The method of obtaining n-dioxanone

 

(57) Abstract:

Usage: in synthesis of monomers for the synthesis of polymer medical applications polydioxanone from which you get various products for surgery, absorbable in the tissues of a living organism. The inventive product n-dioxane. As catalyst, use standard metrogroove catalyst UNH 103 with Cu 65% Cr, about 45% of the Distillation products during the implementation is carried out by adjusting reflux ratio or intensity of heating of the cube so that the temperature of the vapor was 195 200C, and final clean pair of dioxanone carried out by distillation under vacuum of 2 to 3 mm RT. Art. in the presence of boric acid. The degree of purity of the target product 99, 99

The invention relates to the production of monomers and can be used for the synthesis of polymer medical applications polydioxanone from which you get various products for surgery, absorbable in the tissues of a living organism, rezorbiruetsa suture thread.

There are several ways of synthesis of a pair of dioxanone, of which the most important are the following.

The interaction of monolinoleate sodium with monochloracetic acid [1]

Catalytic dehydrogenase diethylene glycol may be vapor-and liquid-phase.

A method of obtaining a pair of dioxanone vapor-phase dehydrogenase diethylene glycol [2] according to which a continuous stream of diethylene glycol at 130 g/h is passed into a chamber containing 150 cm3catalyst consisting of recovered copper and chromium, porous media, and silicon dioxide. During the reaction maintained the temperature of 270-280aboutC. Facing vapor condenses (excluding hydrogen). After distillation of the condensate yield is 75% conversion rate 25% Technical: this method is limited because of its low efficiency.

Known for an improved method of obtaining a pair of dioxanone catalytic vapor-phase digitalangel diethylene if isplsi copper (I), moreover, the optimum catalyst containing about 20 wt.h. chromium 80 wt.h. copper. It is established that it is preferable to treatment of the catalyst with hydrogen at 275-300aboutWith before using.

Vapors leaving the reaction zone is condensed and purified by any method for separating a pair of dioxanone, for example by distillation. The yield of the desired product 84%

Information about the purity of the obtained product are not available.

A method of obtaining a pair of dioxanone with quantitative yield by passing vapors of diethylene glycol through a layer of catalyst containing copper at an acceptable carrier in the presence of added hydrogen gas at a temperature of 200-400aboutC, preferably at 250-350aboutC, at atmospheric pressure [4]

Disadvantages headspace methods is the relative complexity (the need of the evaporation source of diethylene glycol, the selection of the reactor, providing uniform contact of the vapors with the catalyst) and extremely hard the synthesis conditions (temperature up to 400aboutC).

A method of obtaining a pair of dioxanone liquid-phase dehydrogenation of diethylene glycol [5] in the presence of a catalyst of copper chromite containing 30-40%eshiwani catalyst with diethylene glycol in the reactor distillation and heating at a temperature of 240-280aboutC at atmospheric pressure. The yield of the desired product in 81% of the Data on the quality of the target product are not available.

The disadvantage of this method is the complexity of the process, due to the need for preparation of the catalyst.

The aim of the invention is to simplify the process by using the industrial catalyst and improve the quality of the target product.

The method of obtaining n-dioxanone liquid-phase dehydrogenase diethylene glycol is characterized by the fact that as the catalyst use standard catalyst UNH-103, distillation products during the reaction is carried out by adjusting reflux ratio so that the temperature of the vapor was 195-200aboutWith, and the final purification of n-dioxanone raw carried out by distillation at 2-5 mm RT.article in the presence of boric acid.

Using as a catalyst of national industrial catalyst brand UNH-103 (VNII Neftekhim-103, THE 3810284-83 changes 1,3,4 Cu not less than 65% SG not less than 45%) were ideal for this process. It managed to get raw with a concentration of 97-98% with a total yield of 80% and more.

It was also shown that if the distillation product is made to obtain the fraction of dioxanone raw with a concentration of up to 95% and above, almost free from diethylene glycol.

In addition, for the first time managed to get n-dioxane high purity of 99.99% This is achieved by the fact that the final purification of n-dioxanone raw conducting the distillation in the presence of boric acid.

The essence of the method consists in the following.

Conduct liquid-phase dehydrogenization of diethylene glycol in the presence of a standard catalyst UNH-103. Within 10 hours at a temperature in the cube 240-270aboutC, atmospheric pressure, reflux 1:2 rectification receive n-dioxane raw concentration 97-98% with a total yield of 80% and more. Then dioxane raw rectificatum to the degree of purity of the product is equal to 99.5-99.7% of

Received para-dioxanone load in cubic flask, add boric acid and at a vacuum of 2-3 mm RT.article distilled target product with a purity of 99.99%

P R I m m e R. Synthesis of a pair of dioxanone conducted at the facility, consisting of a bottom of the flask, a distillation column, a head full of condensation, two thermometers, a receiver and traps. In cubic flask is charged 1118 g of diethylene glycol and 50 g of catalyst UNH-103. Within 10 hours at a temperature in the cube 240-270aboutC, atmospheric pressure, reflux 1:2 rectif the lyst rectificatum once or twice to obtain 688 g of the product purity of 99.5-99.7% of

After that, 688 g of dioxanone raw load in cubic flask, add 5 g of boric acid and installation, consisting of a dephlegmator, head full of condensation, equipped with a thermometer, a distillation under a vacuum of 2-3 mm RT. Art. obtain 600 g of paradoxien purity of 99.99% Yield 57%

Thus, the proposed method allows to obtain, using available domestic raw materials n-dioxane on melastatin technology with high yield and high quality of the target product.

The METHOD of OBTAINING N-DIOXANONE liquid-phase dehydrogenization of diethylene glycol in the presence of a catalyst containing the oxides of copper and chromium, with subsequent isolation of the desired product by distillation, characterized in that the catalyst used standard copper-chromium catalyst UNH 103, the distillation product of the reaction is carried out by adjusting reflux ratio or intensity of heating of the cube so that the temperature of the vapor was 195 200oWith, and the final purification of p-dioxanone carried out by distillation under vacuum of 2 to 3 mm RT.article in the presence of boric acid.

 

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