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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/046—Salts
• • 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
  • C11D1/38—Cationic compounds
  • C11D1/62—Quaternary ammonium compounds
• • 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
  • C11D11/02—Preparation in the form of powder by spray drying
• • 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
  • C11D3/168—Organometallic compounds or orgometallic complexes
• • 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
  • C11D3/26—Organic compounds containing nitrogen
  • C11D3/33—Amino carboxylic acids
• • 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
  • C11D3/36—Organic compounds containing phosphorus
  • C11D3/361—Phosphonates, phosphinates or phosphonites
• • 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
  • C11D3/37—Polymers
  • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/3757—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions
  • C11D3/3761—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions in solid compositions
• • 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
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/02—Inorganic compounds
  • C11D7/04—Water-soluble compounds
  • C11D7/10—Salts
• • 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
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/22—Organic compounds
  • C11D7/32—Organic compounds containing nitrogen
  • C11D7/3245—Aminoacids

Definitions

• the present invention relates to detergent powders which essentially comprise a complexed chelating agent and an anionic polymer.
• the powders may be readily prepared by spray drying.
• Detergent components and compositions have been made using various spray drying techniques for many years. Typically various detergent active materials are dissolved or dispersed in an aqueous solution which is then pumped under high pressure to an atomiser, such as a nozzle or a spinning disc.
• an atomiser such as a nozzle or a spinning disc.
• chelating agents are frequently precomplexed with magnesium in order to protect them from degradation in the presence of bleach.
• molar ratios of magnesium : chelating agent of greater than 3:1 are difficult to prepare due to precipitation from aqueous solution. Precipitation in a spray drying process rapidly leads to blockage of the nozzle.
• powders which essentially consist of chelating agent / magnesium complex have a very low rate of solubility.
• anionic polymer also enables powders to be prepared which have a very high organic content, preferably greater than 80%. Such powders which are difficult to prepare by other means, provide a convenient method for handling and processing organic polymers.
• the present invention relates to free-flowing detergent powder which is prepared by spray drying, the powder comprising :
• the powder comprises less than 20%, more preferably less than 10% by weight (on anhydrous basis), of inorganic components other than the metal ion (a)(ii). Most preferably the total level of aluminosilicate and carbonate (on anhydrous basis) is less than 10% by weight.
• the chelating agent is preferably selected from the group consisting of phosphonic acid, succinic acid, the salts of phosphonic or succinic acid, or mixtures thereof, even more preferred chelating agents are diethylene triamine penta (methylene phosphonic acid), or ethylenediamine-N-N'-disuccinic acid, or their salts, or mixtures thereof.
• the preferred metal ion is magnesium.
• the molar ratio of the metal ion to the chelating agent is preferably greater than 3:1.
• the polymer may comprise carboxylate functional groups, especially the water-soluble salts of homo-and copolymers of aliphatic carboxylic acids such as acrylic acid, maleic acid, vinylic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid, methylenemalonic acid and mixtures thereof.
• carboxylate functional groups especially the water-soluble salts of homo-and copolymers of aliphatic carboxylic acids such as acrylic acid, maleic acid, vinylic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid, methylenemalonic acid and mixtures thereof.
• a preferred polymer is a copolymer of maleic and acrylic acid having a molecular weight of from 2000 to 100 000.
• the free-flowing detergent powder may also comprise a cationic surfactant.
• the cationic surfactant may be present at from 1% to 80% by weight , from 2% to 20% by weight of dimethyl ethoxy ammonium chloride being preferred.
• the essential components of the present invention are a chelating agent and a polymer comprising anionic functional groups. Examples of these will now be given in more detail.
• the chelating agents suitable for use in the present invention can be chosen from a wide range of chemicals which are known to the man skilled in the art.
• suitable chelating agents are phosphonic and succinic acids and their salts.
• the polyphosphonates are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-1,1-diphosphonic acid and the sodium and potassium salts of ethane, 1,1,2-triphosphonic acid.
• particularly suitable chelating agents are ethylene diamine tetra (methylene phosphonic acid) and diethylene triamine penta (methylene phosphonic acid).
• EDDS ethylenediamine-N,N'-disuccinic acid
• Preferred EDDS compounds are the free acid form and the sodium or magnesium salt thereof.
• Examples of such preferred sodium salts of EDDS include NaEDDS, Na2EDDS and Na4EDDS.
• Examples of such preferred magnesium salts of EDDS include Mg EDDS and Mg2EDDS.
• the magnesium salts are the most preferred for inclusion in compositions in accordance with the invention.
• EDDS can be synthesised, for example, from readily available, inexpensive starting material such as maleic anhydride and ethylene diamine as follows : A more complete disclosure of methods for synthesising EDDS from commercially available starting materials can be found in US Patent 3,158,635, Kezerian and Ramsay, issued November 24, 1964.
• the [S,S] isomer of EDDS can be synthesised from L-aspartic acid and 1,.2-dibromoethane, as follows : A more complete disclosure of the reaction of L-aspartic acid with 1,2-dibromoethane to form the [S,S] isomer of EDDS can be found in Neal and Rose, Stereospecific Ligands and Their Complexes of Ethylenediaminediscuccinic Acid, Inorganic Chemistry, Vol 7 (1968), pp. 2405-2412.
• carboxylates and other chelanting agents which are suitable for use in the present invention are given below.
• the polymers and co-polymers of the present invention may be chosen from a wide range of organic polymers, some of which also may function as builders to improve detergency. Included among such polymers may be mentioned sodium carboxy-lower alkyl celluloses, sodium lower alkyl celluloses and sodium hydroxy-lower alkyl celluloses, such as sodium carboxymethyl cellulose, sodium methyl cellulose and sodium hydroxypropyl cellulose, polyacrylates, polyaspartates and various copolymers, such as those of maleic and acrylic acids. Molecular weights for such polymers vary widely but most are within the range of 2,000 to 100,000.
• Polymeric polycarboxyate builders are set forth in U.S. Patent 3,308,067, Diehl, issued March 7, 1967. Such materials include the water-soluble salts of homo-and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylenemalonic acid.
• copolymers of maleic and acrylic acid having a molecular weight of from 2000 to 100000, carboxymethyl cellulose and mixtures thereof.
• Optional ingredients in the spray dried powder of the present invention are cationic surfactants.
• Useful cationic surfactants include water-soluble quaternary ammonium compounds of the form R4R5R6R7N+X ⁇ , wherein R4 is alkyl having from 10 to 20, preferably from 12-18 carbon atoms, and R5 is C1 to C20, R6 and R7 are each C1 to C7 alkyl preferably methyl; X ⁇ is an anion, e.g. chloride.
• Examples of such trimethyl ammonium compounds include C12 ⁇ 14 alkyl trimethyl ammonium chloride, C12 ⁇ 14 alkyl dimethyl ethoxy ammonium chloride and C12 ⁇ 14 alkyl trimethyl ammonium methosulfate.
• An essential step of the process of making the spray-dried powder of the present invention is the preparation of the complex of the chelating agent with the metal ion. Preferably this is done by dissolving a salt of the metal ion into a solution of the chelating agent in the required ratios.
• the molar ratio of metal ion to chelating agent is preferably at least 1:1, the present invention allows molar ratios of greater than 3:1 to be prepared, most preferred is a molar ratio of about 5:1. Whilst any metal salt may be used, magnesium sulphate is most preferred.
• the anionic polymer is added to the solution comprising the complex together with any other optional ingredients.
• the resulting slurry or solution is then spray dried by conventional means.
• the most preferred method for spray drying is the use of spinning disc atomiser.
• the free-flowing spray-dried powder is admixed with other detergent powders to form a finished granular detergent product. It is an important advantage of the present invention that the spray-dried powder dissolves rapidly in water to release the chelating agent and polymer as early as possible into the washing process.
• Components of the finished detergent composition may be chosen from a very wide range of detergent active materials. Common examples include surfactants, builders, bleach, bleach activator, enzymes, optical brighteners, soil release polymers, dye transfer inhibiting agents, softening clay, perfume, etc.
• the spray-dried powder of the present invention may be further processed, for example by additional granulation, agglomeration, compaction steps.
• a particularly preferred process is described in EP 508543, published on 14th October, 1992.
• a process is disclosed for structuring or "conditioning" a high active surfactant paste and then granulating in the presence of detergent powder.
• the spray-dried powder may be a component either of the conditioning step, or of the granulation step, or of both steps.
• Using this process in combination with the spray-dried powder of the present invention enables free-flowing detergent granulates to be produced having a surfactant content of at least 40% by weight, and a bulk density of at least 600 g/l.
• the composition was prepared by mixing a 40% active solution of the sodium salt of the copolymer, a 25% active solution of the phosphonic acid and the sulphate powder (MgSO4 . 7 H2O) to give a slurry.
• the slurry was then processed through a continuous spray dryer with co-current air inlet and a rotating disc (15000 rpm) at the top of the tower. After the exit from the bottom of the tower, two fluid beds in series provide further drying and cooling of the spray dried product.
• the resulting spray dried powder had a bulk density of 450 g/l (measured by the repour cup method).
• the resulting powder is free flowing and has a bulk density of 460 g/l.
• the resulting powder is free flowing and has a bulk density of 450 g/L.
• the resulting powder is free flowing and has a bulk density of 430g/L.

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

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Publications (1)

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Cited By (9)

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• 1994
  • 1994-04-20 EP EP94201092A patent/EP0678572A1/de not_active Ceased
• 1995
  • 1995-04-20 PE PE26682295A patent/PE996A1/es not_active Application Discontinuation
  • 1995-04-20 AU AU24602/95A patent/AU2460295A/en not_active Abandoned
  • 1995-04-20 BR BR9507326A patent/BR9507326A/pt not_active Application Discontinuation
  • 1995-04-20 WO PCT/US1995/004799 patent/WO1995029216A1/en not_active Ceased
  • 1995-04-20 CA CA 2187517 patent/CA2187517A1/en not_active Abandoned
  • 1995-04-20 JP JP7527734A patent/JPH09512300A/ja active Pending
  • 1995-04-20 CN CN 95193528 patent/CN1150450A/zh active Pending
  • 1995-07-19 TW TW084107455A patent/TW341597B/zh active

Patent Citations (6)

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