The method of receiving performancenow
(57) Abstract:The invention relates to the technology for performancenow, in particular freon, OCTAFLUOROPROPANE, deceptibot used as insulators, refrigerants, components in the foaming and other compositions. Perforamcne get the fluoridation of performancenow C2-C4in a homogeneous phase in the environment of low molecular weight perforated solvent at a concentration of ftorirovannogo compounds 1-5 wt.%. Process temperature from minus 35 to minus 15oC. the Yield of the target products is 99 to 99.9%. 1 C.p. f-crystals, 2 tab. The invention relates to the technology for performancenow, in particular freon, OCTAFLUOROPROPANE, deceptibot used as insulators, refrigerants, components in the foamable compositions and laser environments, the working fluid in the plasma-chemical etching of semiconductor materials.Way of obtaining performancenow (APF) is known for the following: pyrolysis organofluorine raw materials, gas-phase fluorination of hydrocarbons and their galijasevic. The main drawback of these methods is the large number of products requiring imesa the APF receive or fluoridation of elemental fluorine or cobalt TRIFLUORIDE (wylo. application Japan 90-131438 and 85-81134, ed.St. The USSR 1630241, 1984). To regulate the heat dissipation processes lead in the environment diluent - tetrafluorodichloroethane (tiled Japan's bid 90-131438) or in two stages with the dilution of gesprochenen OCTAFLUOROPROPANE at the stage of start (ed.St. The USSR 1630241).For the prototype accepted way of getting one of performancenow - freon, which consists in the fluoridation of tetrafluoroethylene elemental fluorine in the environment of the diluent - tetrafluorodichloroethane, taken in an amount of 10 to 100 mol per 1 mol of tetrafluoroethylene, the ratio of fluorine to tetrafluoroethylene 1,2/1, the temperature of the process - an 80.2oC, freon - 87,8% (wylo. Japan's bid 90-131438).The disadvantages of this method include:
1. The method developed to obtain one perftoran - freon and was conducted in an environment OzonAction diluent.2. The yield of the target product is not high enough.The problem solved by this invention is to develop a universal method of fluorination performancenow with carbon chain C2-C4optimal combination of heat and material balances process and is suitable for industrial implementation proizvoditelna the essence of the invention consists in the following: the process is conducted in a homogeneous phase in the environment perfluorocarbons, which is a solvent for the fluorine and ftorirovannogo perforamcne, which together with thermophysical properties of perfluorocarbons provides intensive heat and mass transfer, preventing the destruction of carbon-carbon connection, the concentration of ftorirovannogo connection should not exceed 5 wt. %; the process temperature is minus 35 to minus 15oC; to prevent transfer of carbon-containing components in the gas phase process pressure support is not lower than the saturated vapor pressure of the solvent at the temperature of the process. If all these conditions, the yield is 99-99,9%.Deviations from the technological regime lead to the following effects:
when the temperature rises above minus 10oC, as well as the concentration perforamcne above 5%, the process becomes unstable, often accompanied by small explosions-clapping, and sometimes the explosion of the whole system; if the temperature is above -15oC reduces the yield of the target product;
at temperatures below minus 35oC and concentration perforamcne below 1% of the speed of the process is slowed down, resulting in reduced performance of the process.Used perfluorocarbon dissolve the Oia.Example 1.In the reactor of 12CR18NI10TI steel with a diameter of 45 mm and a height of 250 mm, provided with a jacket, stirrer, siphons for supplying fluorine and ftorirovannogo perforamcne, shutoff valves and pressure gauge, load 200 ml of perfluorinated solvent and cooling the reactor to a temperature of minus 30oC, then deliver the original perforance, and then the fluorine with a slight excess of stoichiometry (0,1 - 3%). After completion of the reaction the reaction mass is neutralized by passing through a filter with KPI (chemical lime absorber), and analyzed by GLC. The results obtained are presented in table. 1.From the data table. 1 shows that by increasing the concentration perforamcne more than 5% of the fluorination process becomes unstable and is accompanied by explosions-clapping. In the reaction mass, there are products of destructive fluorination - op. 4 and 5 - CF4in the op. 9 and 10 - CF4C2F6on the inner walls of the reactor and the siphons detected soot.Example 2.In the reactor described in example 1 and filled with solvent, serves simultaneously fluorine and perforance with the speed of 40.5 - 42 ml/min and 40 ml/min, respectively, the reaction products by flowing fitting received in the tion analyzed by GLC. If used, the solvent other than the target product, the products are subjected to rectification. The process parameters and the results are shown in table. 2.From table. 2 shows that during the process in these technological limits achieved a high yield of target product, and the process goes smoothly, with no explosions.Example 3.In the reactor, made of steel 12X18H10T, with a diameter of 0.4 m and a height of 1.9 m, equipped with a cooling jacket and the coil, the two bubblers and overflow fitting in the upper part of the load when cooled to -30oC 120 kg C3F8. The bubblers serves fluorine with a speed of 0.3-1.5 m3/h with an excess of 0.5% and hexaferrite with a speed of 0.3-0.5 m3/H. the reaction Products by flowing fitting come in the collection, cooled to minus 30-20oC, then the cartridge with KPI. The yield of the target product of 99.5%. Performance up to 15 kg/hAs can be seen from the experimental data, the proposed organization of the technological process allows to solve problems of heat transfer and get a number of performancenow one technology with high yield and productivity, acceptable to propyleneglycol technical and economic parameters of the process.Sources of information
1. Pat. USA 3222406, 260-653, 1965.2. Pat. USA 4377715, 570-123, 1983.3. Wylo. C-ka Japan 90-131438, C 07 C 19/08, 1990.4. Wylo. C-ka Japan 85-81134, C 07 C 19/08, 1985.5. Auth.St. The USSR 1630241, C 07 C 19/08, prior. 1984. 1. A method of obtaining a perfluorinated alkanes fluoridation performancenow elemental fluorine in the environment of fluorine-containing compounds, wherein the process is conducted in an environment of low molecular weight perfluorinated solvent components of the reaction at a temperature of minus 15 to minus 35oC and the concentration of the original perforamcne 1 to 5 wt.%.2. The method according to p. 1, characterized in that as the source perforamcne take perforamcne carbon chain WITH2- C4.
FIELD: industrial organic synthesis.
SUBSTANCE: invention is dealing with production of chlorohydrocarbons exhibiting plasticizing properties in polymer compositions in production of synthetic building materials, varnishes and paints, artificial films and leathers, in rubber industry, and as fire-retardant additives in polymers. Process comprises chlorination of waste obtained in production of C14-C32 fraction by ethylene-α-olefin oligomerization. Chlorination is accomplished in two steps: addition chlorination at 35-55°C followed by substitution chlorination at 40-105°C. Chlorohydrocarbons thus obtained can, in particular, be used as secondary plasticizer in polyvinylchloride compositions.
EFFECT: reduced expenses due to using production waste.
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