The method of purification of 1,1,1-ferrichloride

 

(57) Abstract:

The method of purification of 1,1,1-ferrichloride refers to the chemical industry and can be used to remove impurities chloride vinylidene of 1,1,1-ferrichloride (halon V, or hydrochlorofluorocarbons FC-V), which is used as ozone-component fluids, aerosols, pore-formers, solvents, and as an inhalation anesthetic. The method consists of contacting halon V in the liquid phase with halogen. As the use of halogen gas is fluorine. Contacts are by ozonation last through the cleaned refrigerant V when pressure and temperature, which determine the presence of halon V in the liquid phase. Fluorine take in the amount of 1.2 to 5, preferably 2 to 3 mol per 1 mol of chloride vinylidene in the treated product. You can use electrolytic fluorine, purified from hydrogen fluoride. The invention can effectively clean the refrigerant V without loss last in the cleaning process. 3 C.p. f-crystals, 1 table.

The invention relates to the chemical industry and can be used to remove impurities chloride vinylidene of 1,1,1-ferrichloride (halon V, or hydrochlorofluoro, solvents, as well as inhalation anesthetic. Chloride vinylidene

highly toxic impurity, are not separated from the halon V rectification because of the proximity of the boiling points (at 31.7 and 31,9oC, respectively).

A known method of purification of 1,1,1-ferrichloride from unsaturated compounds by adsorption on activated carbon with a specific particle size (U.S. patent N 4950816, 1990). The residual chloride content of vinylidene in purified product 0,02%

In another known method (U.S. patent N 4940824, 1990) conducted a cleanup 1,1,1-ferrichloride in liquid or gas phase to a residual chloride content of vinylidene 0.005 wt. using as adsorbent carbon molecular sieve with a pore size of 0.42 to 0.45 nm, -20 to +60oC.

Both these methods require cooking and frequent regeneration of the adsorbents, and the latter have a limited life; all this complicates the known methods using adsorbents.

For removal of chloride of vinylidene know the use and chemical cleaning methods. So, in one of them (European patent N 0353059, 1990) 1,1,1-ferrichloride obtained gas-phase catalytic reaction of chloride vinylidene with fluoride votary delete processing of the water alkaline permanganate solution (chloride vinylidene oxidized, the oxidation products laundered), or bromirovanii (chloride vinylidene turns into a high-boiling dibromopropane, which is separated by rectification). The disadvantage of this method is that in the process of cleaning chloride vinylidene converted into unusable connection.

Closest to the proposed combination of essential characteristics is known (European patent N 0401493), in which a liquid mixture containing 1,1,1-ferrichloride and chloride vinylidene, treat it with chlorine, and then irradiated with ultraviolet light receiving chloride vinylidene product of his fotogalereya 1,1,1,2-tetrachlorethane, easily detachable from 1,1,1-ferrichloride rectification.

The disadvantage of this method is the partial chlorination in the treatment process and the 1,1,1-ferrichloride that leads to its loss.

The technical problem solved by the invention is the elimination of this drawback. The task is solved in that in the known method of purification of 1,1,1-ferrichloride by contacting in the liquid phase with halogen as the use of halogen gas is fluorine, and the contacting lead by ozonation of fluorine gas through the eyes of the phase. When the fluorine take in quantities of 1, 2 5, preferably 2 to 3 mol per 1 mol of chloride vinylidene in the treated product. In addition, the use of electrolytic fluorine, purified from hydrogen fluoride.

Example. For cleaning take halon V obtained by hydroperiodide chloride vinylidene or chloroform. The content of impurities in the source halon in each experiment is shown in table. As a cleansing agent used fluoride obtained by electrolysis TRIFLUORIDE, potassium, purified from hydrogen fluoride (op. 9 and 10), and without purification from hydrogen fluoride (all other experiments).

Experiments 1 13 held in the reactor column type with a diameter of 37 mm and a height of 525 mm, made of fluoroplastic-4, equipped with a back-brine refrigerator of the same material, thermogenesis and switchgear in its lower part for supplying fluorine. Experiments 14 and 15 carried out in a reactor with a diameter of 24 mm and a height of 460 mm similar design made of Nickel and is additionally equipped with a brine shirt; these experiments were conducted at atmospheric pressure, although it can be carried out at elevated temperature and pressure required to maintain halon V is dubsta the dosage on loss of pressure) is supplied from the tank into the reactor through a calibrated metering washer. Previously in the reactor is placed purified Halocarbon V and include cooling the back of the refrigerator. Fluorine is served in the lower part of the reactor, barbotine it through a layer of cleaned halon. Unreacted fluorine and acid components absorb in the system of wash tanks with a water solution iodotope potassium, which direct the gases after the return of the refrigerator. Neutral gas is quantitatively collected in a Gasometer. The helium gas analysis calculate the flow rate of the fluorine in the experience. At the same time replacing the Gasometer select a sample of liquid refrigerant from the reactor, after which the washing of acidic impurities and drying analyze chromatography. The composition of the purified product is shown in the table. Analysis of wash water and the quantity of fluorine determine the degree of reaction of fluorine. The specific conditions of the experiments and the results in the table.

From the above results of the experiments shows that the proposed method allows you to clear the halon V from chloride vinylidene to content less than 0.001 mol. However, observe conditions effective ozonation of fluorine through the layer of liquid refrigerant, which requires a sufficient height of the liquid layer. You can use untreated electrolytic FPO is either op.9 and 12) and other conditions. He is always slightly above stoichiometric, as part of the fluorine spent on the destruction of moisture. So, when a molar ratio of fluorine to chlorine vinylidene less than 1.2, the degree of purification is insufficient (op. 8). However, the high consumption of fluoride (more than 5 mol per 1 mol of chloride vinylidene) is not justified economically. The best results are achieved when the molar ratio of fluorine to chlorine vinylidene 2 3.

The table shows that in the cleaning products contain almost no halon 133, which is the product of the fluorination of 1,1,1-ferrichloride, indicating the absence of losses last in the cleaning process.

Thus, the proposed method allows efficient purification of 1,1,1-ferrichloride from chloride vinylidene lossless 1,1,1-ferrichloride in the cleaning process.

1. The method of purification of 1,1,1-ferrichloride from chloride vinylidene by contacting in the liquid phase with halogen, characterized in that as the use of halogen gas is fluorine and the contacting lead by ozonation of fluorine gas through the purified 1,1,1-ferrichloride when pressure and temperature, causing the stay 1,1,1-ferrichloride in the liquid phase.

the second product.

3. The method according to p. 2, characterized in that the fluorine take 2 to 3 mol per 1 mol of chloride vinylidene in the treated product.

4. The method according to PP. 1 to 3, characterized in that use electrolytic fluorine, purified from hydrogen fluoride.

 

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