor is fed to the catalyst bed for 0.5-3 hours at a rate of one vapor volume per hour per one catalyst volume. After that, the inert gas and phenol supply is turned off and a mixture of phenol and n-decene taken in a molar ratio of 1: 1, with a space velocity of 1 h “ ^l , at 200 ° C and atmospheric pressure, is passed. The catalyst in this mode worked for 120 h without regeneration and changes in activity and selectivity.

2- (1-methylnonyl) phenol isolated by distillation, collecting the fraction boiling at 318-320 ^° C, 0.9280;

1.5022. The yield of the target product is 90.5%. The product obtained by the known method had the same constants.

500-550 ° С are loaded with a guide VNIIIPI Order 6063/23

Example 2. In a flow reactor loaded hydrothermally spent alumina promoted with Ag ions. The catalyst was treated prior to the reaction similar to the Example 1. Then, the catalyst layer is passed through a mixture of phenol and n-hexene-1, taken in a molar ratio of 1: 1, at a space velocity 4- 1 ^1, at 200 ° C and atmospheric pressure. 2- (1-Methylpentyl) phenol is removed by distillation, collecting a fraction boiling off at 265-266 ° С, Г 4 ° 0.9545; n * ° 1.5135. The yield of the target product is 90.5%.

Example 3. The catalytic interaction of phenol with n-octene-1 is carried out analogously to example 1. 2- (1-Methylheptyl) phenol is isolated by distillation, collecting a fraction boiling off at 290 ° C, 0.9380;

1.5055, the yield of the target product 90.6%.

Example 4. In a flow reactor load dehydrated hydrothermally treated alumina promoted by Ag ions. The pretreatment conditions of the catalyst with phenol vapor and the reaction are similar to Example 1. Phenol and n-hexadecene-1 are taken as the reaction mixture.

2- (1-Metilpentadetsil) phenol isolated by distillation, collecting the fraction boiling at 386-387 C ^e, 0.9028;

4 ° 14923. The yield of the target product is 86.5%.

The proposed method allows to obtain continuously 2- (1-methylalkyl) phenols with a yield of 86-90%, which exceeds by 18-22% the yield of products in the known periodic method. This was achieved through the use of hydrothermally treated alumina promoted with silver ions. The catalyst operates for a long time without changing its activity and selectivity and does not need regeneration after 120 hours of operation.

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Branch of the PPP Patent, Uzhgorod, Project 4,

Claims (3)

METHOD FOR PRODUCING 2- (1-METHYLALKyl) -PHENOLS of the general formula where n = 3-13, by the interaction of phenol with normal structure d-olefins in the presence of alumina at atmospheric pressure and a temperature of 19O-22O ° C, characterized in that, in order to increase yield of the target product and simplification of the technology, olefins are used as o (olefins) and the process is conducted in the presence of hydrothermally treated alumina containing 0.01-1 wt.% silver ions in a flow reactor, with a feed volumetric rate of 0.2- 3.2 h ~ ¹ . uwn ^{: i:} ns 1 1182020