The method of obtaining oxide hexaferrite

 

(57) Abstract:

The invention relates to a method for producing oxide hexaferrite liquid-phase oxidation of hexaferrite environment, trifluorotrichloroethane, and the oxidation of hexaferrite carried out in the presence of heated metal surface with a temperature below 170°C with simultaneous removal of heat from the reaction zone. The invention can be used in organofluorine chemistry to obtain oxide hexaferrite, which is an intermediate for obtaining surfactants, oils, solvents, etc. the Technical result - obtaining conversion hexaferrite, close to 100% when entering the downloaded HEXAFLUOROPROPYLENE about 75-85%. table 2.

The inventive object is to organofluorine chemistry. Oxide of hexaferrite (EGFP) are used for obtaining surfactants, parfocality oils, solvents, perfluorinated alkylvinyl esters, etc. (L. F. Sokolov, P. I. Shafts, S. C. Sokolov. // USP, 1984. So LIII. Vol. 7. C. 1222-1246).

A method of obtaining EGFP oxidation of hexaferrite (HFP) an alkaline solution of hydrogen peroxide (Eleuterio H. S. // J. Macromol. Sci., Chem., 1972, v. The paragraph does not exceed 45%.

Output EGFP does not exceed 50% and in another way - oxidation HFP hipogalactiei alkali and alkaline earth metals in aqueous solution at atmospheric pressure and room temperature (Izv. An SSSR, Ser. chem., 1979, S. 2812. A. J. Zapevalov, and others).

Closest to the claimed is a method for EGFP oxidation HFP oxygen in inert solvent (U.S. Pat. USA 3536733, 1970). The process is carried out in a stainless steel autoclave with stirring at a temperature of 430 K, a pressure of 2.8 MPa in the environment of Halocarbon 113. Conversion of HFP reaches 70%, and the output EGFP on unreacted HFP - 70%,

Further processing EGFP raw involves dividing EGFP and HFP, which have practically the same boiling point - 29oC. Commonly used methods of extractive distillation and the photochemical synthesized or chlorination lead to a significant complication of technology, the increase of the expenditure ratio and the cost of the target product.

Therefore, the main task for the authors of the present invention was to obtain the highest possible conversion of HFP with acceptable yield and reaction time.

To solve the task oxide using submersible heated metal surface with a temperature not lower than 170oC, which in these conditions generates active centers, as the initiator of the chain oxidation process. Unlike the closest analogue that allows you to get the HFP conversion close to 100%, and the output EGFP reaches 87%.

Table 1 shows the mapping of the data closest analogue and the proposed method. As can be seen from table 1, the inventive method is characterized by higher than in the nearest analogue output EGFP and conversion of HFP. close to 100%, which allows to exclude from the process flowsheet stage of purification of the target product from the source of raw materials.

The applicant asserts that the proposed facility meets the criteria of the invention "inventive step", because in the patent and scientific and technical documentation are not found together claimed funds in the solution method of obtaining EGFP known to specialists in this field.

Examples of industrial application of the claimed method.

Example 1. In a reactor of 10 l load 8 kg halon 113 and 4 kg of HFP. Heat the reaction mixture to 150oC. with Nitrogen to create a pressure of 3 MPa. Include mixing. Using a submersible heat exchanger remove heat of reaction and maintain temp nl/hour. These settings support for 100 minutes Off the oxygen supply. Poured the reaction mixture. 4 kg loaded HFP get 330-350 g EGFP.

Example 2. In a reactor of 10 l load 8 kg halon 113 and 4 kg of HFP. Heat the reaction mixture to 150oC. Nitrogen creates a pressure of 3 MPa. Include mixing. Include oxygen with a flow rate of 400 to 450 nl/h. The reactor is mounted submerged in the reaction mixture an electric fuel element in a metal casing, the surface of which is supported at a temperature of 175oC. the Heat of reaction away with coolant, which is supplied to the jacket of the reactor. These settings support for 100 minutes Off the oxygen supply. Poured the reaction mixture. 4 kg loaded HFP get 330-350 g EGFP.

The main options of the industrial implementation are shown in table 2, including the option # 1. The Complainant submits that all the intervals of variation of parameters are workable.

This shows that the applied method allows in industrial conditions to obtain the oxide of hexaferrite with the release of 75-85% on the downloaded HEXAFLUOROPROPYLENE when conversion hexaferrite, b is on in the environment, trifluorotrichloroethane, characterized in that the oxidation hexaferrite carried out in the presence of heated metal surface with a temperature below 170°C with simultaneous removal of heat from the reaction zone.

 

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