JPS6038324B2 - Production method of SF↓5Cl - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing SF5CI, and particularly to a method for producing SF5CI with high purity and high yield by relatively simple means and without complicated separation and purification means.

It is known that SF5, which is useful as a high voltage insulating material, can be obtained by thermally decomposing SF5CI. Conventional methods for manufacturing SF5CI include, for example, NO
By reacting F. Genka with sulfur dichloride to once produce SF4, removing the by-products produced at the same time, and reacting the purified SF4 with NOF and chlorine gas,
SF5CI was obtained together with the originating organism, and SF5 was purified from this.
A method for obtaining CI has been proposed.

(Refer to Special Publication No. 52-7398) However, according to this method, SF4 is once produced, purified, and further reacted with NOF, resulting in the production of SF5CI.
There are by-products mixed in, so not only did we find a complicated process to purify and remove them, but NOF is also highly corrosive, especially in the presence of trace amounts of moisture, which can lead to reactions. This method has drawbacks such as requiring fairly expensive corrosion-resistant materials for the equipment, etc., and cannot be said to be an industrially satisfactory method.

As a result of various studies and examinations aimed at eliminating these drawbacks and finding a means to obtain high-purity SF5CI through a simple reaction, the present inventor used a pyridine compound of hydrofluoric acid and combined it with sulfur dichloride and excess It has been found that by reacting with chlorine, SF5CI can be easily obtained selectively and in a gaseous state with good yield, and the above object can be achieved.

Further, according to studies by the present inventors, it has been found that in addition to pyridine, amines such as tertiary amines such as trimethylamiso and triethylamine, and pyridine derivatives such as quinoline and picoline can be used in the same manner.

The amine compound of hydrofluoric acid containing these amines used in the present invention is represented by the general formula A(HF)n.

The value of n is usually 1 to 6, and when employing 2 to 4 among these, it is particularly preferable because an industrially sufficient reaction rate can be obtained. Further, the above amines may be used alone or two or more of them may be mixed in an appropriate ratio.

There are no particular limitations on the method for synthesizing the amine compound of hydrofluoric acid used in the present invention, and known means may be employed as appropriate.

That is, for example, a method is employed in which an amine is placed in a hydrofluoric acid-resistant container such as polyethylene, and hydrogen fluoride (anhydrous hydrofluoric acid) is introduced while cooling from the outside. Such an amine compound of hydrofluoric acid is reacted with sulfur chloride and excess chlorine.

When carrying out the reaction, it is appropriate to introduce an amine compound of hydrofluoric acid into the reactor in advance, and then introduce sulfur chloride and excess chlorine in predetermined amounts into the reactor. There are no particular restrictions on the method of synthesizing sulfur chloride to be used in the reaction. For example, sulfur monochloride and chlorine may be reacted, or sulfur may be suspended in an inert solvent, a catalyst such as iodine may be added, and chlorine and chlorine may be synthesized. Any known method such as reaction may be employed as appropriate. When carrying out the method of the present invention, the amount of the amine compound of hydrofluoric acid used is:
A commonly used amine compound of hydrofluoric acid, namely A (HF)
Although it is strictly determined by the value of n, the charging molar ratio A/S (S: sulfur) is usually about 1 to 1, preferably about 4 to 8, per mole of sulfur in sulfur chloride. It is appropriate to adopt

If the amount used is less than the above range, the reaction rate of sulfur chloride will be low; on the other hand, if it exceeds the above range, a higher reaction rate can no longer be expected, and the amine compound of hydrofluoric acid will be unnecessarily degraded. Both methods are undesirable because they only increase the amount of amine handled in the post-treatment step. Further, the amount of chlorine used is in excess, and the amount is preferably more than 2 moles and less than 10 moles per mole of sulfur in the sulfur chloride used.

If the amount of chlorine used is less than the above range, the yield of SF5CI obtained will be insufficient for industrial purposes, and if it exceeds the above range, a large amount of unreacted chlorine will be mixed into the reaction product. Both are unfavorable because of the lotus.

Thus, to carry out these reactions, temperatures of 0 to 60°C;
It is appropriate to adopt a pressure of about 1 to 10 k9/swim-G.

Among these, when the temperature exceeds 60° C., the sulfur chlorides and amines used as raw materials may partially decompose, and reactions other than the intended reactions may proceed, creating dust, so care must be taken.

Although the reaction can be carried out in the absence of a solvent, it is preferable to use a solvent because the reaction can be carried out smoothly.

The solvent used must itself be inert to the raw materials and products, and halogenated hydrocarbons are generally suitable. Among these, methylene chloride, chloroform, carbon tetrachloride, fluorotrichloromethane, and trichlorotrifluoroethane are preferred, and these may be used alone or in an appropriate mixture. The appropriate amount of these solvents to be used is about 10 to 200% by volume based on the total amount of the reaction raw materials.

Further, as an apparatus for carrying out the reaction, for example, a complete mixing type reactor such as a batch type or a continuous type is suitable, and a complete mixing type reactor of a continuous raw material supply type is particularly preferred as an industrial apparatus.

When the method of the present invention is adopted, the amine itself does not directly participate in the reaction, but rather serves as a reaction medium, and the amine compound of hydrochloric acid produced by the reaction can be easily removed by reacting it with HF. It is possible to regenerate hydrofluoric acid as a reaction raw material into an amine compound, and when the method of the present invention is employed, there is an advantage that there is no need to use expensive fluorine gas at all.

Next, the present invention will be explained by examples.

Claims (1)

[Scope of Claims] 1. A hydrofluoric acid amine compound represented by the general formula A(HF)n (n=1 to 6), sulfur chloride consisting of sulfur dichloride and/or sulfur monochloride, and sulfur in the sulfur chloride. A method for producing SF_5Cl, which comprises reacting 1 mole with more than 2 moles and less than 10 moles of chlorine. However, the amine (A) is a single or a mixture of pyridine derivatives such as pyridine, quinoline, and picoline, and tertiary amines such as trimethylamine and triethylamine. 2. The method according to claim 1, wherein the amine compound of hydrofluoric acid to be subjected to the reaction has a charging molar ratio A/S (S: sulfur) of 1 to 15 with respect to 1 mole of sulfur in sulfur chloride.