The method of obtaining organosiloxane silanes

 

(57) Abstract:

Describes how to obtain organosiloxane silanes by reacting granular magnesium obtained by granulation in a magnetic field, with organohalogenated and tetrafunctional the silane at high temperatures, namely, that as granulated using magnesium magnesium obtained by granulation in a magnetic field in the presence of helium-air atmosphere. The technical result is to reduce the viscosity of the product of synthesis and the reduction of the length of the induction period.

The invention relates to the chemistry of organosilicon compounds, in particular to methods for organoselenium silanes, and can be used to obtain silicone fluids and resins of various types.

A method of obtaining organosiloxane silanes (Ed. mon. The USSR 477626, publ. B 30, 1985) by the interaction of granulated magnesium with organohalogenated and tetraalkoxysilane. Magnesium is used in the form of granules with a size of up to 0.6 mm

However, the use of magnesium of this type does not allow continuous synthesis. Small particle sizes do not allow reached the same which leads to the decrease of the degree of utilization of magnesium.

Also known is a method of obtaining organosiloxane silanes (Ed. mon. The USSR 726825, publ. B 30, 1985) by the interaction of granulated magnesium granule size 1-20 mm organohalogenated and tetraalkoxysilane at elevated temperature.

However, the use of granulated magnesium of this type yields a product with high viscosity and a high content of magnesium in it. Another disadvantage of the process is the significant cost of this type of magnesium associated with the lack of domestic (Russian) production of this type of magnesium and monopolist manufacturer.

Closest to the proposed number of common features is a method for organoselenium silanes (RF patent 2079502, publ. B 14,, 20.05.1997) by the interaction of granulated magnesium granule size 1-20 mm, obtained by granulation in a magnetic field in an atmosphere of air, with organohalogenated and tetrafunctional the silane at high temperatures.

The disadvantages of this method of obtaining organosiloxane silanes are significant viscosity products synthesis, essential will continue orida and not more of 50.4% for formanilide). And used granulated magnesium obtained in a magnetic field in an air atmosphere, has a low quality due to the ingress of gas inclusions of air in the granules of magnesium, in addition, the form of granules in needle form does not allow you to speed up the synthesis of silanes.

The objective of the invention is to eliminate the disadvantages of the prototype, namely the decrease of the viscosity of the product of synthesis and the reduction of the length of the induction period.

The technical result is to increase conversion organomanganese

The task is solved in that in the method of obtaining organosiloxane silanes by reacting granular magnesium obtained by granulation in a magnetic field, with organohalogenated and tetrafunctional the silane at high temperatures, it is new that as granulated using magnesium magnesium obtained by granulation in a magnetic field in the presence of helium-air atmosphere.

The use of granulated magnesium obtained in a magnetic field in the presence of helium-air atmosphere, higher quality and spherical shape reduces the viscosity of the product of synthesis, to reduce the duration indunil the applicant's analysis of the prior art, including searching by the patent and scientific and technical information sources and identify sources that contain information about the equivalents of the claimed invention, has allowed to establish that the applicant had not found the source, which is characterized by signs, identical all the essential features of the invention. The definition from the list of identified unique prototype as the most similar set of features analogue has allowed to establish the essential towards perceived by the applicant to the technical result of the distinctive features in the proposed method, set forth in the claims.

Therefore, the claimed invention meets the condition of "novelty."

To verify compliance of the claimed invention the term "inventive step", the applicant conducted an additional search of the known solutions to identify signs that match the distinctive features of the prototype of the characteristics of the claimed method. The search results showed that the claimed invention not apparent to the expert in the obvious way from the prior art because the prior art, a particular applicant identified the impact of the envisaged sushestvenno, the claimed invention meets the condition of "inventive step".

Getting granular magnesium in a magnetic field in a helium-air atmosphere produced as follows. Included the electric furnace and was heated magnesium in the tank to the melting temperature, applied voltage from the transformer on metalloprokat with dispersant and warming them up to 700-750oWith the included supply of helium under the bell. Since the density of helium is much less than density of air, he pushed the air from the bell and created a layer of a given thickness. Before applying metal dispersant turned on the electromagnet and created a magnetic field of more than 1,6105A/m, and the electrodes of the dispersion chamber filed a voltage from an AC field. The oscillation frequency is set from 400 to 800 Hz. Drops were steroidesherbal in an inert gas (helium) and after cooling in air to fall in the form of granules in a container for collecting the finished product (in detail in the patent of the Russian Federation 2117553).

Example 1.

In a two-liter chetyrehosnuju flask equipped with a stirrer with trap, thermometer, reflux condenser and a separating funnel, downloaded 73 kg magnesium obtained by granulation in magnetic Rive flask was heated to 150-160oC and from a separating funnel introduced part (20-40 ml) of a mixture of 310 ml chloride benzene with 20 ml of bromacil and 40 ml of phenyltrichlorosilane. The synthesis began that hour, without an induction period. The rest were introduced at a temperature of 140-170oWith over three hours. The heat of reaction averted by cooling the flask in an oil bath. After stirring the contents of the reactor for three hours at a temperature of 150-160oWith the process stopped.

Received the product with a viscosity of 18 cSt.

The composition phenylsilane silanes, wt.%:

The tetraethoxysilane - 39

Phenyltriethoxysilane - 30

Diphenyldichlorosilane - 14

The calculated composition of the product of synthesis conversion formanilide amounted to 70%.

Example 2 - the prototype.

In a two-liter chetyrehosnuju flask equipped with a stirrer with trap, thermometer, reflux condenser and a separating funnel, downloaded 73 kg magnesium obtained by granulation in a magnetic field in an atmosphere of air, with grain sizes 1-8 mm (mainly in the form of needles in size 4-8 mm) and 630 ml of tetraethoxysilane. The contents of the flask were heated to 150-160oFrom a separating funnel introduced part (20-40 ml) of a mixture of 310 ml chloride benzene with 20 ml of bromacil and 40 m is of three hours. The heat of reaction averted by cooling the flask in an oil bath. After stirring the contents of the reactor for three hours at a temperature of 150-160oWith the process stopped.

Received the product with a viscosity of 50 Centistokes.

The composition phenylsilane silanes, wt.%:

The tetraethoxysilane - 39

Phenyltriethoxysilane - 29

Diphenyldichlorosilane - 10

The calculated composition of the product of synthesis conversion formanilide was 62%.

As can be seen from examples 1 and 2, the proposed method for phenylsilane silanes leads to lower viscosity of the product of synthesis from 50 to 18 cSt, the elimination of the induction period, the increase in conversion phenylaniline from 62 to 70%.

Example 3.

In a two-liter chetyrehosnuju flask equipped with a stirrer with trap, addition funnel and reflux condenser, downloaded 73 kg magnesium (3.0 g-at) obtained by granulation in a magnetic field in a helium-air atmosphere, with a grain size of 1-3 mm spherical shape. The contents of the flask were heated to 60-70oFrom a separating funnel introduced part (10-20 ml mixture) ethylchloride (126 ml, 1,800 mol) of tetraethoxysilane (168 ml; 0,750 mole) and 300 ml of toluene. The reaction started immediately or through titerature 40-60oWith in 30 minutes. Then the flask immediately or within half an hour was introduced a mixture of ethylchloride (84 ml, 1.200 mol), tetrachlorosilane (69 ml; 0,600 mole) 253 ml of toluene also during cooling and the temperature of 40-60oWith in 30 minutes.

Received the product with a viscosity of 2.7 cSt.

The composition tilsammen silanes, wt.%:

Diethylmethoxyborane - 43

Triethylaluminium - 16

Hexaethyldisiloxane - 1

The calculated composition of the product of synthesis conversion ethylaniline amounted to 97.8 per cent.

Example 4.

In a two-liter chetyrehosnuju flask equipped with a stirrer with trap, addition funnel and reflux condenser, downloaded 73 kg magnesium (3.0 g-at) obtained by granulation in a magnetic field in an air atmosphere, with a granule size 1-8 mm (mainly in the form of needles with a size of 4-8 mm). The contents of the flask were heated to 60-70oFrom a separating funnel introduced part (10-20 ml mixture) ethylchloride (126 ml, 1,800 mol) of tetraethoxysilane (168 ml; 0,750 mole) and 300 ml of toluene. The reaction started immediately or after two minutes and was characterized by the rise of temperature up to 75-90oC. the Remaining part was introduced during cooling and the temperature of 40-60oWith in 30 minutes. Then the flask immediately or within half an hour was introduced a mixture of these is P>oWith in 30 minutes.

The duration of the induction period of 10-20 minutes.

Received the product with a viscosity of 9.0 cSt.

The composition tilsammen silanes, wt.%:

Ethyltriethoxysilane - 7

Diethylmethoxyborane - 55

Triethylaluminium - 8

Ethyltrichlorosilane - 3

Diethyldichlorosilane - 19

Triethylchlorosilane - 5

Hexaethyldisiloxane - 2

The calculated composition of the product of synthesis conversion ethylaniline was 93%.

As can be seen from examples 3 and 4, the proposed method for tilsammen silanes leads to lower viscosity of the product of synthesis from 9 to 2.7 cSt, to eliminate or reduce the duration of the induction period of up to two minutes, increase conversion ethylaniline from 93 to 97.8 per cent.

The method of obtaining organosiloxane silanes by reacting granular magnesium obtained by granulation in a magnetic field, with organohalogenated and tetrafunctional the silane at elevated temperature, characterized in that the quality of wood pellets using magnesium granules obtained in a magnetic field in a helium-air atmosphere.

 

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