US1007680A - Process of making soap powder. - Google Patents
Process of making soap powder. Download PDFInfo
- Publication number
- US1007680A US1007680A US53123609A US1909531236A US1007680A US 1007680 A US1007680 A US 1007680A US 53123609 A US53123609 A US 53123609A US 1909531236 A US1909531236 A US 1909531236A US 1007680 A US1007680 A US 1007680A
- Authority
- US
- United States
- Prior art keywords
- soap
- alkali
- pounds
- cocoanut oil
- glycerin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000000344 soap Substances 0.000 title description 32
- 238000000034 method Methods 0.000 title description 12
- 239000000843 powder Substances 0.000 title description 12
- 239000003921 oil Substances 0.000 description 17
- 235000019198 oils Nutrition 0.000 description 17
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 16
- 235000013162 Cocos nucifera Nutrition 0.000 description 15
- 244000060011 Cocos nucifera Species 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000003513 alkali Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- 235000014113 dietary fatty acids Nutrition 0.000 description 10
- 239000000194 fatty acid Substances 0.000 description 10
- 229930195729 fatty acid Natural products 0.000 description 10
- 150000004665 fatty acids Chemical class 0.000 description 10
- 235000011187 glycerol Nutrition 0.000 description 8
- 238000007127 saponification reaction Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- 230000001427 coherent effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229940072033 potash Drugs 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000003925 fat Substances 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 235000015320 potassium carbonate Nutrition 0.000 description 3
- 235000011118 potassium hydroxide Nutrition 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000010009 beating Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 235000012343 cottonseed oil Nutrition 0.000 description 2
- 239000002385 cottonseed oil Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000021588 free fatty acids Nutrition 0.000 description 2
- 230000035876 healing Effects 0.000 description 2
- 238000005185 salting out Methods 0.000 description 2
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 description 2
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 1
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 1
- WEEGYLXZBRQIMU-UHFFFAOYSA-N 1,8-cineole Natural products C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 description 1
- 241000723346 Cinnamomum camphora Species 0.000 description 1
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 1
- WEEGYLXZBRQIMU-WAAGHKOSSA-N Eucalyptol Chemical compound C1C[C@H]2CC[C@]1(C)OC2(C)C WEEGYLXZBRQIMU-WAAGHKOSSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000005844 Thymol Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 235000013871 bee wax Nutrition 0.000 description 1
- 239000012166 beeswax Substances 0.000 description 1
- 229960000846 camphor Drugs 0.000 description 1
- 229930008380 camphor Natural products 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 229960005233 cineole Drugs 0.000 description 1
- 230000000249 desinfective effect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000000266 injurious effect Effects 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- 229940041616 menthol Drugs 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 210000004761 scalp Anatomy 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 239000012177 spermaceti Substances 0.000 description 1
- 229940084106 spermaceti Drugs 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 229960000790 thymol Drugs 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S159/00—Concentrating evaporators
- Y10S159/14—Soap
Definitions
- soap powders containing 3% to 6% of glycerin and 15% to 10% of 'dry readily an otash may be made so as to (I produce a satisfactory pulverulent powder free from caking action.
- the stock be light colored in order that the resultant powder may be white or nearly so.
- the use of low grade greases and fats in any large quantity is proscribed, Ordinarily, I prefer to use a considerable quantity of free Specification of Letters Patent. I 4 Patented Nov, 7, 1911. Application filed December 3, 1909. Serial No. 531,236.
- fatty acid in the manufacture of these products and preferably employ the fatty acids derived from cocoanut oil or similar stearic acid, the commercial double pressed' variety which is sufficiently white for thespecific purposes herein mentioned.
- Fatty acids such as red oil or commercial oleic oming to their dark color are not so desira c. with considerable difliculty so that they are not generally available for this purpose.
- the fatty acids obtained by distillation of the fatty acids from cottonseed oil produce a fairly white product although the soaps made therefrom are'not as dry and pulverulent as those from cocoanut oil and stearic acid but are more inclined to be slightly sticky or gummy.
- glycerin In a soap materially intended for use on the person, a moderate amount of glycerin is desirable owing to its healing act-ion and to the tonic effect which it produces on the skin. Cocoanut oil also is believed to have certain healing and medicinal properties and this together with its free lathering powers, makesit a very desirable ingredient in the present composition.
- Cocoanut oil is saponified with approximately twice the amount of alkali required for its complete saponification, using perhaps an equal These acids moreover. are bleached"- out in the usual manner,-
- This I accomplish in amount to twice the amount of water reckoned on the cocoanut oil employed.
- cocoanut oil equal in weight to that of the cocoanut oil originally used, is added to the mixture and rapidl agitated with heating until the excess 0 alkali is substantially neutralized. Then, the mass is subjected to powerful agitation usinguse of an excess of water, the frame should be cooled in some manner as for example, by means of a jacket containing cold water. As otherwise, in so fluent a condition, the soapy material might contract and lose more or less of its porosity. When the same has hardened, it may be run through a slicing apparatus and then passed into a drying oven. This preferably should be heated only to 60 or 80 C.
- waxy material In order to enhance the beneficial effect of gylcerin, it is sometimes desirable especially in shaving soaps to add a small quantitysay from 2 to 5% of waxy material.
- This for example may be bleached beeswax, spermaceti, paraffin wax and the like. It preferably should be added to the fatty acids which are added to the strongly alkaline soap during the stage of-neutralization.
- An illustrative formula under the present invention is made by saponifying 10 pounds of cocoanut oil with 2? ⁇ pounds of caustic soda and 11 ⁇ pounds of caustic potash, using about two gallons of water for solution of the alkali in its reaction on the cocoanut oil.
- This may be boiled down in a steam jacketed -potash 2 pounds, cotton seed oil fatty acid 10 pounds, all combined as above set forth.
- carbonate of soda or potash may displace in whole or in part the caustic alkali used although it is better for the saponification of the cocoanut oil to use the canstic alkali, using a small excess of this and introducing the remainder of the alkali in the form of carbonate if desired.
- Another formula consists of cocoanut oil 10 pounds, caustic soda 3 pounds, caustic potash 1 pound, stearic acid 8 pounds, still stock 2 pounds.
- the alkali preferably employed is a mixture of soda and potash while in the following intended more for use as a shampoo powder, caustic soda is used as the sole alkali.
- the formula is cocoanut oil 10 pounds, caustic soda i pounds, red oil 5 pounds, still stock 5 pounds. These materials are incorporated as above indicated and when reduced to a powder, a pound of pine tar is added and worked into the powdered material, when the mixture may be reground if desired. Powdered camphor, menthol and thymol may be added to such a mixture in order to suitably medicate it.
- These powders may be combined if desired with suitable filling materials such as talc or ground soap stone or light colored infusorial earth.
- peroxids, perborates and the like may be introduced, provided they are not materially incompatible with the other bodies employed, or by virtue of any internal reactions deteriorate the materials on keeping.
- the perborates are especially useful for giving to shaving soap powders desirable hygienic properties.
- other antiseptic materials may be added in small quantities such for example, as carbolic acid, eucalyptol and the like.
- alkali comprislng caustic soda and caustic potash
- said alkali comprislng caustic soda and caustic potash
- easily soluble non-coherent soap powder which consists in saponifying a quantity of a glycer-id with a quantity of alkali substantially more than sufiicient to neutralize -the fatty acids of said.
- glycerid in thereupon adding sufiicient freefatty acid to neutralize the excess of alkali and in beating and agitating the mass whilein a plastic condition to substantially increase its volume and convert it into a vesicular condition In witness whereof I have afiixed my signature in presence of two witnesses.
Description
j I TA E NT OFFICE;
CARLETON or MONTCLAIR, N JERSEY, ASSIGNOB 'ro ntms-ros'rnn coni-- run, a CORPORATION or NEW JERSEY.
PROCESS OF MAKING SOAP POWDER.
nooflcso. No Drawing.
To all whom it may concern Be 'it known thatI, CARLnroN ELLIs, a citizen of the United States, residing at Montclair, in the county of Essex and State of New Jersey, have invented certain new and useful Improvements in Processes of Making Soap Powder, of which the following is a specification.
, ciently free lathering to have marked detergent action and without injurious effect on the hair or scalp. r
If ordinary soap is dried, it will be found that it has a tendency as a rule on standing in the container to form coherent masses.
Furthermore, owing to its density, it is not freely soluble and does" not immediately produce a free lather. Soaps which contain glycerin or potash are particularly dilficult to dry owing to their hygroscopic properties. In the endeavor to dry such soaps, high temperatures have been employed with the result that often" times the fat or the jglycerin is decomposed into products having disagreeable odor and with more or less discoloration of the soap. Even the UStL of vacuum pans does not readily overcome the difiiculty.
Under the present invention, soap powders containing 3% to 6% of glycerin and 15% to 10% of 'dry readily an otash may be made so as to (I produce a satisfactory pulverulent powder free from caking action. In the selectionof the materials to be used under this process, and forthe purposes herein specifically mentioned, it is desirable that the stock be light colored in order that the resultant powder may be white or nearly so. For this reason, the use of low grade greases and fats in any large quantity is proscribed, Ordinarily, I prefer to use a considerable quantity of free Specification of Letters Patent. I 4 Patented Nov, 7, 1911. Application filed December 3, 1909. Serial No. 531,236. I
fatty acid in the manufacture of these products and preferably employ the fatty acids derived from cocoanut oil or similar stearic acid, the commercial double pressed' variety which is sufficiently white for thespecific purposes herein mentioned. Fatty acids such as red oil or commercial oleic oming to their dark color are not so desira c. with considerable difliculty so that they are not generally available for this purpose. The fatty acids obtained by distillation of the fatty acids from cottonseed oil produce a fairly white product although the soaps made therefrom are'not as dry and pulverulent as those from cocoanut oil and stearic acid but are more inclined to be slightly sticky or gummy.
In a soap materially intended for use on the person, a moderate amount of glycerin is desirable owing to its healing act-ion and to the tonic effect which it produces on the skin. Cocoanut oil also is believed to have certain healing and medicinal properties and this together with its free lathering powers, makesit a very desirable ingredient in the present composition. In the saponification of cocoanutoil, some 10% or 12% of glycerin is produced and inasmuch as it is not ordinarily feasible to remove this-glycerin by salting ow,ing to the act that during the process of salting out, some changes apparently take placein the character of the material which may be due in a measure to the pres ence of some absorbed salts, etc., it is desirable that saponification be so conducted that the salting out process is eliminated and the glycerin retained in the mixture. However, as a proportion of 10 or 12% of glycerin in. the product is not desirable it having been found that 4 to 6% glycerin is sufiicient' for the purposes hereinbefore mentionedmeans must be taken to reduce the content of glycerin to approximately 'the lesser amount. the following manner: Cocoanut oil is saponified with approximately twice the amount of alkali required for its complete saponification, using perhaps an equal These acids moreover. are bleached"- out in the usual manner,-
This I accomplish in amount to twice the amount of water reckoned on the cocoanut oil employed. When .tainedfrom cocoanut oil equal in weight to that of the cocoanut oil originally used, is added to the mixture and rapidl agitated with heating until the excess 0 alkali is substantially neutralized. Then, the mass is subjected to powerful agitation usinguse of an excess of water, the frame should be cooled in some manner as for example, by means of a jacket containing cold water. As otherwise, in so fluent a condition, the soapy material might contract and lose more or less of its porosity. When the same has hardened, it may be run through a slicing apparatus and then passed into a drying oven. This preferably should be heated only to 60 or 80 C. as a much higher temperature tends to decompose the fatty material to some extent. Owing to the extremely porous character of the material, the water departs very rapidly and a soap which in the non-vesiculated condition might require several days exposure to this temperature to properly effect the drying, is dried in" the course of a few hours when in aforesaid porous state.
In the manufacture of cocoanut oil soaps,
a great difficulty has heretofore been experienced in the production of a soap which does not rancidify in the course of time.
Apparently, this is in a large measure due to the difiiculty of complete saponification of the fat resulting in the presence in the finished soap of a small quantity of unsaponi fied material which eventually becomes rancid. By the present process, saponification of the cocoanut oil with a large excess of alkali overcomes this difficulty and a soap is produced which remains free from rancidity for an indefinite time.
In order to enhance the beneficent effect of gylcerin, it is sometimes desirable especially in shaving soaps to add a small quantitysay from 2 to 5% of waxy material. This for example may be bleached beeswax, spermaceti, paraffin wax and the like. It preferably should be added to the fatty acids which are added to the strongly alkaline soap during the stage of-neutralization.
An illustrative formula under the present invention is made by saponifying 10 pounds of cocoanut oil with 2?} pounds of caustic soda and 11} pounds of caustic potash, using about two gallons of water for solution of the alkali in its reaction on the cocoanut oil.
This may be boiled down in a steam jacketed -potash 2 pounds, cotton seed oil fatty acid 10 pounds, all combined as above set forth. Of course, carbonate of soda or potash may displace in whole or in part the caustic alkali used although it is better for the saponification of the cocoanut oil to use the canstic alkali, using a small excess of this and introducing the remainder of the alkali in the form of carbonate if desired. Another formula consists of cocoanut oil 10 pounds, caustic soda 3 pounds, caustic potash 1 pound, stearic acid 8 pounds, still stock 2 pounds.
In the above formulas, the alkali preferably employed is a mixture of soda and potash while in the following intended more for use as a shampoo powder, caustic soda is used as the sole alkali. The formula is cocoanut oil 10 pounds, caustic soda i pounds, red oil 5 pounds, still stock 5 pounds. These materials are incorporated as above indicated and when reduced to a powder, a pound of pine tar is added and worked into the powdered material, when the mixture may be reground if desired. Powdered camphor, menthol and thymol may be added to such a mixture in order to suitably medicate it. These powders may be combined if desired with suitable filling materials such as talc or ground soap stone or light colored infusorial earth.
To give a saponifying or disinfecting effect, peroxids, perborates and the like may be introduced, provided they are not materially incompatible with the other bodies employed, or by virtue of any internal reactions deteriorate the materials on keeping. The perborates are especially useful for giving to shaving soap powders desirable hygienic properties. Of course, other antiseptic materials may be added in small quantities such for example, as carbolic acid, eucalyptol and the like.
While it has heretofore been customary to pass soap materials in the process of manufacture through crutching devices, more particularly for the purpose of making a uniform mixture and for working the perfumed materials well into the soap, and also for reducing the specific gravity of the soap in those applications where the soap is de sired to be somewhat lighter in water, there has been, so far as I am advised, no application of the process of heavily crutching or beating a fluent or plastic soap mass to incorporate into the soap a very substantial amount of air globules so as to render the soap extremely light and porous and by such an operation to substantially double its volume; or for the purpose of rendering the soap highly porous so that it may be readily ground and so that the ground particles owing to their substantially vesicular character exist not as dense pellets but as flakes or vesicules soluble in water with great ease.
While I do not wish to limit myself in the process herein described to the step of crutching to a volume substantially double that of theoriginal soap mass or in'other words introducing into the mass a volume v of air substantially equal to that of the soap mass itself, yet I have found that employing these proportions, a product is obtained which is very readily handled and I prefer to conduct the operation substantially in this manner.
What I claim is:-
1. The process of making a free lathering,
easily soluble non-coherent soap pow.der,.
which consists in saponifying a glycerid of fatty acid with substantially twice the amount of alkalirequired to neutralize the fatty acid in said glycerid, in adding after complete saponification, a quantity of free fatty acid suflicient to neutralize the excess of alkali and in crutching the material to a highly vesicular condition and in drying and grinding the resulting product;
3. The process of making a free lathering, easily soluble non-coherent soap powder which consists in saponify'ing cocoanut oil.
with twice the amount of alkali required for its ,saponification, said alkali comprislng caustic soda and caustic potash, in adding easily soluble non-coherent soap powder which consists in saponifying a quantity of a glycer-id with a quantity of alkali substantially more than sufiicient to neutralize -the fatty acids of said. glycerid, in thereupon adding sufiicient freefatty acid to neutralize the excess of alkali and in beating and agitating the mass whilein a plastic condition to substantially increase its volume and convert it into a vesicular condition In witness whereof I have afiixed my signature in presence of two witnesses.
CARLETON ELLIS. Witnesses:
NATHANIEL L. FOSTER, JAMES T. ERNOTT.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US53123609A US1007680A (en) | 1909-12-03 | 1909-12-03 | Process of making soap powder. |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US53123609A US1007680A (en) | 1909-12-03 | 1909-12-03 | Process of making soap powder. |
Publications (1)
Publication Number | Publication Date |
---|---|
US1007680A true US1007680A (en) | 1911-11-07 |
Family
ID=3075992
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US53123609A Expired - Lifetime US1007680A (en) | 1909-12-03 | 1909-12-03 | Process of making soap powder. |
Country Status (1)
Country | Link |
---|---|
US (1) | US1007680A (en) |
-
1909
- 1909-12-03 US US53123609A patent/US1007680A/en not_active Expired - Lifetime
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