US2412944A - Method of producing a detergent composition - Google Patents

Method of producing a detergent composition Download PDF

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US2412944A
US2412944A US539596A US53959644A US2412944A US 2412944 A US2412944 A US 2412944A US 539596 A US539596 A US 539596A US 53959644 A US53959644 A US 53959644A US 2412944 A US2412944 A US 2412944A
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acid
solution
soap
alkali metal
water
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US539596A
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Frederick C Bersworth
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    • 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
    • C11D9/00—Compositions of detergents based essentially on soap
    • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
    • C11D9/22—Organic compounds, e.g. vitamins
    • C11D9/30—Organic compounds, e.g. vitamins containing nitrogen

Definitions

  • This invention relates to detergent comp'ositions and more particularly to detergent compositions suitable for use in hard, saline, and hardsaline water, and is an improvement invention of the invention described'and claimed in copending application Serial No. 539,595, filed June 9, 1944, which application is assigned to the same assignee as the present invention.
  • One of the objects of the present invention is to provide a detergent composition for use in hard, saline, and hard-saline water.
  • Another object is to provide a composition having detergent and deionization properties for use alone or in combination with alkali metal-fatty acid soap compounds in hard, saline and hardsaline water.
  • Still another object is to provide a deionlzation agent compatible with alkali metal-fatty acid soap compounds in aqueous solutions.
  • alkali metal salts utillzable as deionization agents and electrolyte-carrying agents with alkali metalfatty acid soap compounds in aqueous solutions are the acid-alkali metal salts of the aliphatic amino polycarboxylic acids, particularly those amino acids containing more than two carboxylic acid groups attached directly to amino nitrogens, such as the acid-alkali metal salts of ethylene diamine tetracarboxylic acid which in molar weight aqueous solution have a PH between 7 and 9.5, preferably those having a pH of approximately 8,
  • a detergent composition consisting of an equilibrium mixture of the acid-alkali metal salt of the amino acid, particularly ethylene dianiine tetracarboxylic acid, and a mono-basic fatty soap acid, such as stearic acid, in aqueous solution having a pH within the range '7to 9.5 but preferably approximating a pH of about 8, by saponifying the fatty acid in an aqueous solution of the tetra alkali metal salt of the amino-acid until the pH of the solution approximates 8 or is within the range 7 to 9.5.
  • This equilibrium solution of amino acid, fatty acid and caustic alkali, having a pH of about 8, is a detergent composition suitable for use in hard water of various de rees of hardness, in water containing neutral electrolytes such as sodium chloride or sodium sulfate, and also in hard-saline water such as sea water.
  • the said equilibrium 2 solution is also miscible in all proportions with alkali metal-fatty acid soap compounds to form a plurality of detergent compositions that are also suitable for use in hard water'of various derees of hardness, in water containing strong neutral electrolytes, and in hard-saline water, such as seasvater.
  • the invention will be described as it has been adapted to the forma tion of a detergent composition consisting of an equilibrium mixture of an acid-alkali metal salt of ethylene diamine tetracarboxylic acid and the alkali metal salt of stearlcacid.
  • a detergent composition consisting of an equilibrium mixture of an acid-alkali metal salt of ethylene diamine tetracarboxylic acid and the alkali metal salt of stearlcacid.
  • an aqueous solution of the tetrasodium salt of ethylene diamine tetracarboxylic acid containing one molar weight (or 380 grams) in 3% liters of water (3500 c; c.) having 9.
  • PH of about 10.5 is digested under a reflux condenser with 1 /2 molar weights (427.5 grams) of stearic acid, at elevated temperatures approximating the boiling point of the solution for an extended time interval until the pH of the solution approximates 8.
  • the resulting solution is filtered while hot, to remove therefrom any unsaponifled fatty acid, and then is cooled to atmospheric temperatures. At atmospheric temperatures the solution solidifies to a substantially transparent jelly which is 'completely soluble in cold or warm water.
  • the solution may be heated in an autoclave under a pressure of steam approximating 20 pounds.
  • the chemical reaction involved in this process is essentially one of saponification of the stearic acid by the caustic alkali set free in aqueous solution by ionization of the tetrasodium salt of the amino acid.
  • This salt in aqueous solution has a pH of about 10.5 and, in accordance with my experiments, the tetra salt in aqueous solutions of about this concentration hydrolyzes with liberation of two molecules of caustic alkali per molecule of tetra salt present.
  • Stearic acid in an amount somewhat in excess of that approximately suihcient to combine with one of the molecules of caustic alkali liberated by the tetra salt, is preferably employed, to shorten the time interval of heating required to obtain, by saponiflcation of the stearic acid, a lowering of the pH of the solution to the desired figure of pH 8 within the range 7 to 9.5.
  • the saponiflcation reaction proceeds to an equilibrium composition consisting essentially oi the acid-trisodium salt of reaction time and reaction pressures, as one v skilled in the art may perceive.
  • I may form substantially the same detergent composition by digesting at elevated temperatures, one molar weight of the amino acid and 1 /2 molar weights of the stearic acid in an aqueous caustic alkali solution of the same approximate volume containing about 4 molar weights of caustic alkali (NaOH), until a solution having a pH of approximately 8 is obtained.
  • the detergent composition obtained by the practice of the above disclosed method is miscible in all proportions with alkali metal-fatty acid soap compounds to form detergent compositions suitable for use in a plurality of different types and kinds of hard waters, electrolyte-carrying waters and in hard-saline waters.
  • a soa solution containing 10 to 15% alkali metal-fatty acid soap compounds is usually employed to which soap solution various water softening agents in proportion to the hardness of the water being used may be added to form a stock soap solution.
  • soap solution various water softening agents in proportion to the hardness of the water being used may be added to form a stock soap solution.
  • from to (dry weight) of the detergent composition of the above speciflc example based on the weight of the soap compounds present in the soap solution, is added to the soap solution for use with medium to hard water; from 10 to of the composition is added for use with hard to very hard water and with water containing moderate amounts of electrolytes; and from 15 to of the composition is added for extremely hard water or for water containing relatively large amounts of electrolytes and for hard-saline water, such as sea water.
  • I may also employ a large number of other organic acids, such as the di-basic acids and poly-basic acids to neutralize the free alkali of the solution and to obtain Various equilibrium mixtures having a pH within the range specified which, while not necessarily being detergent compositions, are miscible in all proportions with alkali metal-fatty acid soap compounds to form a detergent composition containing the deionizing and electrolytecarrying acid-alkali metal aliphatic polycarboxylic acid complex of the presentinvention and of the invention of my co-pending application Berial No. 539,595, above identified.
  • a detergent composition consisting of a water soluble mixture of an acid alkali metal salt of an aliphatic amino polycarboxylic acid having more than two carboxylic acid groups attached directly to amino nitrogens with at least one of the carboxylic groups in excess of two unneutralized by alkali metal and an alkali metal salt of a monobasic fatty soap acid, which comprises forming an aqueous solution of the fully neutralized alkali metal salt of said amino acid, adding thereto the monobasic fatty soap acid in such an amount required to combine with at least one of the alkali metal ions of each molecule of the salt of said amino acid and to lower the pH of the solution to a pH within the range '7 and 9.5, heating the solution for an extended time interval to solubilize the mono-basic fatty soap acid as the alkali metal salt of mono-basic fatty soap acid, and filtering the solution while hot to remove the excess monobasic fatty soap acid present therein.

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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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

' Patented u e. 24, 1
1 U TED -mirnon or rnonucmo a DETERGENT ooMrosmoN Frederick c. Bersworth, erona, N. .1.
No Drawing. Application June 9, 1944, Serial No. 539.595
' 2 Claims. (01. 252-117) This invention relates to detergent comp'ositions and more particularly to detergent compositions suitable for use in hard, saline, and hardsaline water, and is an improvement invention of the invention described'and claimed in copending application Serial No. 539,595, filed June 9, 1944, which application is assigned to the same assignee as the present invention.
One of the objects of the present invention is to provide a detergent composition for use in hard, saline, and hard-saline water.
Another object is to provide a composition having detergent and deionization properties for use alone or in combination with alkali metal-fatty acid soap compounds in hard, saline and hardsaline water.
Still another object is to provide a deionlzation agent compatible with alkali metal-fatty acid soap compounds in aqueous solutions.
Other objects will be apparent as the invention is more fully hereinafter disclosed.
' In accordance with the disclosure of my copending application Serial No. 539,595, above noted, I have discovered that the only alkali metal salts utillzable as deionization agents and electrolyte-carrying agents with alkali metalfatty acid soap compounds in aqueous solutions are the acid-alkali metal salts of the aliphatic amino polycarboxylic acids, particularly those amino acids containing more than two carboxylic acid groups attached directly to amino nitrogens, such as the acid-alkali metal salts of ethylene diamine tetracarboxylic acid which in molar weight aqueous solution have a PH between 7 and 9.5, preferably those having a pH of approximately 8,
In accordance with the present invention 1 form a detergent composition consisting of an equilibrium mixture of the acid-alkali metal salt of the amino acid, particularly ethylene dianiine tetracarboxylic acid, and a mono-basic fatty soap acid, such as stearic acid, in aqueous solution having a pH within the range '7to 9.5 but preferably approximating a pH of about 8, by saponifying the fatty acid in an aqueous solution of the tetra alkali metal salt of the amino-acid until the pH of the solution approximates 8 or is within the range 7 to 9.5.
This equilibrium solution of amino acid, fatty acid and caustic alkali, having a pH of about 8, is a detergent composition suitable for use in hard water of various de rees of hardness, in water containing neutral electrolytes such as sodium chloride or sodium sulfate, and also in hard-saline water such as sea water. The said equilibrium 2 solution is also miscible in all proportions with alkali metal-fatty acid soap compounds to form a plurality of detergent compositions that are also suitable for use in hard water'of various derees of hardness, in water containing strong neutral electrolytes, and in hard-saline water, such as seasvater.
As a specific embodiment of this invention, but not as a limitation thereof, the invention will be described as it has been adapted to the forma tion of a detergent composition consisting of an equilibrium mixture of an acid-alkali metal salt of ethylene diamine tetracarboxylic acid and the alkali metal salt of stearlcacid. In this example an aqueous solution of the tetrasodium salt of ethylene diamine tetracarboxylic acid containing one molar weight (or 380 grams) in 3% liters of water (3500 c; c.) having 9. PH of about 10.5 is digested under a reflux condenser with 1 /2 molar weights (427.5 grams) of stearic acid, at elevated temperatures approximating the boiling point of the solution for an extended time interval until the pH of the solution approximates 8. The resulting solution is filtered while hot, to remove therefrom any unsaponifled fatty acid, and then is cooled to atmospheric temperatures. At atmospheric temperatures the solution solidifies to a substantially transparent jelly which is 'completely soluble in cold or warm water.
To materially shorten the time interval of heatms to obtain the saponification ofthe stearic acid by the free alkali present in the aqueous solution of the tetra salt, the solution may be heated in an autoclave under a pressure of steam approximating 20 pounds.
The chemical reaction involved in this process is essentially one of saponification of the stearic acid by the caustic alkali set free in aqueous solution by ionization of the tetrasodium salt of the amino acid. This salt in aqueous solution has a pH of about 10.5 and, in accordance with my experiments, the tetra salt in aqueous solutions of about this concentration hydrolyzes with liberation of two molecules of caustic alkali per molecule of tetra salt present. Stearic acid, in an amount somewhat in excess of that approximately suihcient to combine with one of the molecules of caustic alkali liberated by the tetra salt, is preferably employed, to shorten the time interval of heating required to obtain, by saponiflcation of the stearic acid, a lowering of the pH of the solution to the desired figure of pH 8 within the range 7 to 9.5.
The saponiflcation reaction proceeds to an equilibrium composition consisting essentially oi the acid-trisodium salt of reaction time and reaction pressures, as one v skilled in the art may perceive.
Alternatively, I may form substantially the same detergent composition by digesting at elevated temperatures, one molar weight of the amino acid and 1 /2 molar weights of the stearic acid in an aqueous caustic alkali solution of the same approximate volume containing about 4 molar weights of caustic alkali (NaOH), until a solution having a pH of approximately 8 is obtained.
The detergent composition obtained by the practice of the above disclosed method is miscible in all proportions with alkali metal-fatty acid soap compounds to form detergent compositions suitable for use in a plurality of different types and kinds of hard waters, electrolyte-carrying waters and in hard-saline waters.
As an illustration, in accordance with usual laundry practice a soa solution containing 10 to 15% alkali metal-fatty acid soap compounds is usually employed to which soap solution various water softening agents in proportion to the hardness of the water being used may be added to form a stock soap solution. In accordance with the present invention, from to (dry weight) of the detergent composition of the above speciflc example, based on the weight of the soap compounds present in the soap solution, is added to the soap solution for use with medium to hard water; from 10 to of the composition is added for use with hard to very hard water and with water containing moderate amounts of electrolytes; and from 15 to of the composition is added for extremely hard water or for water containing relatively large amounts of electrolytes and for hard-saline water, such as sea water.
The addition of the detergent composition of the present invention to soap solutions or to solid and liquid soap compounds presents no particular problem as the detergent is miscible in all proportions with such soap compounds. In general, identically the same practice as has heretofore been followed in the soap art is followed in the forming of bar, flake, powder, or liquid soap compositions including the detergent composition of the present invention or in the forming of concentrated aqueous soap solutions.
In the adaptation of the present invention to the forming of detergent compositions consisting of a mixture of the acid-alkali metal salts of any of the other aliphatic amino polycarboxylic acids heretofore recognized in the art as strong deionizing agents and the alkali metal salt of a. soa fatty acid, substantially the same procedure is water soluble alkali metal salts of the fatty acid, thereby lowering the pH of the solution to within the range 7 to 9.5 and preferably to a pH of about 8. The precise amount of fatty acid required to obtain this desired result will vary with respect to variation in the amount of free alkali liberated by the amino acid salt in aqueous solution or present in the solution in addition thereto.
In place of a soap fatty acid, I may also employ a large number of other organic acids, such as the di-basic acids and poly-basic acids to neutralize the free alkali of the solution and to obtain Various equilibrium mixtures having a pH within the range specified which, while not necessarily being detergent compositions, are miscible in all proportions with alkali metal-fatty acid soap compounds to form a detergent composition containing the deionizing and electrolytecarrying acid-alkali metal aliphatic polycarboxylic acid complex of the presentinvention and of the invention of my co-pending application Berial No. 539,595, above identified.
Having hereinabove described the present invention generically and specifically and given one specific example of the same, it is believed apparent that the same may be widely varied without essential departure therefrom and all such modifications and adaptations of the same are contemplated as may fall within the scope of the following claims:
What I claim is:
1. The method of forming an aqueous solution containing about one molar weight of the trisodium salt of ethylene diamine tetracarboxylic acid and about 1 molarweight of the sodium salt of stearic acid which comprises dissolving about one molar weight of the tetrasodium salt followed as hereinabove described, namely thev aqueous solution of the fully neutralized salt of the amino acid is digested with the said fatty soap acid until the free alkalicontent of the aqueous solution has been substantially removed therefrom by reaction with the said fatty acid to form of the said amino acid in a volume of water, adding thereto about 1 /2 molar weights of stearic acid, and heating the solution for an extended time interval until the pH of the solution is stabilized at a pH of about 8, and filtering the solution while hot to remove the excess stearic acid present therein.
' 2. The method of producing a detergent composition consisting of a water soluble mixture of an acid alkali metal salt of an aliphatic amino polycarboxylic acid having more than two carboxylic acid groups attached directly to amino nitrogens with at least one of the carboxylic groups in excess of two unneutralized by alkali metal and an alkali metal salt of a monobasic fatty soap acid, which comprises forming an aqueous solution of the fully neutralized alkali metal salt of said amino acid, adding thereto the monobasic fatty soap acid in such an amount required to combine with at least one of the alkali metal ions of each molecule of the salt of said amino acid and to lower the pH of the solution to a pH within the range '7 and 9.5, heating the solution for an extended time interval to solubilize the mono-basic fatty soap acid as the alkali metal salt of mono-basic fatty soap acid, and filtering the solution while hot to remove the excess monobasic fatty soap acid present therein.
FREDERICK C. BERSWORTH.
US539596A 1944-06-09 1944-06-09 Method of producing a detergent composition Expired - Lifetime US2412944A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2673144A (en) * 1950-06-10 1954-03-23 Standard Oil Co Auxiliary alcohol-water fuel
US2828262A (en) * 1955-04-19 1958-03-25 Exxon Research Engineering Co Soap-salt complex thickened grease compositions
US3074982A (en) * 1959-02-19 1963-01-22 Anderson Lab Inc Method of fat extraction and extractant therefor

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2673144A (en) * 1950-06-10 1954-03-23 Standard Oil Co Auxiliary alcohol-water fuel
US2828262A (en) * 1955-04-19 1958-03-25 Exxon Research Engineering Co Soap-salt complex thickened grease compositions
US3074982A (en) * 1959-02-19 1963-01-22 Anderson Lab Inc Method of fat extraction and extractant therefor

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