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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0047—Detergents in the form of bars or tablets
  • C11D17/006—Detergents in the form of bars or tablets containing mainly surfactants, but no builders, e.g. syndet bar
• • 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/2093—Esters; Carbonates

Definitions

• This invention relates to improvements in synthetic detergents, and more particularly to an improved method of treating detergent masses comprising solid, synthetic organic detergent material to produce a compacted mass or body which is cohesive and firm, and which can be readily formed into a commercially desirable bar or cake.
• the invention in its broadest aspect comprises the improvement in the process or plodding a detergent composition
• a detergent composition comprising essentially solid, synthetic, organic non-soap detergent material which comprises heating and plodding the synthetic detergent mass while the same is of low or reduced moisture content, and contains sufficient amount of a high molecular weight organic compound or mixture of organic compounds which function both as a plasticizer and a plasticity modifier so that the plasticity range or temperature at which the detergent mass may be plodded is considerably wider than otherwise would be the case.
• Suitable amounts of other substances such as fillers, builders, coloring material, perfume, etc. also may be incorporated to produce a finished product having the physical characteristics desired.
• the temperature to which the detergent mass is subjected during plodding will depend largely upon the particular synthetic material used as well as the plasticizer employed, but is sufiicient to maintain the mass soft and workable but not so high as to convert the same into a liquid state.
• the moisture content of the detergent mass is reduced to a low percentage amount, or such that it does not contain more than about 5% by weight and preferably is below 2%, A suitable amount of a nonvolatile high molecular weight organic plasticity modifying agent is incorporated, and the mass is heated to a plastic state and plodded while thus heated.
• the working temperature for plodding solid synthetic non-soap detergent m a s s e s generally lies within a critical range of a few degrees, and, unless strict control is exercised, sticking and damage to the equipment and/ or synthetic product during plodding may result.
• the detergent mass sets either too rapidly or too slowly, so that the batch can not be used.
• the non-soap synthetic detergent material may include the solid, water-soluble salts of one or more sulfated or sulfonated organic compounds, the alkyl radical groups of which contain at least eight carbon atoms, such. as higher fatty alcohol sulfates (Gardinols), sulfated or sulfonated monoglycerides i. e. sodium glyceryl monolaurate sulfate (Syntex M), secondary alcohol sulfonates i. e. dioctyl sodium sulfosuccinate (Aerosol O.
• sulfated or sulfonated organic compounds the alkyl radical groups of which contain at least eight carbon atoms, such. as higher fatty alcohol sulfates (Gardinols), sulfated or sulfonated monoglycerides i. e. sodium glyceryl monolaurate sulfate (Syntex M), secondary
• alkyl aryl sulfonates i. e. sulfonated benzene which contains an alkyl substituent of about to 14 carbon atoms
• alkyl sulfonates i. e. sodium alkyl sulfonates produced from petroleum or similar hydrocarbons (Mersolates, Merpols, etc.)
• fatty acid esters of alkyl hydroxy or amine sulfonic acid i. e.
• Nonionic, solid synthetic detergents may be used, i. e. polymerized ethylene oxide condensates, fatty acid polyoxyethylene derivatives, etc., and marketed under such names as Biopal, Sorapal, Igepal, etc. Also mixtures of the nonionic type detergents with ionic detergents may be utilized.
• Plasticizing agents are organic compounds which are solids, semi-solids or oily liquids at ordinary temperatures and of the high boiling non-volatile type havin limited solubility in water, or at least dissolve very slowly therein. They are also resistant to crystallization and segregation under the diiferent temperature and aging conditions to which the detergent bar or cake may be subjec' ed during storage and use.
• the plasticizing substances which are solid or semisolid, and which maintain a more or less definite form at ordinary temperatures, are hereinafter referred to as normally solid substances.
• Organic compounds which have been found to function satisfactorily as plasticizing agents which broaden the plasticity range, as aforementioned, are the high molecular weight fatty acid esters of polyhydrlc alcohols.
• lhese compounds also function as emulsifying agents, thus promoting the formation of a synthetic detergent bar having a smooth, uniform texture throughout.
• organic plasticizing agents which may be used are the normally solid polyethylene glycols (a known product being sold under the name Carbowax), glycerol mono esters of coconut fatty acids, ethylene glycol distearate, and the diethylene glycol mono and di-esters of palmitic, myristic, oleic, lauric and coconut oil acids; propylene glycol mono and di-esters of stearic, oleic, lauric, myristic, palmitic, coconut oil fatty acids, etc., as well as suitable glyceryl and ethylene glycol mono esters of such fatty acids, and the like, which esters are normally solid, or Olly liquids, and which dissolve in water but at a slow rate.
• a plodded detergent bar which contains plasticity modifying agent as herein described, hardens gradually upon standing in the air at room temperatures without changing its other physical properties or its chemical properties.
• plasticizer varies depending upon the composition to be plodded and the plasticizing agent employed. Additions of relatively small amounts up to 20% or more by weight of the detergent mass may be utilized to advantage.
• the moisture content of the synthetic detergent mixture plcdded is preferably reduced as much as practicable, as by initially spray drying or roll drying the mass prior to plodding so that most or practically all the water is removed.
• the lower water content of the synthetic detergent mass from which the bars and cakes are produced in accordance with this invention has the further advantage of permitting the exercise of some control over the speed at which the synthetic cake dissolves in water. For example, by varying the proportion of the constituents while maintaining the synthetic detergent mass substantially anhydrous, the water dissolving properties of the finished bar or cake may be varied, and bars made which dissolve in water at a slower and more satisfactory rate.
• the plodding may be accomplished while the mass is heated to around 115 F., or lower, although for most purposes the plodding is carried out between about 120 and 150 F.
• Any waste or scrap detergent formed may be reworked even after aging several days or a month without producing an inferior detergent bar.
• the plodder is stopped during operation, it is unnecessary to remove the synthetic detergent material, or disassemble and clean the plodder prior to resuming plodding, as has been often required heretofore, particularly where attempts have been made to plod a synthetic detergent body which contained substantial amounts of water.
• Example I Percent by weight Sodium salt of the sulfated monoglycerides of coconut oil fatty acids (salt-free) 78.0 Zinc stearate l 15.0 Diethylene glycol monostearate 6.0 Titanium dioxide 0.5 Perfume 0.5
• the above mixture comprising the synthetic detergent, filler, and plasticizer was roll dried to provide a low moisture mass, and the detergent mixture was then passed, through a three-r011 mill several times during the latter part of which operation the perfume was incorporated. Thereafter the warm ribbons formed on the roll, and containing approximately one percent moisture, were transferred to a plodder and plodded at a temperature of between to F. In this instance, the plodding was carried out under a vacuum, such as described in the United States patent to Schwa-ntes 2,146,770, to produce a higher specific gravity non-floating bar.
• the mass was extruded in the form of a bar which was cut into cakes or blanks and pressed in a die to provide a finished cake of the desired shape and markings.
• the extrusion nozzle of the plodder was heated somewhat above the plodding temperature, as in Example I, to produce an extruded bar having a smooth, even surface.
• Example II The spray dried solid synthetic detergent and remaining ingredients were suitably admixed and aeaaoer milled as described in Example I.
• a smooth plodded bar was obtained which was cut into blanks to form cakes.
• Example IV Percent by weight Sodium salt of the sulfated monoglycerides of coconut oil fatty acids (salt-free) 48.0 Igepon T (sodium fl-oleyl-amino-ethanesulfonate) 2.0 Boric acid 23.0 Disodium diacid pyrophosphate 10.0
• Carbowax 4000 solid polyethylene glycols 10.0
• Glycerine 1.0 Sodium soap chips 2.0 Irish moss 2.0 Titanium dioxide 1.0 Perfume 1.0
• Example V Percent by weight Sodium salt of the sulfated monoglycerides of coconut oil fatty acids (35% active synthetic) 88.75 Diethylene glycol monostearate 10.00 Coloring material 0.25 Perfume 1.00
• Example II The constituents were admixed similarly as in Example I to provide a low moisture mass which was plodded while heated to between 115 and 125 F.
• Example VI Percent by weight Oronite (sodium salt of alkyl aryl sulfonate active synthetic) 87.00
• Example IV The above ingredients were roll dried as in Example IV to produce a low moisture mass which was plodded while heated to between 120 and 130 F.
• Example VII Percent by weight Spray-dried Igepon AP (sodium salt of 13- laurylethanesulfonate active synthetic) 80.00 Magnesium stearate 12.00 Diethylene glycol monostearate 6.00 Titanium dioxide 1.00 Perfume 1.00
• Example II The constituents were suitably mixed as described in Example I to provide a detergent mass having a low moisture content. The mass was then plodded while heated to between and Example VIII Percent by weight Spray-dried sodium salt of the sulfated monoglycerides of a mixture containing 65% hydrogenated tallow and 35% hydrogenated coconut oil 10% active synthetic) 82.0 Zinc stearate 12.0 Diethylene glycol monostearate 5.0 Titanium dioxide 0.5 Perfume 0.5
• Example III The ingredients were admixed as described in Example III to provide a low moisture detergent mass which was heated to a temperature between 130 and F. and plodded.
• Example VIII illustrates the use of sulfated hydrogenated tallow and coconut oil in place of coconut oil fatty acids, or the like fatty oil acids.
• Mixtures of hydrogenated tallow with fatty oil acids i. e. stearic, palmitic, etc. may also be utilized.
• fatty oil acids i. e. stearic, palmitic, etc.
• a bar having higher or lower solubility may be produced.
• higher amounts of hydrogenated tallow there is produced correspondingly lower solubility bars, but with increased amounts the sudsing and lathering properties of the bars are lessened which for some purposes are undesirable.
• the synthetic detergent may contain relatively large or small amounts of sodium sulfate or such other salts as may be formed during neutralization of the sulfated or sulfonated substances.
• the addition agents i. e. fillers, builders, coloring matter, etc., may be omitted altogether, if desired, or added in substantially reduced amounts such as illustrated in Examples V and VI.
• the proportionate amounts of the components used in making the plodded detergent mass are not critical and may be widely varied and substitutions made depending upon the properties wanted in the final product.
• the synthetic detergent may comprise relatively large or small amounts of salts or modifying agents, such as may be formed during production of the synthetic detergent salt, as aforementioned, or as subsequently incorporated.
• inorganic builders such as phosphates, carbonates, bcrax, etc.
• organic builders i. e. carboxymethylcellulose, higher fatty acid alkylolamides, and etc.
• inorganic or organic coloring materials 1. e. pigments, dyes etc., may be utilized to give the plodded detergent mass or bar a pleasing color or tint.
• Glycerine may be incorporated, as is illustrated in Example IV, to impart emollient characteristics to the finished bars or cakes, and to enhance their gloss.
• Olive oil also may be used for this purpose, and if desired germicidal substances may be added which are compatible and stable.
• sodium salts of the different sulfated or sulphonated synthetic detergents are generally preferred, other salts may be used, and may be more advantageously employed in certain instances.
• the corresponding salts of calcium, barium or magnesium, or mixtures thereof may be utilized.
• plodder Various methods may be employed to heat the plodder, such as by the use of fluid heated jackets, electrical resistances or the like, the plodder being heated sufliciently to cause the detergent mass to become plastic and workable, but not so high as would transform the mass into a liquid state or melt.
• the nozzle of the plodder is heated so that its temperature is somewhat above that of plodding in order to produce an ironing effect on the detergent mass as it is extruded, smoothing out any slight imperfections at the surface which might otherwise produce perceptable serrations on the surface of the bar as it is extruded.
• a milled nonsoap detergent in bar form consisting essentially of detergent material and a plasticizer
• said detergent material being a water-soluble salt of an organic sulfuric reaction product having in its molecular structure a radical selected from the group consisting of sulfonic and sulfuric acid ester radicals and said plasticizer being a normally solid ether-alcohol fatty acid ester which dissolves slowly in water
• said steps which comprise drying the detergent material to a moisture content of not more than by weight, incorporting up to 20% by weight of said plasticizer, heating the resulting mass to a temperature between 110 and 170 F. to render the same plastic and workable but insufficient to cause liquefication of the same, and subjecting said mass while thus heated to a plodding treatment to form a compacted, firm, cohesive detergent body.
• a milled nonsoap detergent in bar form consisting essentially of detergent material and a plasticizer
• said detergent material being a water-soluble salt of an organic sulfuric reaction product having in its molecular structure a radical selected from the group consisting of sulfonic and sulfuric acid ester radicals and said plasticizer being a normally solid partial ester of a long-chain fatty acid and a polyhydric alcohol
• the steps which comprise removing moisture from the detergent material to reduce the moisture content so that it is not more than 5% by weight, incorporating up to 20% by weight of said plasticizer, heating the resulting plasticized mass to a temperature between and F. to render it plastic and workable, and subjecting said mass while thus heated to a plodding treatment to produce a compacted cohesive detergent body.
• a milled nonsoap detergent in bar form consisting essentially of detergent material and a plasticizer
• said detergent material being a water-soluble salt of an organic sulfuric reaction product having in its molecular structure a radical selected from the group consisting of sulfonic and sulfuric acid ester radicals and said plasticizer being normally solid diethylene glycol monostearate
• said steps which comprises drying said detergent materials to produce a detergent mass having a moisture content of not more than 5% by weight, incorporting up to 20% by weight of said plasticizer, heating the resulting plasticized mass to a temperature between 110 and 170 F. to render the same plastic and workable, and plodding said mass while thus heated to produce a compacted cohesive detergent body.
• said detergent material comprises a water-soluble salt of the sulfuric acid ester of a high molecular weight fatty acid monoglyceride.
• said detergent material comprises a water-soluble salt of alkyl aryl sulfonates.
• said detergent material comprises a water-soluble salt of an alcohol sulfonate.

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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)
• Health & Medical Sciences (AREA)
• Emergency Medicine (AREA)
• Detergent Compositions (AREA)
• Cosmetics (AREA)

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Cited By (29)

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Citations (3)

• 1948
  • 1948-08-04 US US42537A patent/US2678921A/en not_active Expired - Lifetime
• 1949
  • 1949-08-03 GB GB20242/49A patent/GB689569A/en not_active Expired
  • 1949-08-04 FR FR991938D patent/FR991938A/fr not_active Expired

Patent Citations (3)

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