The method of purification of perfluorinated organic compounds

 

(57) Abstract:

The invention relates to technology for deep cleaning perfluorinated aliphatic and cyclic compounds, such as performability, perpendicular, perfluorooctane, and perfluorinated polyethers, from chemically active fluorine-containing impurities. Perfluorinated compounds qualification "biologically inert" is produced by adsorption absorption of impurities. Pre-cleaned to the content of fluoride ion (2-4)10-4mol/l perfluorinated compound is passed through a column filled with Tripoli, and the process is conducted at 18-100°C until the content of fluoride ion (1-2)10-5mol/L. purification judged by the content of the fluoride ion in the treated compounds by the method of measurement of electrical resistance, which is 11015- 11016Omsm. The technical result - the simplification and cheapening of the way, reducing cleaning time. table 1.

The invention relates to technology for deep cleaning perfluorinated compounds aliphatic and cyclic - performability, performanceline, perfluorooctane, and perfluorinated polyethers.

These compounds find wide approx is orhii as intraoperative funds and perfluorinated polyethers used as a means for long-term tamponade of the retina. In connection with application in medicine the problem of purification of these compounds to biologically inert state, which is characterized by the presence of impurities in terms of the associated fluoride ion is not more than 10-5mol/l Value associated fluoride ion is characterized by the number of reactive fluorine-containing compounds present as impurities in the target perfluorinated compounds, and is determined by direct potentiometry using forselecting electrode. The accuracy of the method allows to determine the fluoride ion in an amount of 1 to 10-5mol/L.

In the process of fluorination any fluorinating agents perfluorinated compounds are formed along with detachable hard products of incomplete fluorination, volatile complex fluorides, including metal fluorides, which are chemically active impurities and can lead to instability of target products during storage and operation, which requires cleaning them at least until the qualification of "technical product" with the content of the linked fluoride ion (2-4)10-4mol/L.

Currently, technology is obtained by fluorination reaction mixture is "raw" water or aqueous-alcoholic alkali solution to remove the hydrogen-containing and acidic impurities, followed by distillation of the organic fraction (U.S. patent 3381201, J.-L. go active. chemistry, 1996, T. 69, vol. 1, S. 112-119, European patent 271272) and deep purification of the products obtained from traces of hydrogen and olefinic compounds of lower aliphatic primary or secondary amines (European patent 415264) or by fluorination of elemental fluorine, followed by neutralization and filtration through a column with silica gel and activated carbon (W-l go active. chemistry, 1996, T. 69, vol. 1, S. 112-119).

As the prototype is set to the method described in the above journal of applied chemistry (S. 116), which are as follows, through the rectified obtained after treatment with a water-alcohol solution of alkali content of fluoride ion 210-4mol/l, bubbled 10-30% ferastrau the mixture at 10-20oC for 10-15 hours fluorinated product is neutralized and sequentially passed through the adsorbent is silica gel and activated carbon. Purified in this way, the product has the following characteristics quality: the fluoride ion (1-3)10-5mol/l and negligible absorption in the region of 200-320 nm UV spectrum that is teaching the prototype is a multistage - treatment with fluorine, neutralization, adsorption treatment and is associated with the use of toxic elemental fluorine.

The invention solves the problem of obtaining high-purity perfluorinated compounds using on the stage of deep cleaning only adsorption methods, which leads to a considerable simplification and cheapening of the way, and reduce cleaning time.

The invention consists in the following: pre-cleaned to the content of fluoride ion (2-4)10-4mol/l perfluorinated compound is passed through a column filled with Tripoli, and the process is conducted at 18-100oC to the content of fluoride ion (1-2)10-5mol/L.

Tripoli (diatomaceous earth) - friable sedimentary rock consisting mainly of silica with a mixture of alumina, iron oxides, calcium, magnesium, without organic residues (BAS, 1956, T. 43, S. 196; encyclopedia of inorganic materials, 1977, so 2, S. 586; BAS, 1977, T. 26, S. 545).

It is known that the diatomaceous earth used as sorbents in the regeneration of transformer oils, filter, oil products and gases in processes of cleaning and bleaching of sugar syrups, animal and vegetable oils, glycerin, fruit juices. Information is the connection, no. In addition, the authors found that when cleaning the Tripoli improving such factors as the electrical resistance, which indicates the absence of impurities, not defined potentiometric and not fixed by a known method.

Examples.

Deep cleaning by the claimed method were subjected to the following connections:

perpendicular, perpertrating, performability, performability ether, perfluorinated polyethers of the General formula

< / BR>
(fraction with the initial boiling point 130oC at 1 mm RT.CT.) (Industrial organic products. The Handbook. - St. Petersburg: Chemistry, 1996, S. 485).

A typical experiment.

In column equipped with a bottom fitting, height 1000 mm, an inner diameter of 10 mm load 100 g of Tripoli and pass the cleaned product. The process parameters, the source and purity of the final product presented in the table.

From the presented experimental data it follows that the proposed cleaning method is simple, does not require the use of toxic fluoride and allows you to get perfluorinated compounds qualification "biologically inert" a higher degree of purification, as evidenced by Tae other silicon-containing sorbents, even such are similar in composition and properties to Tripoli, as diatomite, does not achieve the desired result (TSB, 1952, so-14, S. 308 and TSB, 1972, T. 8, S. 240).

The method of purification of perfluorinated organic compounds from chemically active fluorine-containing impurities, comprising contacting the purified compounds with silicon-containing sorbent, wherein the perfluorinated compounds having the value associated fluoride ion (2-4)10-4mol/l, is subjected to contact with Tripoli at 20-100oC.

 

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