USRE13234E - Samuel henry fleming - Google Patents

Description

UNITED STATES PATENT OFFICE.

SAflUEL HENRY, FLEMING, OF CAMDEN, NEW JERSEY, ASSIGNOB T'O E. I. DUPONT DI NEMO'UZRS IOWIDEZB' CONTPANY, OF WILMINGTON, DELAWARE, A CORPORATION OF New JERSEY.

mn'rnon or riuaa'r ino GLYCERIN.

Specification o1 Reissued Letters Patent. Reiggud May 9, 1911.

110, Drawing. Original No. 969,159, dated Septeinber 6, 1810, Serial No. 498,749. Application for reissue filed December 20, 1910. Serial No. 598,482.

To all whom it may concern: v Be it known that I, SAMUEL HENRY FLEMING, a citizen ofthe United States, residing at Camden, county of Camden, and State of New Jersey, have invented a new and" useful Improvement in Methods of Treating Glycerin, of which the following is a full, clear; and exact description.

Polymerized glycerin or poly-glycerin is a term used for a glycerin in which, as is generally supposed, two. or more of the glycerin molecules are combined together.

There are several ways in which this is produced atthe present time; thus it has been produced by heating alone, which is very slow and not effectiveand produces a product which is quite impure. 'In order to accelerate the reaction, certain alkalis have 1 been used, among which caustic soda,

NaOH, is the most prominent. The use of caustic soda, while it accelerates the reaction, has a tendency to produce by-products, Q which are deleterious to the glycerin. I,-

have carried on a line of work with respect to this so-called polymerized glycerin or poly-glycerin a'nd'I am led "to believe that there is not only a union of the molecules of the glycerin but also that a certain propor- I tion of the water of the combining molecules is driven ofi, thus producing a condensation product of glycerin.

The glycerin treated as before described has certain advantages in that it may be used in the manufacture of nitroglycerin compounds for explosives which will have a lower freezing point than 'where nitroglycerin made from (glycerin not so treated 1s used. Iam also le tests, that nitro-glycerin made from glycerin so treated is less liable to decompose than-is nitro-glycerin made from glycerin' not so treated. .In working on this-line I have discovered that if instead of. using an alkali, I use an acetate which may be any of the acetates, preferablyn odium ace-. tate, NaC H,,O,, but otherwise treated as" before described, the 'productwill be produced with much less decom 'sition of the glycerin than occurs where a kalis are used. Preferably, I addthe acetate in quantity of one-half to one per cent. of the weight of the glycerin. This mixture is subjected to a temperature of 275 to 280 centigrade.

to-belie've, from many The water which separates in the reaction is distilled ofi, leaving a mixture of this glycerin, which isgenerally known as polymerized glycerin or polyglycerin, and

sodium acetate in which about. seventy per cent. of the glycerin is so-called polymerized. The detailed statement ,of the process and the rationale of the same are as follows:

The glycerin used is what is known as dy-' namite glycerin, which is a highly purified glycerin containing 98 to 99% glycerin. The reaction .according to which glycerin is condensed to diglycerin is as follows:

3 5 s 2 s s) 2 4 I Triglycerin is formed as follows I a 5 3 s 2 5 011,011 't'Hon been 1H,

time I omen k ln,

" on 42H, 2111011 trno'nfl tn, om n t f 1 a 1511-. AJELOH ()HOH cal - tion as here used will be found defined on page 578 of Arbeitsmethoden fair, Organz'sch Uhemz'sche Laboratorz'en, Lassar- Cohn, 3rd edition, 1903.

that converted goes to the form of diglycerin and only a small percentage to triglycerin. Probably no more than traces pass into tetragly'cerin, and the higher products, if, in fact, any at all sufl'ers this change.

Adherence to the following directions will enable any one to carry out my process: A suitable vessel of glass, metal or.ot-her material which will stand the working temperature is "selected, with an outlet sufficient in size to permit of the ready exit of the'water vapors formed, and the small amount of glycerin which accompanies them. This giycerin is of a quality suitable for the man. u acture of ordinary nitroglycerin. --The glycerin is weighed and from this weight,- the proper amount of anhydrous sodium acetate is computed and added, although it is possible to obtain results withthe crystallized salt. 1' Of course, it is immaterial whethermixture of glycerin, and sodium acetate is efi'ected in or outside of the heating vessel. The contents of the vessel are now raised to a boiling temperature, which increases a little as the reaction progresses, the average being in the neighborhood of 280 C. The heating is continued for a suitable length of time. After about an hour, the product will contain about 70% of polymerized glycerin if 1% sodium acetate has been used.

Havin now fully described my invention, what I c aim and desire to protect by Let ters Patent is: i

1. The hereinbefore described method of treating concentrated glycerin, which consists in mixing with the glycerin an acetate;

and subjecting the mixture to heat.

2. The herembefore described method of treating glycerin, whichconsists in mixing with the glycerin-an acetate and subjecting the mixture to a heat of approximately its As a matter of fact, when glycerin is'polymerized by the method at present known, practically all of sists in mixing with the glycerin an acetate,

e hereinbefore' described method of treating concentrated glycerin, which con sists in mixing with the glycerin an acetate and subjecting the mixture to a heat of approximately its boiling point.

4. The hereinbefore described method of treating concentrated glycerin, which consists in mixing with the glycerin an acetate, and subjecting the mixture to heat, the acetate being in quantity from one half to one per cent. of the weight of the glycerin.

5.- The hereinbefore describedmethod of treating glycerin, which consists in mixing with the glycerin an acetate, and subjecting the mixture to a heat of approximately its boiling point, the acetate being in quantity from one-half to one per cent. of the weight of the glycerin. Y

6. The hereinbefore described method of treating concentrated glycerin, which conand subjecting the mixture to a heat of approximately its boiling point, the acetate being in quantity from one half to one per cent. of the weight of the glycerin."

7. The hereinbeforefldescribed method of treating glycerin, which consists in mixing with the glycerin sodium acetate, and sub jecting the mixture to heat. I

8. The hereinbefore described method of treating glycerin, which consists in .mixing with the glycerin sodium acetate, and subjecting the mixture to heat, the sodium acetate being in quantity from one half to one per cent. of the weight of the glycerin.

9. The hereinbefore described method of 95 treating concentrated glycerin, which consists in mixing with the glycerin sodium acetate, and subjecting the mlxture to heat.

10. The hereinbefore described method of .treating glycerin, which consists in mixing with the glycerin sodium acetate and subjecting the mixture to a heat 01% approxi-- mately its boilin point.

11. The hereinieforedescribed method of treating concentrated glycerin, which consists in mixing with the glycerin sodium aceta'te, and subjecting the mixture to a heat of approximately its boiling point.

12. The hereinbefore described method of treating concentrated glycerin, which consists in mixing with the g ycerin sodium acetate, and subjecting the mixture to heat, the sodium acetate being in quantity from onehalf to one per cent. of the weight of the glycerin.

, 11 5 13. The hereinbefore described method of treatin l cerin which consists'in mixing g g f with the g ycerin sodium acetate and 'sub jecting the mixture to aheat oi approximately its boiling point, thesodium acetate being in quantit from cue-half to one per dinm acetate being in quantity from one-- cent. of the weig t of the glycerin. half to one per cent. of the weight of the 14. The hereinbefore described method of glycerin; v treating concentrated glycerin, which con- SAMUEL HENRY FLEMING. v 5 sists in mixing with the glycerin sodium Witnesses:

acetate, and subjecting the mixture to a. heat R. H. HARVEY,

of approximately its boiling point the so- M. B. GREENE.