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
  • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents 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
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/66—Non-ionic compounds
  • C11D1/72—Ethers of polyoxyalkylene glycols
• • 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
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads

Definitions

• the new method includes the mixing of the liquid nonionic material with specific particulate carrier materials in amounts varying from 30 to 85 weight percent.
• Suitable carrier materials include compounds having functional properties in detergent formulations.
• the free flowing nonionc surfactantcarrier pre-mix is very suitable for post addition to spray dried detergent formulations in order to increase their content of nonionic surfactant.
• the invention pertains to heavy duty particulate detergent formulations that include anionic, cationic, or nonionic surface active agents and detergent builders. More specifically the invention provides heavy duty detergents having a relatively high content of nonionic surface active agent.
• anionic compounds having detersive properties. Typical of these anionic compounds are the higher alkyl mononuclear aromatic sulfonates such as the higher alkyl benzene sulfonates. These synthetic detergents are very effective in removing dirt from textile fabrics when utilized in conjunction with phosphate builders which function to soften the water being used and to provide detersive action.
• phosphate builders which function to soften the water being used and to provide detersive action.
• the phosphate compounds present in detergent containing waste water are a prime factor in promoting this phenomenon.
• nonionic surfactants are not as effective as anionic surfactants in the presence of large amounts of phosphate builders, it has been discovered that when the phosphate content of a detergent formulation is substantially reduced, the nonionic surfactants appear to provide detergency properties that are superior to anionics in the same reduced phosphate content formulation. Apparently the detersive effectiveness of nonionic surfactants is affected much less by water hardness than that of the commonly used anionic surfactants. In the event that phosphate builders are totally or partially removed from detergents, the incorporation of greater and greater amounts of nonionic surfactants into detergent formulations will become very desirable.
• nonionic surfactants are added to detergent formulations, primarily to reduce the amount of foam generated during the washing cycle.
• the most commonly used nonionic surfactants are long carbon chain alcohols ethoxylated with ethylene oxide.
• the nonionic ethoxamer used has a 12 to 18 carbon atom alkyl chain and an average of about to l9-ethylene oxide units.
• the range of ethylene oxide content that provides the greatest detergency in these surfactants usually results in a nonionic material that is a viscous liquid at room temperature and therefore unsuitable for direct addition to the dry detergent powder.
• the primary objective of the present invention is to provide a method for converting liquid nonionic surfactants to dry free flowing particulate form so that they may be post added to spray dried detergent formulations and thereby significantly increase the nonionic surfactant content of the final detergent product.
• the maximization of the nonionic surfactant content of the post addable free flowing powder and the selection of particularly suitable carriers for the nonionic materials are important further objectives of the invention.
• the present invention provides a method for obtaining free flowing particulate materials having a nonionic surfactant content of up to about by weight, and preferably above 30% by weight.
• the new materials are very suitable for post addition to spray dried detergent powders in order to substantially raise the nonionic surfactant content of the finished detergent product.
• the invention provides specific carrier materials for nonionic surfactants that are capable of high nonionic loadings; some of which also contribute functional characteristics to the detergent formulation.
• silica substances in general, and microsized silicon dioxide particles in particular are capable of carrying a high loading (about 85% by weight) of nonionic surfactant without losing their free flowing characteristics.
• microsized silicon dioxide is used as an anti-oaking agent in some detergent formulations, its use as a liquid nonionic carrier provides anti-caking properties as well as a higher nonionic content to the detergent formulation it is ultimately combined with.
• the aforementioned silica substances when added to a mixture of nonionic surfactant and other carrier, in accordance with the invention, substantially increases the maximum nonionic loading of the resulting post addable, free flowing mix.
• nonphosphate detergent builders are suitable carriers for liquid nonionic surfactants.
• these builder-carrier substances are the sodium salts of nitrilotriacetic acid (NTA), sodium carbonate and sodium citrate. Loadings of up to about 50% by weight of nonionic surfactant have been obtained with these buildercarriers either individually or in combination with each other in multi-component systems.
• the nonionic loading of these builder-carriers can be increased to over about 60 weight percent by adding a small amount, typically about 5- percent by weight, of a silica substance, preferably microsized silicon dioxide particles, to the blend.
• a silica substance preferably microsized silicon dioxide particles
• pyrogenic microsized silicon dioxide particles are preferred in the practice of the invention other microsized silicon dioxide particles such as silica gel and diatomaceous silica have given satisfactory results.
• peroxygen bleaching agents have been found to be suitable carriers for nonionic surfactants while still retaining their free flowing properties.
• Peroxygen bleaching agents are advantageous carriers for liquid nonionic surfactants when it is also desirable to include a bleaching component in the final formulation. This is particularly so when only one post addition operation can be performed since both post additives can be added simultaneously in accordance with this aspect of the invention.
• the silicon dioxide particulate material used is available under the trademark Cab-O-Sil, grade EI-I- from the Cabot Company, Cab-O-Sil is a submicroscopic particle size silica prepared by vapor phase hydrolysis of silicon tetrachloride at 1100 C. All experimental runs were made at room temperature and atmospheric pressure.
• EXAMPLE 1 50 grams of molten nonionic surfactant was heated to slightly above room temperature until clear in appearance and then sprayed onto grams of colloidal pyrogenic silicon dioxide. The resulting mixture was a free flowing powder having a nonionic loading of 83.3% by weight. The following techniques were used.
• the solidification mechanism of the foregoing procedures is believed to involve the coating of the liquid surfactant particles by the microscopic silicon dioxide particles rather than the absorption or adsorption of the liquid by the particles.
• the free flowing powder produced by the foregoing method can be post added to spray dried detergent powders or, detergent builders and other detergent ingredients can be added to the nonionic powder to produce a finished detergent formulation.
• An example of the latter procedure is to first prepare a free flowing powder consisting of 250.0 grams of a liquid nonionic surfactant and 50.0 grams of silicon dioxide carrier (83.3 weight percent nonionic). To this blend 100.0 grams of sodium salts of (NTA) and 100.0 grams of sodium citrate were added and blended to produce a finished detergent formulation having the following approximate composition:
• Nonionic surfactant 50 Silicon dioxide 10 Sodium salt of NTA Sodium citrate 20 This later formula can be utilized as a detergent itself or as an additive to other detergent systems.
• EXAMPLE 2 The liquid nonionic surfactant was slowly added to a laboratory mortar containing any one or a combination of the following inorganic particulate materials: sodium carbonate, clays (such as bentonite and zeolite), diatomaceous earth (Celite Filteraid available from Johns- Manville Company) or aluminum oxide. Upon blending the liquid nonionic and the inorganic particulate material with a pestle, partial solidification of the mixture occurs. Upon setting at room temperature for about one hour a free flowing powder is obtained.
• inorganic particulate materials sodium carbonate, clays (such as bentonite and zeolite), diatomaceous earth (Celite Filteraid available from Johns- Manville Company) or aluminum oxide.
• liquid nonionic loadings as high as 50% by weight can be obtained without impairing the fiowability of the resulting solid particulate material.
• EXAMPLE 3 Colloidal pyrogenic silicon dioxide, in various amounts, was thoroughly mixed into the partially solidified mixture of Example 2 before final setting.
• Nonionic surfactant loadings of from 50 to weight percent (based on the total inorganic content) were obtained when from about 5 to 25 percent by weight pyrogenic silicon dioxide was added to the mixture.
• Representative free flowing compositions obtainable by this method are:
• Nonionic 60.0 Sodium carbonate 35.0 SiO 5.0
• EXAMPLE 4 From 50 to 80 weight percent of the liquid nonionic surfactant was blended with a mixture of 15 to 45 weight percent of an organic nitrogenous compound chosen from the group consisting of melamine, glycine and iminodiacetic acid and from 0 to 50 percent by weight of any one or a mixture of the inorganic carriers of Example 2. Upon mixing, partial solidification occurs. The addition of at least 5 percent by weight of colloidal pyrogenic silicon dioxide and subsequent thorough blending results in solidification of the mixture. The solidified mixture can be broken up into a free flowing, non-caking powder. The following free flowing powder compositions have been obtained by the foregoing method:
• Nonionic 70 Sodium salt of glycine or iminodiacetic acid 20 SiO 10
• Nonionic 80 Sodium salt of glycine or iminodiacetic acid 3 Bentonite 7 SiOz 10
• Nonionic 80 Sodium salt of glycine or iminodiacetic acid 10 SiO 10 5
• Nonionic 80 Sodium salt of glycine or iminodiacetic acid 3 SiO 15
• the procedures and compositions of Example 4 were followed except that a non-nitrogenous organic material chosen from the group consisting of sodium glycolate, glycolic acid, sorbitol, and potassium sodium tartrate, was substituted for the nitrogen containing organic compounds.
• the following free flowing powder formulations were obtained by the foregoing method:
• Nonionic surfactant 56.6 Sodium salt of NTA 13.0 Sodium citrate 13.0 Si0 17.4
• the resulting free flowing powder is very suitable for post addition to a spray dried detergent powder. Similar free flowing powder can be obtained without the addition of SiO by reducing the nonionic content to about 30 percent by weight.
• Nonionic surfactant 60.0 Sodium salt of NTA 15.0 Sodium carbonate 15.0
• the resulting free flowing powder is very suitable for post addition to a spray dried detergent powder.
• EXAMPLE 8 35 weight percent of liquid nonionic surfactant is blended together with 65 weight percent sodium perborate monohydrate. The resulting mixture is a free flowing powder suitable for post addition to spray dried detergent formulations.
• Runs similar to Examples 1-8 were made using liquid nonionic surfactants having a longer alkyl chain than Neodol 4511, i.e. 16-18 carbon atoms, and a higher ethylene oxide content, i.e. an average of 19 ethylene oxide units.
• a suitable liquid nonionic meeting these requirements is available from the Continental Oil Company under the trademark Alfonic 1618-78. It was found that, Alfonic 1618-78 can be solidified with less effort, i.e. in less time, than Neodol 45-11 and to approximately the same loadings.
• Non-caking powders Functional carriers that can be heavily loaded with nonionic surfactants and still remain free flowing, non-caking powders were found to include pyrogenic silicon dioxide, which functions as an anti-caking agent in the final formulation, and various detergent builders such as NTA, sodium carbonate and sodium citrate.
• pyrogenic silicon dioxide which functions as an anti-caking agent in the final formulation
• various detergent builders such as NTA, sodium carbonate and sodium citrate.
• sodium perborate monohydrate is a surprisingly good carrier for the nonionic component since both can thereby be added in one post addition operation.
• the addition of a small amount of pyrogenic silicon dioxide to mixtures of liquid nonionic surfactant and carrier material have been found to significantly increase the nonionic loadings of the final post addable mixture while still retaining the necessary free flowing characteristics.
• phosphate detergent builders have also been found to be very suitable carriers for liquid nonionic surfactants, their use is not preferred at this time because of the alleged contribution of phosphates to the eutrophication process in natural bodies of water.
• all or part of the phosphate builder can be added to the formulation subsequent to spray drying as a carrier for nonionic surfactants.
• phosphate builders such as the sodium tripolyphosphate can be loaded with up to about 30 percent by weight liquid nonionic surfactant while still retaining free flowing properties.
• the nonionic loading on phosphate carriers can be increased to about 50 percent by weight by adding about 5 percent by weight of a microsized silica substance to the nonionic-carrier mixture before final setting.
• the invention represents a significant step towards the substantial reduction of phosphate builders from detergent formulations without a significant decrease in cleaning eflicacy.
• a heavy duty detergent which includes the step of spray drying a detergent slurry to form a dry, free-flowing powder, the improvement comprising adding to said spray dried powder a free flowing pre-mix including about 85% by weight of a liquid ethoxylated alcohol nonionic surface active agent and at least 5% by weight of microsized silica particles said pre-mix being prepared by mixing said liquid nonionic with a sufficient quantity of silica particles to fully solidify said liquid nonionic.
• silica particles comprise a silicon dioxide compound.

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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)
• Inorganic Chemistry (AREA)
• Detergent Compositions (AREA)

Applications Claiming Priority (2)

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Cited By (36)

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• 1971
  • 1971-02-09 US US00114073A patent/US3769222A/en not_active Expired - Lifetime
• 1972
  • 1972-01-31 GB GB442272A patent/GB1369352A/en not_active Expired
  • 1972-02-02 DE DE2204842A patent/DE2204842C2/de not_active Expired
  • 1972-02-02 CA CA133,787A patent/CA971071A/en not_active Expired
  • 1972-02-07 FR FR7203954A patent/FR2124523B1/fr not_active Expired
  • 1972-02-07 CH CH171472A patent/CH567569A5/xx not_active IP Right Cessation
  • 1972-02-07 AU AU38759/72A patent/AU464206B2/en not_active Expired
  • 1972-02-08 AT AT99672*#A patent/AT335026B/de not_active IP Right Cessation
  • 1972-02-09 NL NLAANVRAGE7201725,A patent/NL178263B/xx not_active Application Discontinuation
• 1973
  • 1973-02-26 US US335873A patent/US3915878A/en not_active Expired - Lifetime

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