The method of obtaining 4-cyclohexyl-4-methylpentene-2

 

(57) Abstract:

The inventive product 4-cyclohexyl-4-methylpentane-2. Reagent 1: 4-phenyl-4-methyl-pentanone-2. Reagent 2: hydrogen. Reaction conditions: the hydrogenation is carried out in the presence of a copper-chromium catalyst at 210-250oand a pressure of 5.0-15.0 MPa, and the reaction mixture digitalout at 260-270oand a pressure of 0.2 to 2.5 MPa. table 2.

The claimed method belongs to the technology of organic compounds, in particular the production of 4-cyclohexyl-4-methylpentene-2 (CIP) of the formula:

< / BR>
CIP is used in perfumery and cosmetics industry as odorants.

From analogs of well-known way to obtain DSM (the Netherlands, application N 300113 standard from 10.09.65) by hydrogenation of 4-phenyl-4-methylpentanol-2 over Raney Nickel at 150oC and 10.0 MPa, followed by oxidation of the obtained 4-cyclohexyl-4-methylpentanol-2 chromium mixture. This method has the following disadvantages:

the use of high-risk in the treatment of the catalyst;

the complexity of the technological design process associated with the filtration of fine catalyst;

a large amount of waste is diluted sulfuric acid containing toxic chromium salt;

required is a small autoclaves, the frequency of operation of the autoclaves.

The closest analogue to the technical nature of the claimed is a method for CIP set forth in article journal "oil and Fat industry", 1958, No. 12, S. 23-25. "Catalytic dehydrogenation of alcohols", B. N. Karasev, A. A. Bach, L. L. Malkina, O. M. Holmer.

The technical essence of the method according closest analogue is the dehydrogenation of 4-cyclohexyl-4-methylpentanol-2 in the presence of a copper-chromium catalyst supported on asbestos in the vapor phase. Synthesis is carried out by skipping pair of source materials through the catalyst at a residual pressure of 0.5 mm RT. Art. and temperature 240oC.

This method has the following disadvantages:

low sensitivity of the original product;

little performance related to the process in the gas phase (less than 0.5 kg/l catches );

the complexity of the disposal of spent catalyst associated with use as a carrier of carcinogenic asbestos;

high energy costs and the complexity of the technological design associated using deep vacuum.

The technical nature of the claimed method is that CIP was obtained as is at a temperature of 210-250oC and a pressure of 5.0-15.0 MPa, then the reaction mixture digitalout in a stream of nitrogen at a temperature of 260-275oC and a pressure of 0.2-2.5 MPa for copper-chromium catalyst.

Stage hydrogenation according to the claimed method is performed at the following technological parameters:

the hydrogen pressure of 5.0-15.0 MPa

the temperature of the hydrogenation 210-250oC

contact load of 1.2-1.8 kg/l catches.

Conversion at this stage is 90-95%

The second stage dehydrogenation is carried out at the following technological parameters:

a nitrogen pressure of 0.2-2.5 MPa

the temperature of the dehydrogenation 260-275oC

contact load 1.0 to 1.2 kg/l catches.

Conversion of the target product is 90-95% Yield after CIP allocation is 82-90%

Control reaction mixtures is carried out by GLC.

Stage hydrogenation and dehydrogenation is carried out in continuous mode, at a fixed-fixed catalysts.

Below is a table 1 comparable data closest analogue and the claimed method.

As you can see, the claimed method increases the yield of the target product and performance.

Variant implementation of the claimed method # 1. oC at the same time serves 4-phenyl-4-methylpentane-2 with a speed of 18 ml/HR and hydrogen at a pressure of 10.0 MPa at a rate of 25 l/h

The reaction mixture containing 4-cyclohex - force-4-methylpentanol-2 is collected in the collection.

The composition of the mixture, wt.

4-Cyclohexyl-4-methylpentane-2 2,0

4-Cyclohexyl-4-methylpentanol-2 92,3

4-Phenyl-4-methylpentanol-2 Traces

Volatile impurities 5,7

2. Into the reactor containing the recovered copper-chromium catalyst at a temperature of 260oC simultaneously serves obtained under item 1 of the reaction mixture at a rate of 12 ml/h and nitrogen at a pressure of 2.0 MPa at a rate of 25 l/h

The reaction mixture composition, wt.

4-Cyclohexyl-4-methylpentane-2 95,0

4-Cyclohexyl-4-methylpentanol-2 3,3

4-Phenyl-4-methylpentane-2 Traces

Volatile impurities 1,7

3. The reaction mixture obtained under item 2, is subjected to vacuum distillation. Output 4-cyclohex-force-4-methylpentene-2 86%

4. The obtained 4-cyclohexyl-4-methylpentane-2 has the following physical specifications:

M. C. 182,30

n2D01,475-1,480

d2409441 kg/m3< / BR>
tKip239-240oC (75 mm RT.CT.)

Other options intervale, in table 2, including an implementation option # 1.

As you can see, the claimed method provides a high yield of the product (see examples 1-3). Provided that the violation stated intervals (see examples 10-17 N) output is reduced.

Based on the above description of the method of obtaining 4-cyclohexyl-4-methylpentene-2 inventive side claims that the specified object corresponds to a characteristic of the invention "industrial applicability" and is fully responsible for this criterion.

The method of obtaining 4-cyclohexyl-4 methylpentene-2 using 4-cyclohexyl-4 methylpentanol-2, which digitalout in the presence of a copper-chromium catalyst at elevated temperature, characterized in that 4-phenyl-4-methylpentane-2 hydronaut in the presence of Nickel-copper-chromium catalyst at 210 250oC and a pressure of 5.0 15.0 MPa and the resulting reaction mixture containing 4-cyclohexyl-4-methylpentanol-2 digitalout in a stream of nitrogen at 260 270oC and a pressure of 0.2 to 2.5 MPa.

 

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