The method of obtaining and purifying 1,1-differetn and thus obtained product

 

The invention relates to cleaning and getting 1,1-dottorato, which is used for foaming plastics or as a propellant in aerosols. The cleaning method is carried out by processing gidroftoridakh crude 1,1-diflorasone, in which the content of the hydrochloride is less than 1 mole per 1 mole of 1,1-differetn. The treatment is carried out in conditions similar to the conditions of synthesis of 1,1-differetn by hydroperiodide chlorinated hydrocarbon. Preferably the treatment is carried out in the liquid phase in the reaction medium containing at least 500 grams of HF per 1 kg of 1,1-diflorasone, in the presence of a catalyst. As catalyst, use derivatives of metals of groups IIIa, IVa, IVb, Va, Vb, and VIb of the Periodic table of elements and mixtures thereof. Method for obtaining 1,1-deepthroatin by the interaction of hydrohloride with chlorinated precursor 1,1-diflorasone, optionally in the presence of a catalyst. Get the crude product containing 1,1-differetn and hydrochloride, which is separated. The resulting product containing less than 1 mol Hcl 1 mol of 1,1-differetn, treated with gidroftoridakh and get purified 1,1-differetn. Also suggested that a mixture containing 1,1-differetn with purity above and 99.8 weight. % polucheniya - the increased purity of the target product. 3 S. and 7 C. p. F.-ly, 3 tables. , 2 Il.

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Claims

1. The method of purification of 1,1-differetn from vinyl chloride, comprising processing gidroftoridakh crude 1,1-diflorasone, in which the content of the hydrochloride is less than 1 mol per 1 mol of 1,1-diflorasone, in conditions close to the conditions of synthesis of 1,1-differetn by hydroperiodide chlorinated hydrocarbon.

2. The method according to p. 1, in which the crude 1,1-differetn contains 1 kg of 1,1-differetn less than 50 g of 1-chloro-1-floridana and less than 20 g of 1,1-dichloroethane.

3. The method according to p. 1 or 2, in which the treatment is carried out in the liquid phase in the reaction medium containing at least 200 g of HF to 1 kg, preferably at least 500 g HF 1 kg.

4. The method according to one of paragraphs.1-3, in which the treatment is carried out in the presence of a catalyst of hydroperiodide selected from the group comprising derivatives of metals of groups IIIa, IVa, IVb, Va, Vb, and VIb of the Periodic table of elements and mixtures thereof, preferably from derivatives of tin, molybdenum, titanium, vanadium, antimony or tungsten.

5. The method according to one of paragraphs.1-4, in which the processing of crude 1,1-differetn provide continuous method at a flow rate of from 0.01 to 5 kg/Gerasim predecessor 1,1-diflorasone, if necessary, in the presence of a catalyst of hydroperiodide obtaining a crude product containing 1,1-differetn and hydrochloride, Department hydrochloride obtained from the crude product and the subsequent processing of the obtained product containing less than 1 mol Hcl 1 mol of 1,1-diflorasone, gidroftoridakh obtaining purified 1,1-differetn.

7. The method according to p. 6, characterized in that the separation of Hcl is carried out in a distillation column to remove Hcl from the upper part of the column and removing from the lower portion of the column of the crude reaction product intended for further processing.

8. The method according to p. 6, characterized in that the separation of Hcl is carried out in a distillation column to remove Hcl from the upper part of the column, the lateral extraction of the crude reaction product intended for further processing, and removing VAT residue containing products heavier than 1,1-differetn, and this VAT residue, if necessary, return to step a).

9. The method according to one of paragraphs.7 and 8, characterized in that it contains an additional distillation of the crude reaction product leaving the column distillation Hcl, extracted from the upper part of the column of product, prednaznachen heavier than 1.1-differetn, and this VAT residue, if necessary, return to step a).

10. A mixture containing 1,1-differetn with purity above and 99.8 wt.%, preferably than 99.9 wt.%, received hydropericardium chlorinated hydrocarbons, and containing a vinyl chloride below 10 mg/kg, preferably below 5 mg/kg

 

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