CS240262B1 - A method for saturating pyridine sulfur or quinolinic acid - Google Patents

Abstract

The method of saturating pyridinesulfuric or quinolinesulfuric acid in the technological process of obtaining pyridine or quinolinesulfuric bases is discussed. Its essence lies in the fact that ammonia water or ammonia distillate from the distillation processing of crude tar and benzole is used to saturate pyridinesulfuric or quinolinesulfuric acid in the production of pyridine and quinolinesulfuric bases.

Description

The invention solves the process of: saturating pyridine sulfuric acid or quinoline sulfuric acid in a process for obtaining pyridine or quinoline bases.

According to known methods, the saturation of pyridinic acid or quinoline sulfuric acid is carried out with gaseous ammonia or an inorganic alkaline solution in order to release the bound bases for their further use. Usually, on an industrial scale, saturation of said acids with ammonia gas is used for ease of manipulability, more convenient use of the resulting ammonium sulfate, and obtaining a more concentrated ammonium sulfate solution. and

In the technological process of _t destilačnlho processing crude tar and benzol formed ammonia water, which are usually connected, are stripped of their most volatile constitutents in the so-called. Ammonia distillate and residual vodný- venturer · -zpracovává on-the sewage-treatment plant.

Ammonia distillate is either disposed of by incineration or used to dispose and neutralize acid waste. According to the analysis carried out, the ammonia distillate contains, in addition to water, a considerable amount of ammonia, hydrogen sulfide, pyridine bases and small amounts of other compounds such as hydrogen cyanide, hydrogen rhodium, phenols, etc.

Many of these compounds are very valuable and their recovery is highly desirable. For example, pyridine bases containing 4 to 8% by weight of ammonia distillate consist of 80% pyridine and 15% 2-methylpyridine. However, neither ammonia water nor ammonia distillate is used in the crude tar and benzol processing complex to obtain the above-mentioned valuable proportions.

This deficiency is solved by the method of saturation of pyridinic acid or quinoline sulfuric acid according to the invention. It consists in using ammonia water or ammonia distillate from the distillation treatment of crude tar and benzene, and / or ammonia distillates obtained from these waters, from which optionally hydrogen sulphide is removed to saturate pyridine sulfuric acid or quinoline sulfuric acid in the preparation of pyridine or quinoline bases. .

By using said method of saturating pyridine sulfuric acid or quinoline sulfuric acid, the ammonia contained in the present ammonia waters and ammonia distillates is utilized and at the same time the pyridine bases contained therein are transferred to the base layer released from the saturated acid. This results in substantial savings in ammonia gas, which is usually carried out by saturation.

A considerable benefit is also obtained by obtaining pyridine and 2-methylpyridine contained in ammonia waters together with bases released from saturated acid.

Indeed, from an economic and balance point of view, ammonia water from crude tar and benzol treatment is a much more advantageous source of pyridine than the tar fractions hitherto used (particularly light and carbolic oil). Also in terms of occupational safety is handling ammonia v-Qda or ammonia distillate. • much safer than handling. with gaseous ammonia.

He did

94.3 parts by weight of pyridine sulfuric acid were saturated with stirring and cooling of 95 parts by weight. parts of the ammonia distillate obtained as the first portion from the distillation of the combined ammonia water from the distillation of tar and crude benzols containing 18.2 wt. % ammonia, 5.8 wt. % hydrogen sulfide, 4.8 wt. % of pyridine bases, 0.5 wt. % phenox, less than Q, 1 wt. neutral organic substances.

Saturation yielded 15 wt. parts of a pyridine base-α-174 _T 3-wt-aqueous ammonium sulfate solution. Saturating the same amount of pyridine sulfuric acid with ammonia gas yielded 10.3 wt. diupyridine bases.

Example 2

The ammonia distillate described in Example 1 was in an amount of 100 wt. parts mixed with 25 wt. parts of a 40% aqueous ferric chloride solution. After separation of the resulting ferrous sulfide, 94.3 wt. % of pyridine sulfuric acid.

Saturation yielded 13 wt. parts of pyridine bases and 171.3 wt. parts of ammonium sulfate solution, wherein the content of hydrogen sulfide does not exceed a 0.05,% <rhmot _<·· · - · · · (unf.f: IU / Vd '.-.' Ή ⁷ '- · Λ' / , 'ϊ

Ibří-kl and d-3. ,;. '·. ·? ·. _: -V _r ~. »·. {Ammoniacal distillate -" PP written · s Example-1 was -v: Quantity - 90.- weight dílů..použit ,, \ saturation 94.3, wt . part of the pyridinic acid. D, o {saturation; of the reaction mixture, e.g., 7.5-8, was preyedan-gaseous, ammonia-saturated. parts of pyridine bases and 172.5 wt. % of ammonium sulfate.

Example'4

Ammonia water obtained in the distillation of tar dewatering, containing 1,2% by weight of water. % pyridine bases, 0.2 wt. % ammonia, 0.5 wt. % hydrogen sulfide and 1.7 wt. phenols, was used in an amount of 100 wt. parts for pre-saturation 94.3 wt. % of pyridine sulfuric acid. After the reaction mixture was saturated with ammonia gas to pH = 8, 11.2 wt. % of pyridine bases.

Example 1 a d 5

The ammonia distillate described in Example 1 was in an amount of 1.00 wt. parts used to saturate 95 wt. parts of quinolinesulfuric acid. After saturating the mixture with ammonia gas to pH = 7.8, 17.4 wt. % of quinoline bases.

Claims (2)

SUBJECT A process for the saturation of pyridine sulfuric acid or quinoline sulfuric acid in a process for obtaining pyridine or quinoline bases, characterized in that ammonia water from the crude dehydrotreatment process and the benzol and / or ammonia distillates obtained therefrom are used for partial or complete saturation. Method according to claim 1, characterized in that hydrogen sulphide is removed from the ammonia water and / or the ammonia distillates before partial or complete saturation.