US1167061A - Process of manufacturing barium chlorid. - Google Patents

Description

pnirnn sra'rns rarnn'r oriuon.

E'INAR VAN'G GRANtjf OF LEONIA, -NEW JERSEY.

PROCESS OF, MANUFACTURING BAR-IUM CHLORIID.

No Drawing.

. T 0 all whom it may concern:

Be it known that I, EINAR VANG GRANo, a citizen of the United States, residing in Leonia, county of Bergen, andrState of New Jersey, have invented new and useful lmprovements in Processes of Manufacturing Barium Chlorid, of which the following is a specification.

This invention relates to the manufacture of barium chlorid from barium sulfid ob-' sufficient quantities in the outlying localities where it is necessary to set up plants for its production if the commercial manufacture is to be successful.

I discovered that not only can a substanti ally quantitative yield of barium chlorid be obtained by the reaction of the chlorin gas (either obtained by electrolysis'or otherwise) upon a strong solution of barium sulfid obtained by the reduction in the well known manner of barytes with carbon and subsequent leaching of the furnaced product with Water, but that the employment of this method enables this process to be carried out in conjunction with other profitable processes wherein chlorin gas is obtained as a by-product. Moreover, in addition to obtaining a quantitative yield of barium chlorid, a substantially quantitative yield of sulfur in a finely precipitated condition can be obtained.

In carrying out my invention I preferably proceed as follows:A concentrated solution of barium chlorid is employed, preferably of specific gravity 20 B., the same being maintained at a temperature of about 85 C. The foregoing density'and tempera ture are desirable to preventcrystallization of barium hydroxid Ba(OI-l) such solutioncontaining approximately 178 grams of Bas per liter. Electrolytic chlorin gas is conducted into the solution, while the same is maintained at the aforesaid temperature of approximately 85 C., and at a point a Specification of Letters Patent.

Patented Jan. 4, 1916.

Application filed'May 4, 1915. Serial No. 25,700.

sufficient distance from thebottom of the body of liquid to permitthe precipitated sulfur to settle to the bottom below the depth to which the agitating-effect of the gas 15 liable to exert itsinfluence or effect reaction. The object of this arrangement is to prevent the sulfur liberated by the chlorin gas from coming in contact with an excess of chlorin whereby there would be a possibility of. the formation of small quantities of sulfuric acid. Such acid would obviously instantaneously decompose a corresponding amount of BaS according to the following reaction To prevent the sulfur already formed from being acted upon by the chlorin gas in the aforesaid manner, a perforated false bottom is inserted in the precipitating vessel at a suitable depth below the lower end of the pipe carrying the chlorin. The open ings in this false bottom are inch in diameter there belng 5 or' 6 to the square inch,

this being sufiicient to permit the sulfur to sink through to the bottom of the precipitating vessel. Preferably in a cylindrical tank 9 feet high by 3 feet in diameter containing liquid to a height of approximately '8 feet, a pipe 1 inch in diameter projects into the middle of the tank to a point 1% feet above the false bottom of said tank, the said'false bottom being in turn placed 1 foot above the real bottom. By such arrange nent the agitating action. of-the gas will cause all sulfur as formed to pass through the perforated bottom after which it will not be reacted upon by the free chlorin, since the same will penetrate but little if at all below said bottom, the pressure under which the chlorin is introduced being adjusted to produce thedesired agitatlon.

precipitated sulfur through the said false,

bottom. An exhaustive investigation of the aforesaid process showed that In order to determine to what extent this acid reaction This I (the oxidation of sulfur by chlorin to sul- I furic acid) will take place when the chlorin by being conducted into the bottom of the vessel is given every opportunity to react upon the nascent sulfur, shows that there will be as high as 12% of the total sulfur oxidized to sulfuricacid, whereas by my invention less than. 2% of sulfur was so converted into sulfuric acid. During the first stages of the reaction it will be observed that the sulfur liberated by the chlorin appears to be partly dissolved by the remaining BaS, the-color of the solution being a 'ohlorin ,While the sulfur is precipitated in ever increasing quantity so that when the process is finally completed the color of the liquid loses its yellow tint. almost instantaneously and becomes clear, whereas the precipitated sulfur will then appear of a pale yellow or almost white color.

Having thus described my invention, What I claim and desire to secure by Letters Patent 1s':

1. The process which consists in subjecting a solution of barium sulfid to the action of chlorin gas. conducted into said solution from an external source, then permitting the same to react while constantly removing from the Zone of influence of said chlorin gas, the sulfur resulting from said reaction, a (1 then separately recovering the barium c lorid and sulfur from said mixture.

2. In the process of making barium chlorid and sulfur the steps which consist in conducting chlorin gas into a concentrated solution ofbarium sulfid while maintaining the solution at a temperature sufficiently high to prevent crystallization of the barium hydroxid from said solution.

Signed at New York, countyand State of New York, this first 'day of May, 1915.

EINAR VANG GRANO.