SU960180A1 - Process for producing organic aerosil - Google Patents

Description

(5) METAL-ORGANIC METHODS. . . .1 (U The invention relates to the chemistry of organosilicon compounds, in particular to an improved method for the preparation of organometallic aerosil, which can be used as a filler, and also as a catalyst for limited synthesis. metal followed by its treatment with a complexing agent 11. The disadvantage of this method is its two-stage process. The closest to the invention the technical essence and the achieved result is the method of obtaining organometallic aerosil by reacting aerosil with copper, cobalt or nickel oxide and organic complexing peaAEROSILA with an amine at 70-90 ° C in an organic solvent medium (21.. A disadvantage of the known method is the duration of the process is h. The aim of the invention is to reduce the duration of the process.; The goal is achieved by the fact that according to the method for producing organometallic aerosil treated Copper aerosil inorganic :: agent using copper / cobalt or nickel and organic KOM complex forming agent amine at 70-90 ° C in an organic solvent medium, copper powder, cobalt or nickel are used as inorganic agent. The proposed method makes it possible to shorten the reaction time in comparison with the known method by 1.5-2 times. Synthesis of organometallic aerosil is carried out in a two-neck reactor em3, 960

bone 100 ml, equipped with a stirrer, brotherly refrigerator and heating device. A mixture of aerosil and metal powder is added to the reactor, a solution of complex-forming reagent in an organic solvent is poured and the reaction mixture is heated to PP-EO C. The surface of the aerosium is painted. After the reactor was boiled down, the metal-borne aerosol was removed from the liquid phase by filtration, washed 2-3 times with a solvent, in which the medium was prepared, 2-3 times with ether. And dried in vacuo. In order to obtain comparable powders in parallel, organometallic aerosils are obtained by a known method.

Synthesis of organometallic aerosil by a known method.

Example1. The reactor is brought

2 g of aerosil, 0.1 g of copper and poured a solution of 3 ml of pyridine in 27 ml of benzene. The reaction mixture; heated with constant stirring for 30 hours. After cooling, the target product is filtered, washed 2-3 times with benzene, 23 times with ether and dried. Output

2.1g. The copper content is 0., 4%. IR spectrum: l), 1590, (c 3300

Example 2 2 g of aerosil, 0.1 g of copper oxide are introduced into the reactor, and a solution of 1 g of 2,2-dipyridyl in 30 ml of dimethylformamide is poured. The reaction mixture is heated at 90 ° C for 18 h. The yield of the target product

2.2g. The copper content is 2.2%. IR spectrum: Vcfsjl620, l) it is 3000-3350.

wide strip.

Example 3 To the reactor, similarly to the previous examples, 2 g of aerosil and 0.1 g of cobalt oxide are introduced and a solution of 3 ml of pyridine in 27 ml of dimethylformamide is poured. The mixture is heated at 90 ° C for 30 hours. The output of the desired product is 2.3 g. ContainingXI

cobalt: 1.8%. IR spectrum:

HI 1570 cm-1 and 3100 cm-T;

Synthesis of organometallic aerosols according to the proposed method.

L | Example. The reactor is brought

2 l and 2 Aerosil, 0.1 g of metallic copper powder, preferably in powder,

poured a solution of 3 ml of pyridine in ml of benzene. The reaction mixture is put on similarly to the previous primate, E 1 at 70 ° C for 13 hours. Yield

R

the left product is 2.2-g. Content

C and 0.5%. IR spectrum: - a 1595 s

Ml

H - 3300 cm) Example 5. The reactor is introduced

2 Aerosil, 0.1 g of metal powder; which copper and pour a solution of 1 g

Th .2; - dipyridyl in 30 ml of dimethylformala. The reaction mixture is heated mr, 90 ° C for 8 h.

0product 2, g. Content of mevo is 2.0% / IR rcneKTp: VcN 1b20,

 3.000-3350. Broad band.

П РИМ эр 6. Contributions are added to the reactor

Aerosil, 0.1 g powder of metal2 cobalt and poured solution

what

3 p pyridine in 27 ml of dimethyl forms. The mixture is heated at 90 ° C for 15 hours. Target product yield

Nor 2 g. Cobalt content of 1.7%

3110 cm

Spectrum: VCN 1570 CMVoH

IR Example 7. Nickel-containing master. . . ,,

Aetores are introduced into the reactor;

ABOUT,

g of metallic nickel powder poured a solution of 3 ml of pyridyl in 27 ml of dimethylformamide. The mixture is not allowed to revolve at 90 ° C for 12 hours. The yield of the desired product is 2.1 g. Nickel retention 1.8 IR spectrum ::

With

1 1580 3120 cM-t

The table shows the time for the synthesis of all-organic aerosils according to the theory and the proposed method under equal conditions.

etc

Claims (2)

1. Yermakov Yu. I. Catalysts containing fixed complexes of transition metals on the surface of carriers. Sat The role of coordination in catalysis. Kiev, Naukova Dumka, 1976, p. 4-9 2. Kokosei V.N. On the role of proton-containing reagents in some reactions; complexation. Conference of Young Chemical Scientists Faculty of Kiev State University. KSU, March 1E80.