US858295A - Manufacture of soap. - Google Patents

Manufacture of soap. Download PDF

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Publication number
US858295A
US858295A US23108604A US1904231086A US858295A US 858295 A US858295 A US 858295A US 23108604 A US23108604 A US 23108604A US 1904231086 A US1904231086 A US 1904231086A US 858295 A US858295 A US 858295A
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soap
insoluble
lime
carbonate
reaction
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US23108604A
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Peter Krebitz
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D13/00Making of soap or soap solutions in general; Apparatus therefor
    • C11D13/02Boiling soap; Refining
    • C11D13/04Continuous methods therefor

Definitions

  • i soap is then converte a ashior soda soluble soapin, a cheap, efliclenti UNITED STATES;
  • Y hisinvention relates to processes of making soap and consists in a method of making grsoa an-organized succession of steps
  • aninso'luble soap is 2 o first pref aredin'a manner permitting both the pro u tionof an article of great purity I and desirable characteristics and the produ-o-- rtion of a gly cerin solution, or sweet watch, oi goodstrength and (purity; -v
  • the base of the insoluble soa may be lime, strontia, baryta or rinc oxid. ut for the 3Q urpose of simplicity of description, lime will; more particularly referred to hereinafter.
  • Q t In theordinary methods ofmaking insolw ble soapfthe fatty matter is usually: eated' ,with water :and hme or other base ar t the h at maintained at or above the boiling point oFwate'ry-stirrin continuously, until saponi- 'fication is ⁇ comp etedl Aside from the heat and power required in'this operation, the re.-
  • lime soap being usually known as lime roc
  • lime roc In orderto'extract glycerin from it, in case no: large excess of water has been "used, it must be disintegrated, and disintegration is necessary in any event before it :can be efficiently converted into soluble soap.
  • the glycerin forms 'an'undesira bly dilute solution.
  • inso uble soap is obtained which is ;very loose and porous in texture, needing no s ecial disintegration and containing the gycerin as a 'com aratively concentr'ated,
  • cent of glycerin may be'directly-obtained. Both because of the open texture of the soap and because the saponification is *more farreaching and complete than in the stated prior art, the glycerin is 'obtainedin larger qu'antity.- To produce this loose-textured lime or other-soap, the fatis first heated to i v 100 0.
  • cent of carbonate over t he""'theoret1cal method, (the separated calcium" carbonate mounts; the stated sources of'loss are avoid? should not contain more thauOA to 0.6 per' "ed and the added excess is readily regained cent" of soap, aiidthe soda'soap'cobtained 99' inlatei'j operations: As facilitating ,cotuver; 'should'no't contain'mo're than,jat the highest, -.i' I

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)

Description

:- No. 858,295. I
i soap is then converte a ashior soda soluble soapin, a cheap, efliclenti UNITED STATES;
PATENT PETER KREBITZQF emoir, eER Anr."
' MANUFACTURE OF '$OAP-' To all, whom it may concern/. Be it known that I, PETER KREBrrz, a citi- Zenof the Empire of Germany, and residing 'at l\lunich, in the Kingdom of Bavaria and 5 the Empire of Germany, have invented cer- .tain' new: and useful Improvements in the Mauufacture of Soap; and'l do hereby dea -claie the following tobea full, clear, and-exact descri tion of the invention, such as will enable :otl iers skilled in the art to which it I: .appertains to make and use the same.,
" Y hisinvention relates to processes of making soap and consists in a method of making grsoa an-organized succession of steps,
: 5980 separatelyuseful, and as a whole 00-.
. oper'ating tomanufacture soap in a cheap and efiic ent manner; all as more fully hereinafter set forth and claimed. l a
thepresent method aninso'luble soap is 2 o first pref aredin'a manner permitting both the pro u tionof an article of great purity I and desirable characteristics and the produ-o-- rtion of a gly cerin solution, or sweet watch, oi goodstrength and (purity; -v The insoluble into the ordinary/pot:
[and thorough manner.-
I The base of the insoluble soa may be lime, strontia, baryta or rinc oxid. ut for the 3Q urpose of simplicity of description, lime will; more particularly referred to hereinafter. Q t In theordinary methods ofmaking insolw ble soapfthe fatty matter is usually: eated' ,with water :and hme or other base ar t the h at maintained at or above the boiling point oFwate'ry-stirrin continuously, until saponi- 'fication is\comp etedl Aside from the heat and power required in'this operation, the re.-
'fs'ultingv product is of undesirable physical 4o characteristics, being a hard, caked mass,v
the lime soap being usually known as lime roc In orderto'extract glycerin from it, in case no: large excess of water has been "used, it must be disintegrated, and disintegration is necessary in any event before it :can be efficiently converted into soluble soap.
' Using an excess of water, the glycerin forms 'an'undesira bly dilute solution. In the first step of the resent method, on the other .5ojhand,-an inso uble soap is obtained which is ;very loose and porous in texture, needing no s ecial disintegration and containing the gycerin as a 'com aratively concentr'ated,
. readily removed so ution. By proper washing',"-.a sweet water containing 12 to 30 per Specification of Letters Patent. Application filed sweater 2, 1904. Serial No. 231,086.
be -performed'ina discontinued.when.the temperature-mac esf ithe necessary point and the cover of the'ket "8p tle removed to. fruit freeevaporation'and 'conisequent cooling During 'the'T-gradual" 'coo reenter-s e 25,1907.
cent of glycerin may be'directly-obtained. Both because of the open texture of the soap and because the saponification is *more farreaching and complete than in the stated prior art, the glycerin is 'obtainedin larger qu'antity.- To produce this loose-textured lime or other-soap, the fatis first heated to i v 100 0. or thereabout and with-it'is thoroughly mcorporated the necessary amount of lime, or otherbase.v Inthe case of'limeylfl i to 14 ementof the weifilfoi-the fat may be emplo ed "Withjthe-l of-"should -.be em ploye a certain small-amount of water, from?" alf thebulkmffiat' to an qualquantityfi 'This water may 'be'very'advantageously re- 7o placed by dilute glycerin solution, later 0btainedh The. mixture of lime, fatand water:
is heated to the boiling oiiit ofwatei' {to be-- gm the reaction,zand o m li continuously-heated and stirred; as in"the- 7.5
rt: tir "irr tt I ur er' eat ing a p 'e t elo "ratioru' heated kettlebhg: tis
inglwhich ensues, the reaction initiated 111 theeating operation spreads throughout the mass, after a time becoming com lete'.i
With ordin, fats this time'is 'qni'. 110- 1 ten hours; y'addition to the fatiof free fatty acid or resin, the reaction'can be much accelerated, being complete in frofil half-an' heur to an hour Five per cent is a suitable at. q pntity; The insoluble soap soproduced is off yery loose tenturexand "1's readily com r'nlriuted by grinding, crushin%1"and: ofonu All theglycerm of the fat, toget erwit that a of the sweet water, if the latter was em eyed 5 in .saponification', is found in comparatively concentrated form in, the, wetting filmion the surfaces of the granules composing'saidloose textured mesa-and it maybe-readily. 4
more r 5 soluble soap formed is also rendered insoluble more carbonate of soda, fol" the decomposi 8o -thoro'ughly incorporated; Double decomare particularly light'in'colorand possesses;
- d 5 solution;
55 separates below-thesaltlyet 6o several-portions of hot water. As'it carries 65" tors, addition ofa little saltis desirable to Owing to theoben texture otthelime soap so iii-event hydrolysis. -About 2 to 3 percentproduced conversion proceedsmore readily of salt in these wash waters is a desirable and thoroughly than withrthe usualihme quantityw-These wash waters may be-used rock, and owing to its purity a better ade to purify thcurd soap, or they may be em- 5 of soap is produced; For a number 0 rea-' played in dissolving carbonate for decorr'ia' osons,.I preferto use an exce$ of so "um-or posing the lime soap, Or, if desired, the
potassium carbonate-over that'theoretically fatty acidsof the soap' in the second and necessary for the conversion of the lime soap. third washings may be thrown out by the ad With the calculated amount of carbonate, 'dition-of a little acid, such as sulfuric. The. ro owing to the laws of mass-action, conversion salt lye separated from the calcium carbon fizs is never complete and the reaction is very ate may have its excess ofalkaline carbonate slow. And the precipitated carbonate of converted into soap and senarated by treat liIne not only contains anadnnxture of lune ment with a little fatty acid orresin, or'a soapbutinsorne manner a POItIOH'Of the may. be used, after addition of water and .and carried downjzperhaps as a double salt. tionof more limesoap. The same salt. lye These losses aggregate very great'amounts; may be used for anumberof'boils in this sometimes ashigh as to 30 per cent of the .manner, since the separation of 'thefca'lciuin soap:- Further, using the molecular amounts carbonate serves to carry down n iuch'colorf i the lime carbonate is "hard to" wash free of ing-mattei' and other'in purities and thereby 85' soap;'probablyfi'om "the presence of the purilyit. j 1 stated double salts By the use of 2to 6 er In proceeding; according to the foregoing. cent; of carbonate over t he""'theoret1cal method, (the separated calcium" carbonate mounts; the stated sources of'loss are avoid? should not contain more thauOA to 0.6 per' "ed and the added excess is readily regained cent" of soap, aiidthe soda'soap'cobtained 99' inlatei'j operations: As facilitating ,cotuver; 'should'no't contain'mo're than,jat the highest, -.i' I
sloniand separation from'the c'alciulncarbon- 0.02 per cent of calciumcarbonate; ate,.somesaltispreferably used withtheso- I A the 'mauufactnre of ot-ash soap, the
1am rbona e-' The-carbonate maybe di conversion should bfi cal'lleg k g I, o ibctly dissolved in 15 percent salt lye; wh ich ate solution alone, assalt would form soda '95 5 maybe one resulting'from-aprvious'slmllar soap, and the solution'of potashsoap is'sepa-"f', operation; ;The water 'present in this operarated frounthe calciulnfcarbon'ate means 1 v a tion should be two. hr threetimes-the uanof afilterpress, oro'thersuitable'meansi --E tityf'(")fi-soda.w From '5 to 20' r cent 0 salt cess ofcarbonate'inthesolutionisneutralized V .ma bef resent in the soda so ution. by the addition of fatty acidprresinjn the rec l hea ali solution, or salt and soda sol u descri manner. {I tion, is brough;t to a boil and'the lime soap Soaps made by the described-procedure! position takes place and'calc'ium carbonate 'tergent qualities as good as any othensoap i 40 1s precipitated, thespeedof the reactiondefrom Ithe'sarne' fats; in many'icases, being' 105 pendingsomewhat on the state of comrmnue'vn superior in adhesrveness. and scourin tion of he-insoluble soap. During its pro qualities; Their durabihty- .1sj good;@they ress, the said insoluble soa should be eve y bleachi pidlyand they donot becomeiran-ff distributed thro hout: t of mass and the 1 cid and'dark, even-after considerable periods 1 r 5 temperature about d be kept at the boiling oftime. The glycerinisobta nedin-a-eoni [no f point; Care. should be taken that the mass centrat ed state, of good purit and'in large does not become too thick, and retains a ceruantifty' ,From the physica P of; v v tain mbbili'ty- Thiclge maybe preventtlie limesoap', its convers on into so ublesoap fj-f ed by suitable additions 0? salt or strong salt is rapid "and complete; using the described l M method. Ofnissiorr'of the usual rolon'ged- 11'5 Y After the conversion is'com'pletefin the heating and stirringeconolnizes in. abon nd V case-of'sodasdap, thesoluble-soapfis salted fuel and obviates the necess ty ofmuch-costly out by a sufficient additionof' saltr The machinery. The loose textured character bf" curd-soap floats and the carbonate of lime the lime soap, also 1contnbutesto the saving .i power and machinery. loose-porous r29 texture of the insoluble soap-not only-permits perfect extraction of the glycerin in'a'concen trated state but also allows at the same time a veryt-horough elimination ofsoluble iinpu'rities, so that the washed soapis verysuiti25 able for making high gradesolubles oap; The Y absence of-thescimpuritiescontributes mater: rially tot-he success of the subsequentoperaitionsas' does also the'open texture-1 1 Sal-t lye and limecarbonate are'separated in any suitable manner,- as, for instance, by theuse of-'a filterpi'ess or a centrifugal'mw" chine. The carbonate is' thenwashed .with' down with it acertainamount of the excess of soda carbonate used,-extraction of the-ad-' hering soap" easy and complete ithout hydrolysis. Inseeo'nd and third wash wa- Having thus fully 'desciibedmy invention;his I Letters Patent of the United States"i s:
3o progresses, 1
' 40 consists in thoroughly incorporating hot fat 50 amount ofwater containing glycerin, heating i v Be sts 'ai what"*I claim as new and desire torsecurelby 1 ,The process of making an insoluble soap which consists in thoroughly incorporating 5 hot'fat' and -'a suitable base-forminginsoluble :soaps with alimited quantity of water, heating the mixture to start the reaction and in; then'allowing the mixture to standfiand cool Y While said reaction r esses: r .o '2. The process 0 ma 'ng alime' soap whic consists. in thoroughly incorporating hot fat with lime and a limited quantity of water, heating the mixture to start the reaction and in thenallowing the mixture to stand and r 5 cool while said reaction progresses.
3. The process of makin an insoluble soap which consists in thoroug hly incorporating hot fat and a suitable base forming insoluble soaps with a limited uantity of water containing glycerin, heating the mixture to start the reaction, and in then allowing the mixture to stand and cool while said reaction ,pro-
gresscs. I
4. The process of making lime soap which 2 5 consists in thorou hly incorporating 'hot fat with lime and a imitcdquantity of Water containing glycerin, heatin the mixture to start the reaction and in then allowing the mixture to stand and cool while said reaction 5. The process of makin an insoluble soap which consists in thoroug ly incorporating hot'fat containing a free acid with a suitable base forming insoluble soaps and 'a limited amount of water, heating the mixture to start the reaction, and in then allowing the mixture to stand and cool while said reaction progresses. I
6. The process of making lime soap which containin free acid with lime and a limited amount 0 Water, heating the mixture to start the reaction and in then allowing the mixture to stand and cool while said reaction progrosses.
7. The process of making an insoluble soap which consists in thoroughly incorporating hot fat containin a free acid with a suitable base forming insoluble soaps and a limited the mixture to start the reaction, and in then allowing the mixture to stand and cool while said reaction progresses. I v 8. The process of forming lime soap which 5 5 consists in thoroughly incorporating hot fat containing a free acid with lime and a limited amount of water containing glycerin, heating the mixture to start the reaction, and in then allowing the mixture to stand and cool while said reaction progresses.
9 The process of making soap which consists in thoroughly incorporati 1g hot fat with a base forming an insoluble soap and with a limited quantity of water, heating the mixture to start the reaction allowing the mix== ture to stand and cool while the reaction pro-.- 'gresses,= washing it free of glycerin and 1 ble impurities and decomposing b'yrboiling with a lye containing an alkaline carbonate in amount at least 2 per cent in excess of that equiva'lentto said insoluble soap.
' 1-0. I The'process of'making soap which con- H sists in forming a granular insoluble soap ofa suitable base and decomposing said soap by boiling with a lye containing an alkaline carbonate in amount between 2 and 6 per cent in excess of that equivalent to said insoluble soap.
11. The process of making soap which consists in forming a granular insoluble soap of a' suitable base and decomposing said soap by boiling with-a'lye containing sodium car onate in amount between 2 and 6 per cent in excess of that equivalent to said insoluble soap and-also containing a few per cent of salt.
12. The process of making soap which consists in forming an insoluble soap of. a suitable v base and decomposing v said soap by boiling with sodium'carbonate dissolved in a-salt lye resulting from a previous operation-pf the same character, said sodiumcarbonatesbeing" i in amount at least 2 per cent miexcess of that" equivalent to said insoluble soap.-
13. The process of making and recovering soap of a suitable base 'decom osing said soap by boiling with a lye contaim iigan alkaline carbonate in amount between 2-and-6 per cent in excess of that e uiva'lent to saidinsoluble soap, separatingt e insoluble'can' bonate formed and washing the same with hot water to remove and receverco-precipi tated alkaline carbonate and soap; .fi 1;
14. The process ofmaking soap which cona lye containing sodium oar mate in amount sists in forming an insoluble soap ofa suitable" 1 base, decomposing said soa by boiling with between 2 and .6 er cent in excess bf that equivalent to said msoluble'soap; adding salt in saltmg-out amount after completio'nof the decomposition, and separating the curd soap and insoluble carbonate formed.
15. The process of makin soap which con-' sists in forming lime soa ecomposing said lime soap by boiling wit sodium carbonate dissolved in diluted salt lye resulting from a revious similar operation said carbonate sing in amount at least 2 er centin excess of that e uivalent to said ime soap, adding salt insa ting out amount after. completion of the decomposition and separating the curd soap and insoluble calcium carbonate formed.
16. The process of 'making soap which con- I sists in forming lime soap by thoroughly incorporating hot fat, lime and a limited quantity of water, heating to start 'the'reaction and allowingto. stand'and cool while said re- V 95. soap which consists informing-an insoluble action progresses, washing theso-formedlime and separating the 'eurd soap and insoluble soa free of glycerin and soluble impurities ca cium carbonate formed. p p "10 with hot water, decomposing said purified, testimony whereof I hereunto aflix' my lime soap by boiling vdth a saltlye contain signature in the presence of two witnesses; ing sodium oarbonatein amount at least 2 PETER KREBITZ.
er cent in excess of that equivalent to aid Witnesses; v v i me soap, a'ddin salt in salting out proportlons after compfetion of the decomposition,
. ULYSSES J; BYWATER, ABRAHAM ScnLEsmGER;
US23108604A 1904-11-02 1904-11-02 Manufacture of soap. Expired - Lifetime US858295A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3051571A (en) * 1959-02-10 1962-08-28 Marcus N Pergament Process of making a stock feed additive
US4826694A (en) * 1985-10-14 1989-05-02 Balfour Manufacturing Company Ruminant feedstuffs, their production and apparatus for use therein
DE112008002315T5 (en) 2007-08-31 2010-12-02 JH Biotech, Inc., Ventura Production of fatty acids in solid form

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3051571A (en) * 1959-02-10 1962-08-28 Marcus N Pergament Process of making a stock feed additive
US4826694A (en) * 1985-10-14 1989-05-02 Balfour Manufacturing Company Ruminant feedstuffs, their production and apparatus for use therein
DE112008002315T5 (en) 2007-08-31 2010-12-02 JH Biotech, Inc., Ventura Production of fatty acids in solid form

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