The method of preparation of the palladium catalyst for the synthesis of ethyl ester of 10-(2,3,4-trimetoksi-6-were) decanoas acid

 

(57) Abstract:

The invention relates to methods of activation unprocessed catalysts used in the synthesis of intermediates of medicines and vitamins. The method of preparation of palladium catalyst on a carbon carrier "Sibunit" hold the influence of ultrasound with an intensity of 0.1 - 3 W/cm2within 5-60 using a conical nozzle ultrasonic transducer that is dipped in a chemical glass with a catalyst, in isopropanole solution of sulfuric acid. 1 table, 3 Il.

The invention relates to methods of activation of the catalysts used in the synthesis of semiconductors medicines and vitamins.

It is known that activation of the catalysts most often carried out by thermal methods, which often leads to disruption of the crystal structure or physical destruction of the catalyst. Known activation method "fresh" catalyst and recovery of fatigued catalysts by treatment of aqueous culture containing bacteria, such as bacteria, reducing sulfates, oxidizing the sulfides of oxidizing iron. Catalyst p is lyst to the carrier, and activating the catalyst by bacteria, located together with the active phase of the catalyst in dilute impregnating solution. After removal of the culture, if necessary, the catalyst is heated to temperatures of 400 - 500oC (Ed.St. USSR N 190288, class B 01 J 37/34).

The disadvantages of this method is that, firstly, it does not completely from the heat treatment in the preparation of the catalyst, secondly, requires for its implementation the combination of microbiological and chemical stages, which leads to the complexity of hardware implementation.

The closest in technical essence is the case of the processing of platinum (Pt) and palladium (Pd) mobiles for subsequent hydrogenation of alkenes, oxidation of ethanol. Pt mobile produced in the presence of ultrasound showed an increase in surface area and magnetic sensitivity. The most active Pt mobile obtained by the treatment frequency 3 MHz, T. J. Mason - London and N.-Y. 1990, p.50).

The disadvantage of this method is that the ultrasonic treatment is not having the carrier catalyst. This allows you to apply powerful ultrasound (more than 1 W/cm2), which leads to grinding of the catalyst and partially due to this increased involvement. Use is not possible, because it leads to his destruction.

Task to be solved using the present invention is improving the quality of the fresh catalyst.

The technical result of the invention improve the performance of the catalyst, expressed in the increase of its activity in the process of obtaining the ethyl ester of 10-(2,3,5-trimetoksi-6-were)decanoas acid.

The technical result is achieved in that in the method of preparation of palladium catalyst on a carbon carrier for synthesis of ethyl ester of 10-(2,3,4-trimetoksi-6-were)decanoas acid, including the effects of ultrasound with a frequency of 22 kHz, using ultrasound with intensity of exposure of 0.1 - 3 W/cm2within 5-60 with the catalyst placed in the solution. As the catalyst used, the palladium catalyst deposited on Sibunit. This palladium catalyst powder (with particle size from 15 to 70 μm), it has a dark grey color. For the ultrasound treatment uses ultrasonic disperser of USDN A. Ultrasonic effect on the planned process for the hydrogenation of ethyl ester 9-(2,3,4 - trimetoksi-6-methylbenzoyl)nonane is 0, moreover, the entire process is carried out using a conical nozzle ultrasonic piezoelectric transducer, and the catalyst is a chemical Cup in isopropanole solution of sulfuric acid (3.8 mol/m3). When the frequency deviation in the lower side is the exit from the zone of ultrasonic vibrations, and when the deviation in a big way in terms of frequency, as well as the deviation in the lower side-intensity ultrasound exposure, it is not possible to achieve the effect of activation. When the deviation of the intensity ultrasound in a big way is the destruction of the catalyst and a significant reduction in its activity. The use of cylindrical nozzles ultrasonic transducer leads to a change in the structure of the acoustic field. In the modified acoustic field is also available for the preparation of the catalyst, but the use of a cylindrical nozzle leads to a significant loss of catalyst during its transfer from the nozzle to the reactor that is unprofitable due to the high cost of palladium. In addition, a further increase of time of ultrasonic treatment makes it impossible to conduct effective activation, resulting in low given the speed of time.

Preparing to activate the raw palladium catalyst deposited on a carbon carrier Sibunit process for the hydrogenation of ethyl ester 9-(2,3,4-trimetoksi-6-methylbenzoyl)nonanalog acid to ethyl ester 10-(2,3,4-trimetoksi-6-were)decanoas acid using ultrasound exposure with an intensity of 0.1-3 W/cm2and processing time 5-60 with in isopropanole solution of sulfuric acid (3.8 mol/m3with the use of conical nozzles ultrasonic transducer is new compared to the prototype.

Under the influence of ultrasonic vibrations is more evenly distribution of palladium on the surface, which apparently contributes to the formation of a larger number of active sites. In addition, according to XPS-spektroskopie ultrasonic effect on the catalyst leads to the accumulation of Pd(II), which also increases the activity.

To explain the method of preparation of the raw catalyst Pd/Sibunit using ultrasonic treatment following drawings, where Fig.1 shows an ultrasound unit (General view), Fig.2 shows the change in the particle size distribution of the catalyst after ultrasonic who 2 and processing time 5 60 does not significantly change the particle size distribution of the catalyst, and hence to its destruction. In Fig.3 shows the dependence of the yield of the reaction product of hydrogenation from changes in the intensity ultrazvukova impact.

The best option of carrying out the invention

For the process of hydrogenation of ethyl ester 9-(2,3,4-trimetoksi-6-methylbenzoyl)nonanalog acid to ethyl ester 10-(2,3,4-trimetoksi-6-were)decanoas acid using a palladium catalyst (dark gray) deposited on a carbon carrier Sibunit. The preparation of the catalyst to increase its activity is carried out in an ultrasonic field.

Ultrasound unit consists of an ultrasonic generator 1 (USDN A) connected to the cable 2 with the ultrasonic emitter 3. Ultrasound emitter 3 sets conical nozzle 4, which is dipped in a chemical glass 5 with a catalyst, in isopropanole solution of sulfuric acid (3.8 mol/m3).

Processing is performed as follows: adjusted ultrasonic generator 1 by time and intensity ultrasound exposure, novelty.

The results of the regeneration of the catalyst are given in table. 1 and in Fig. 3.

The proposed method of regeneration is implemented on the industrial output of the ultrasonic generator, the process is fast and gives good results.

The method of preparation of the palladium catalyst for the synthesis of ethyl ester of 10-(2,3,4-trimetoksi-6-were)decanoas acid, including the effects on the catalyst ultrasound with a frequency of 20 to 22 kHz, characterized in that as a palladium catalyst using a catalyst containing palladium on a carbon carrier Sibunit and influence carry out the ultrasound with intensity ultrasound exposure 0,1 3 W/cm2for 5

60 in isopropanole solution of sulfuric acid.

 

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