The method of producing finaldestination

 

(57) Abstract:

The invention relates to the production of organosilicon compounds, in particular to a method of producing finaldestination that can be used in the manufacture of silicone fluids, resins and rubbers. The technical result of the invention is to increase the output of vinyldithiins. This technical result is achieved in that a method of obtaining vinyltoluene includes heat treatment of vinylpolysiloxane in the presence of hydroxides of alkaline or alkaline earth metals and optionally, of the halides of the alkali or alkaline earth metals as hydroxides of alkali or alkaline earth metals, take in the amount of 0.05 - 10 wt.% from the mass of vinylpolysiloxane. As of hydroxides of metals used KOH, LiOH, NaOH, Ca(OH)2or mixtures thereof, as well as halides of metals - KF, NaF, LiF, CaCl2CaF2or mixtures thereof. 1 C. p. F.-ly, 1 table.

The invention relates to the production of organosilicon compounds, in particular to a method of producing finaldestination that can be used in the manufacture of silicone fluids, resins and rubbers.

Known larianov by the reaction:

< / BR>
The output of vinyldithiins for this reaction is quite high 80-90% of theoretical, but the main disadvantage of this method is the inaccessibility and high cost source of CHLOROSILANES. Vinylidenechloride receive mainly by the reaction magyarkanizsa synthesis, along with the target vinylidenechloride 1 are formed and the products of incomplete organizowanie organdy and organochlorine, compounds II and III, respectively [2]

< / BR>
The separation of by-products from the target due to the close boiling points of these compounds and their high lability difficult and leads to the formation of a large number of products of thermal transformations (mostly plastic). At the same time during the processing of mixtures containing even a small amount of products II and III, a great number of vinylpolysiloxane General formula IV [1]

(CH3)n(CH2-CH)3-nSi[OSi(CH3)n(CH-CH2)2-n]kOSi(CH-CH2)3-n(CH3)n< / BR>
where n is 0 to 2;

k 2 10,

which significantly reduces the yield of the target finaldestination up to 30 to 40% of theoretical. It is known that polysiloxane can disintegrate under the action of hydrogen chloride authorities;

Hal is halogen;

p 1 4.

The reaction takes place when the content of the catalyst is 5 to 10 wt. temperature 30oC. the Yield of the target products 30%

The main disadvantage of this method is that the final product is a mixture of the same hardly separated CHLOROSILANES) I III.

It also describes the cleavage of siloxane bonds under the action of halides of metals [4]

-Si-O-Si- + MHalp__ -Si-Hal + -Si-OMHalp-1< / BR>
where M is a metal atom;

Hal is halogen;

p 3 4.

The process is carried out at a molar ratio of metal halide and siloxane 1 1, a temperature of -10oC. the Yield of the target products around 60%

The main disadvantage of this method, like the previous one, is that the result is a mixture of the same hardly separated CHLOROSILANES) I, III and complexity of separating from the reaction mass the other product of the reaction of Si-OMHalp-1that is a solid.

The closest in technical essence to the invention is a method of producing finaldestination by heat treatment vinylpolysiloxane in the presence of hydroxides and oxides of alkali metals [5]

Chemical transformations, taking place at the same time, can be represented schematically as Aubrey equimolar with respect to polysiloxane content of the catalyst, a temperature of 50 100oC. the Yield of the target products about 50%

The main disadvantage of this method is that the reaction along with the target disiloxane formed and the mixture silanolate organosilanes, the transformation of which into the target disiloxane represent a considerable challenge. This reduces the yield of the target disiloxane.

The technical result of the invention is to increase the output of vinyldithiins.

This technical result is achieved in that a method of obtaining vinyltoluene includes heat treatment of vinylpolysiloxane in the presence of hydroxides of alkaline or alkaline earth metals and optionally, of the halides of the alkali or alkaline earth metals as hydroxides of alkali or alkaline earth metals, take in the amount of 0,05 -10 wt. from the mass of vinylpolysiloxane. As of hydroxides of metals used KOH, LiOH, NaOH, Ca(OH)2or mixtures thereof, as well as halides of metals of KF, NaF, LiF, CaCl2CaF2or mixtures thereof.

The heat treatment is carried out at a temperature of from 50 to 200oC for 2 to 48 hours, the Yield of the target product is up to 65%

Schematically, the process can be reflected as follows:
500 g decivilisation added 2.5 g (0.5 wt.) caustic potassium and 2.5 g (0.5 wt.) fluoride of potassium, maintain the reaction mass at 180oC for 12 h, by distillation in vacuum allocate 150 g (55.3% of theory. ) hexaphenyldisilane, boiling point 58oC/2 mm, n2D0- 1,466; d2u00,8818.

The method according to the other examples perform similarly, the data in the table.

As can be seen from the presented example, under the proposed method get vinyltoluene with yields up to 65% while the prototype yield of the target product is up to 50%

Analysis of the known sources of information did not allow to find solutions describing the joint use of these compounds in the process of obtaining finaldestination to achieve the described result that could not be predicted based on the known level of science and technology. It follows from the above that the proposed solution is, in the opinion of the authors and applicants may be called upon appropriate criteria of "inventive step" and "novelty". The above example of the implementation of the proposed method demonstrates its compliance with the criterion of "industrial applicability".

Thus the proposed solution, according to the applicants and authors, is arabatyvat vinylpolysiloxane, formed as a by-product in a number of processes, expanding the raw material base receiving vinyldithiins.

Literature:

1. Andrianov, K. A. Methods of Organoelement chemistry. Silicon, M. Nauka, 1968, c. 548-581.

2. Mironov, C. F. Sheludyakov C. D. June Century. And. and Some other data about the synthesis of vinylsilanes, Ukr. General chemistry. 1980, so-50, N 4, S. 868-871.

3. Gotz J. Masson R. C. J. Chem. Soc. ser. A, 1970, p. 2683-2686.

4. H. Schmidbaur Hussek H. Schindler F. Chem. Ber. 1964, v. 97, p. 255-257.

5. Timofeeva, N. P. Uzilevsky Y. A. Yudin, I. P. Borisov, S. N. Skodinski K. I. Journal. General chemistry, 1969, T. 39, S. 2506-2509 (prototype).

1. The method of producing finaldestination by heat treatment vinylpolysiloxane in the presence of hydroxides of alkaline or alkaline earth metals, wherein the hydroxide of alkali or alkaline earth metal charge in the amount of 0.05 to 10 wt. from the mass of vinylpolysiloxane and the process is conducted in the presence of the halides of the alkali or alkaline earth metals, taken in an amount of 0.05 to 10 wt. from the mass of vinylpolysiloxane.

2. The method according to p. 1, characterized in that as the halides of the alkali or alkaline earth metals are used LiF, NaCl, NaF, KCl, KF, CaCl2CaF2or mixtures thereof.

 

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