USRE3E - Improved manufacture of coloring-matter - Google Patents

Description

' UNITED STATES PATENT '.OEFICE,

HENRYl STEPHENS, sfr,- .inRYLEBONE ENGLAND.

llvpn'ovso MANU'FAci-unef oF coLomNe-MATTER;

Specification forming part of Letters Patent No,

. -W i'lpril21, 1838.`

1b all whom it may concern:

.Befit known lthat I, HENRY STEPHENS, ra subject of the- Queen of Great Britain, and now residing in Charlotte Street, -in the parish of Saint Marylebone and county of Middlesex, in the said Kingdom, have invented 'or discovered a new and'useful invention of certain improvements in manufacturing coloringmatter and renderingl certain color or colors more applicable to dyeing, staining, and writing; and I do hereby declare that the following is a full and 'exact description thereof.

My improvements 'in .manufacturing color-4 ing-matter;- and rendering certain color orcolors more n applicable to`Y dyeing, staining, and writing, consist; inthe first place, of -improvements; in making or manufacturing the ferro-prossiates, (that is, prussiates of potash .and soda,) and, secondly, .in rendering Prussian blue soluble, and thereby more applicable than heretofore to the purposes of dyeing, staining, coloring, ,and writing, which iu 1- provements I ain-now aboutto describe under different heads or Vsections-that is to say.:

My first improvement consists in convert. ing certain gaseous products arising fromthe present mode of ,making prussiate of` potash or soda from animal matter (which are now commonlyallowed to escape into the atmos# i phere) tothe purpose of.` making prussiate of; potash or soda,

so that an increased quantity .of prussiate of potash or soda may be obtained 1 intoprussiate. Y a is an iron pot, vessel, or ref from a given quantityA of animal matter.

Forthe better explanation of this part of myinvention, I referto the annexed drawings,

v Fi' 1 represents an apparatus for effecting e process of converting the gas evolved tort eh g with alkali and animal or other mattercoutaini'ng azote, or yielding ammonia,

' which vessel is tofbejheated toa low red heat.

This pot or ,vf has a movable cover, which isASo be luted on when"under, operation, buty i may beremOved andv placed upon another 1 b bygdisconnecting the.: joijnt n theipe e joint' allowing the ofthe pot'ln to carried round with the `,connecting-pipe c. The pipe c is for conducting 'the gaseous pro- -duets arising fromv the decomposition of the said.v animal'matterin the potslaor'b into an ironcyludrical or other conveniently-shaped 441, datedlOctober 28, 1837; Reissuedo. 8, dated as a gage-cock to ascertain the state of the gas' within. 'a' t' are furnaces under the pots a and by the connecting-pipe c to the cylinder d,

, where, meeting with the alkali in a state Vof fusion, the veffect will be that the gas becomes and forms prussiate of potash or soda; but

'do not combine or oommix with the alkali, these will pass oiA by the pipe c to the closed vessel f, and if any of the gas thus passed 011' shouldbecapable of combining with the alkawith the alkaline solution is allowed to pass off by the gas-jet pipe g. lThe stateofop'era- 'tion may be ascertained by burning-'the -j,etv gas from'the endv of this' pipe, for. when it ceases to burn freely the connection between fed,and the head and pipe c be removed rou-nd and lute'd onto`v the viouslycharge'd .wit j animal matter and 'alkali, the distillation of which will IIed as before described. When'thegaseousproducts of sev eral charges have beenpassed through the cylinder d ycontaining the alkali,fthe cylinder may be opened and the charge (whichlwill now consist of crude prussiate of potas or soda, or metal, as it is commonly called lnthetrade) bewithdrawn into an iron vessehandwhen cold belixiviated in cold wateriu the usual manner. The further decomposition of the charge of animal matter in the pot'a mayv now be consiate in the open vessel byincreasing the heat, the content-sI being agitated, as usual. This pots a. and b, the completion of thedecompo-l sition ofthe charge of one being effected, while that of theV other issubjected to the lower heat -and the ,operation of distilling off its vapors and passing it ,to the retort or vessel c. A'

vessel, d, heated by a'furnace, h, below. This pipe or burner, g, which is merely intended b. The gas generatedl in the retort a passes.

combined t o a certain degree with the alkali,

there may be portions ofthe said gas which line solutionfit nay do so in the closed: vessel f f, and that portion which does not combine the'pot a and cylinder d shouldbedisconnectf "got'b, .whichis to be preducted in the ordinary manner ofmaking 1.1-

process may be repeated alternately in the two similar effect--viaL,thatA of taking up the gaseous products, so as to produce an additional quantity of crude prussiate of potash or metn al-may be obtained in an open conical chimney having a false bottom or grating or perforated plate, upon which dry "potash or soda isplaced, so that the gas generated in the pot below may pass through the stratum of alkali in the chimney.

Fig. 2 is a sectional elevation representing this application of my improvement. E is the chimney or open cone usually placed o'n the top of an ordinary pot, F, for making prussiate of potash, in order to convey the flame upward. G is a grating or perforated plate placed at the base of the cone E. -Upon this grating or perforated plate G a stratum of dry potash or soda is laid, and as the gas passes `upward through this stratum a portion of it will become combined with the alkali. The chimney, with the stratum of alkali, may bel removed when the llame begins to burn weak, and it maybe set aside and applied to future charges, or put into the pot and worked off .with the charge in the usual manner of making prussiate of potash -or soda. 'Y

. Mysecond improvement-wiz., the mode, method, or process of treating or operating upon Prussian blue so as to render it more perfectly soluble or more readily disposed to be acted upon 'by the subsequent process of solution than when manufactured in the usual way, and in order' that the same may be more applicable to the purposes of dyeing, staining, coloring, and writing-I effect in the following manner: I take the Prussian blue, whetherproduced from a combination of prussiate of potash and salts of iron or the Prussian blue of commerce as commonly manufactured, and I put this `into an earthen vessel, and pour over it a quantity of stronglyconcentrated aeid,suf cient to cover the Prussian blue. Muriatic acid, sulphuric acid, or any other acid which has a sufficient action upon iron will do; but

I prefer the muriatic acid. If sulphurie acid is used, it should be diluted a little-that is, with a quantity of water equal to about its bulk at the time when themass turns white after the Prussian blue is put in. The Prussian blue is to be allowed to remain in the acid from twenty-four to forty-eight hours, or longer. I then dilutethis mixture with a large quantity of water, stirring it'up at the time, for the purpose of washing from it the salts of iron. When in this state of dilution, I suffer it to stand until the color has subsided, when the supernatant liquor is to be drawn off with a Siphon and more water added to it; and I continue the repetition of this process until I judge that the acid with the iron has been completely washed away, and this is known by testing it with prussiate of potash, which will show if it yields any blue precipitate; if not, it is sufficiently washed. I then place it upon a filter and suii'er it to -remain until the liquid has all drained away.

The Prussian blue thus prepared is reduced to a stateas I conceive, containing less iron than the Prussian blue of commerce, in which state it is more readily acted upon and rendered soluble than in any other condition. This Prussian blue may, be then placed in evaporatingdishes and gently dried. To form the Prussian blue so operated upon into a solution I add to it oXalie acid, and mix them carefully together, after which I add cold water, (cold distilled water is best,) a little at a time, making it into a dense or dilute solution, according to the color required. The quantity of oxalio acid may vary according to the quantity of water used. It will be found that the Prussian blue that has undergone the process of digestion as described requires but a small quantity of oxalie acid to dissolve it. About one part of oxalic acid will dissolve six parts of VPrussian blue, (the weight taken before digesting in the acid.)` This will answer for a concentrated solution; but for a dilute solution more acid will be required. Prussian blue that has not undergone digestion in acid in the way above pointed out will require a much larger proportion of oxalie acid, from twice to three times iis weight, and even then it will be greatly liable to precipitation after standing; but when treated in the way described it is not liable to precipitate, but remains a permanent solution.

The chief obstacle to the general employment of the beautiful color obtained by means of the ferro-prussiates to the purposes of dyeing in the silk, cotton, linen, or woolen manufactures, and also to the purposes of staiir ing and writing, hasv been its hitherto supposedinsoluble nature; but by means of oxalic acid (whether obtained by the usual process of mixing or'distilling saeeharine matter in combination with nitric acid or from vegetable or other substances containing oxalic acid or from combinations of oxalates, whether metallic,f earthy, or alkaline)l I obtain the above perfect solution of the Prussian blue, which is applicable to dyeing, coloring, or staining in the various manufactures of woolens, Silks, linen, cotton, paper, and such other substances as are required to be dyed or stained, and which solution is also available to the purposes of writing or forming a writing iluid or ink to be4 used with steel, quill, or other pens.

In conclusion, I desire to be understood that I do not claim any of the apparatus or machinery described, nor the caleination of animal matters in close vessels; but

I do claim-d 1. The method of obtaining a product ol' prussiate of potash or soda from the gases evolved from the distillation of animal matters or any other matters that yield azote and carbureted hydrogen-such, for instance, as

coal'-by means of passing those gases direct into a mass of alkali in a state of ignition and into a solution of alkali contained in separate vessels, either closely or distantly connected with the distillatory apparatus.

2. Ido not claim the` use of acids for iluA purpose of brightening orimpl'oving the eolr of Prussian blue in the ordinary manner, but I do claim the use of strong acids for the purpose of digestin dry Prussian blue of oommeree in order to render it more easily soluble in the oxalio acid than it would be without such digestion.

3. The useof oxalio acid, however obtained, as a solvent for Prussian blue generally, but

more especially as a final prooess for a perfect solution of the Prussian' blue which has been prepared and digested in the manner aboveo In Vilma; vhereof Lum mia Srnrms, have hereunto set my hand 'and seal this 28th day of October, in the year of o'ur Lord 1837. Y

HENRY s'lEPlcE'Ns. [n s] Witnees: a MILBBENY, A Oeo for Patents, 66 Chancery Lane.

J. W. MoFFn'r,

(Herk to the above.

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