EP1491619B1 - Verfahren zur Herstellung von Tensiden - Google Patents

Verfahren zur Herstellung von Tensiden Download PDF

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Publication number
EP1491619B1
EP1491619B1 EP03019852A EP03019852A EP1491619B1 EP 1491619 B1 EP1491619 B1 EP 1491619B1 EP 03019852 A EP03019852 A EP 03019852A EP 03019852 A EP03019852 A EP 03019852A EP 1491619 B1 EP1491619 B1 EP 1491619B1
Authority
EP
European Patent Office
Prior art keywords
agents
process according
precipitate
sodium
sodium laurel
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
Application number
EP03019852A
Other languages
English (en)
French (fr)
Other versions
EP1491619A1 (de
Inventor
Jagdish Pawar
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jp Laboratories Pvtltd
Original Assignee
Jp Laboratories Pvtltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to ES03019852T priority Critical patent/ES2238657T3/es
Priority to AT03019852T priority patent/ATE286531T1/de
Priority to PT03019852T priority patent/PT1491619E/pt
Priority to EP03019852A priority patent/EP1491619B1/de
Priority to DE60300259T priority patent/DE60300259T2/de
Priority to DK03019852T priority patent/DK1491619T3/da
Priority to SI200330025T priority patent/SI1491619T1/xx
Priority to EP04024858A priority patent/EP1586630A1/de
Application filed by Jp Laboratories Pvtltd filed Critical Jp Laboratories Pvtltd
Publication of EP1491619A1 publication Critical patent/EP1491619A1/de
Application granted granted Critical
Publication of EP1491619B1 publication Critical patent/EP1491619B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/146—Sulfuric acid esters
    • 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

Definitions

  • THE PRESENT INVENTION relates to cleaning compositions, and more particularly to processes for preparing granular detergent compositions having relatively high bulk density.
  • the second type of process involves dry mixing the detergent components, and subsequently agglomerating the dry-mixed components in a high or medium speed mixer/densifier, typically in the presence of a liquid binder, such as water, a non-ionic or an anionic surfactant.
  • a liquid binder such as water, a non-ionic or an anionic surfactant.
  • spray-dried detergent compositions have been found to have relatively low bulk density.
  • Spray-drying processes require expensive and complicated machinery and involve relatively high energy consumption.
  • spray-drying processes typically result in the production of fine particles of the detergent composition, with the associated problems with regard to air pollution.
  • Detergent compositions having medium to high bulk densities have been produced by dry-mix agglomeration processes.
  • detergents produced by such dry-mix processes have been found to suffer from a number of problems, including poor dispersion properties and unsatisfactory detergent performance, as discussed in US 6,303,558. Dry-mix processes also require the use of hi-tech mixer/densifier equipment.
  • granular cleaning compositions having a relatively high bulk density may be prepared by a process involving adding water-soluble salts to an aqueous solution of sodium laurel sulphate.
  • the process disclosed herein allows the preparation of a granular cleaning composition without the requirement for expensive spray-drying or mixer/densifier equipment.
  • a process for the production of a high bulk density granular detergent composition or component having a bulk density of at least 500 g/l comprising the steps of;
  • At least one water-soluble salt is chosen from the group consisting of potassium nitrate, potassium chloride, potassium acetate, sodium acetate, sodium chloride, barium chloride, or any combination thereof.
  • At least one water-soluble salt is a sea salt.
  • step (iii) the separation of the precipitate in step (iii) is effected with a filtration apparatus or centrifuge.
  • the separation of the precipitate is effected with a filter press.
  • the product may be dried in step (iv) in a fluid bed dryer, drum vacuum dryer, tray dryer, or any combination thereof.
  • one or more additives may be advantageously added to the separated precipitate formed in step (iii) before drying, to form detergents or cleaning compositions having desired properties.
  • one or more of the additives are chosen from the group consisting of detergency builders, fillers, acid powders, alkali powders, binders, bleaches, bleach activators, fluorescers, anti-tarnish agents, anti-corrosion agents, soil-suspending agents, soil-release agents, germicides, Ph adjusting agents, chelating agent, clays, coating agents, enzymes, enzyme stabilising agents or any combination thereof.
  • Preferred additives include acid powders and alkali powders.
  • the process described herein allows the preparation of relatively high bulk density granular surfactant, detergent or cleaning compositions, without the need for expensive spray-drying, or mixer/densifier equipment.
  • the present invention is concerned with the preparation of a relatively high bulk density detergent composition or component by means of a precipitation process which involves the addition of a water-soluble salt to an aqueous sodium laurel sulphate solution.
  • SLS Sodium Laurel Sulphate
  • the aqueous SLS solution according to the process of the present invention preferably has a concentration of 5 to 40% (w/v),preferably 10 to 35% (w/v) and more preferably 20 to 30% (w/v).
  • the aqueous SLS solution for use in the present process may be prepared by any suitable method. Suitable methods for the preparation of the aqueous SLS solution will be evident to the person skilled in the art, with respect to the particular surfactant selected.
  • the aqueous SLS solution may conveniently, be prepared by a sulphonation process. Suitable conditions for carrying out such a sulphonation process will be known to the person skilled in the art.
  • the sulphonation process may be either a continuous or batch type processes. Continuous sulphonation processes will typically produce aqueous solution of Sodium Laurel Sulphate with a concentration of around 70% (w/v). Batch processes will typically produce an aqueous solutions with a lower concentration of Sodium Laurel Sulphate, typically around 30% to 60% (w/v). Concentrated aqueous solution of Sodium Laurel Sulphate produced in this way can then be diluted to the desired concentration for use in the present process.
  • the concentrated aqueous solution of Sodium Laurel Sulphate may be prepared in-situ, or is readily available from manufacturers. Alternative methods for the production of aqueous solution of Sodium Laurel Sulphate will be evident to the person skilled in the art.
  • salts contemplated for use in this step include organic and inorganic salts.
  • the amount of salt to be added to the aqueous solution of SLS must be an amount sufficient to effect precipitation of the SLS from solution.
  • the amount of salt required to effect precipitation in any given case can be easily determined be the person skilled in the art using standard procedures.
  • the surfactant Sodium Laurel Sulphate is highly soluble in water, but only poorly soluble in aqueous salt solution. It has been found that increasing the concentration of salt in the aqueous solution results in decrease in the solubility of the surfactant compound. With respect to the surfactant Sodium Laurel Sulphate, it has been observed that Sodium Laurel Sulphate is slightly soluble in an aqueous salt solution having a salt concentration of up to about 3% (w/v), and is progressively more insoluble on increase of the salt concentration. It has been observed that Sodium Laurel Sulphate is almost completely insoluble in an aqueous salt solution having a salt concentration of 5% (w/v).
  • the amount of salt added may usefully be an amount to provide aqueous solution having a salt concentration of 5% (w/v) or more, preferably 10% (w/v) or more.
  • the salt may conveniently be added to the aqueous solution of SLS at room temperature.
  • the aqueous solution is mixed or agitated on addition of the salt.
  • Preferred salts for use in the process include potassium nitrate, potassium chloride, barium chloride, sodium chloride, sodium acetate, potassium acetate or combinations thereof. It has been found that variation of the salt added to the aqueous solution of Sodium Laurel Sulphate, results in variations in the physical characteristics, e.g. density, particle size, shape and form of the resultant granular product.
  • One or more salts may be used to obtain desired particle size, density, shape and form.
  • Particularly preferred salts for use in the process include salts from natural sea water.
  • Sea salts contain a mixture of natural salts, the major component being sodium chloride. It has been found that granular product having a bulk density of over 500 g/l can be achieved using sea salts. Sea salts have the advantages of being cheap and readily available by evaporation of sea water.
  • the particular method used for separating the surfactant precipitate is not important. Any simple separation method may conveniently be used, for example, filtration methods e.g. filter press, vacuum filtration, or with a centrifuge.
  • filtration methods e.g. filter press, vacuum filtration, or with a centrifuge.
  • the use of a filter press is particularly suitable for producing a separated precipitate having a low moisture content.
  • the separated precipitate preferably has a moisture content of 5% to 35% (w/w).
  • the aqueous salt solution can be concentrated and the salts recovered by known methods.
  • simple solar evaporation methods can be conveniently be used for recovery of many salts, particularly where sea salts are used. In this way the salt solution by-product can be recycled, with the associated economic and environmental advantages.
  • one or more additives may be added to the separated SLS precipitate before drying.
  • high density powders, liquid additives or fillers which can be added to produce detergent compositions having a higher bulk density than dried granules of surfactant composition alone, for instance to obtain granules with a high bulk density of over 700g/l, and/or to provide variation in the particle size, form or shape of the resultant granular detergent product.
  • acidic powders such as Picric acid, para toluene sulphonic acid and/or alkaline powders, such as sodium carbonate, or sodium bicarbonate, can be added to enhance the dissolution and foaming properties of the detergent composition. It has been found that, where a mixture of alkaline and acidic powders are added, as additives, the product detergent composition liberates carbon dioxide gas in aqueous media, improving the solubility and dispersion properties of the detergent composition.
  • any standard detergent additives can be added to provide granular detergent composition having desired properties.
  • Preferred additives include fillers, detergency, builders, acid powders, alkali powders, binders, bleaches, bleach activators, fluorescer anti-tarnish agents, anti-corrosion agents, soil-suspending agents, soil-release agents, germicides, Ph adjusting agents, chelating agents, clays, coating agents, enzymes, enzyme stabilising agents or any combination thereof.
  • Other suitable additives will be well known to the person skilled in the art.
  • Drying of the product in step (iv) can be carried out in any simple dryer.
  • suitable simple dryers include fluid bed dryers, tray dryers or drum vacuum dryers.
  • Other suitable dryers will be known to the skilled person. It has been found that granular product having a moisture content in the range of 0.5%-2% (w/w) can be achieved using a vacuum dryer.
  • Drying the wet-cake of surfactant in this manner requires a considerable lower energy consumption than that used in many conventional processes for the drying of surfactant slurry or aqueous solution (e.g spray-dry methods).
  • the process according to the present invention allows the production of high bulk density granular free-flowing detergent component or composition having a bulk density of at least 500 g/l.
  • the process of the invention provides an economic and efficient method for the preparation of high bulk density, free-flowing granular detergent compositions.
  • the process allows the production of granular products having a range of desired bulk densities, particle sizes, shapes and forms, which can be used in a variety of detergent and cleaning composition applications.
  • the process of the invention can be used to provide granules of Sodium Laurel Sulphate having a bulk density in the range of between 500 to 710 g/l.
  • the process of the present invention avoids the need for complicated and expensive equipment, and provides an economical and energy-efficient process for the manufacture of low dosage volume, compact granular surfactant and detergent compositions. Additionally the aqueous salt solution by-product produced in the process of the present invention as described can be recycled, recovering the corresponding salts.
  • Example 2 The process was carried out as in Example 1 with the addition of the different salts as shown in Table 1 below to 100ml of 20% (w/v) solution of Sodium Laurel Sulphate: Salt (10g) Bulk density of granules (g/l) Potassium nitrate 700 Potassium chloride 680 Potassium acetate 620 Sodium acetate 590 Sodium chloride 550

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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)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Claims (8)

  1. Verfahren zur Herstellung einer körnigen Reinigungsmittelzusammensetzung oder komponente mit einer Schüttdichte von wenigstens 500 g/l, das die Schritte umfasst:
    (i) Bereitstellen einer wässrigen Lösung von Natriumlaurelsulfat,
    (ii) Zugeben eines oder mehrerer wasserlöslicher Salze zur wässrigen Natriumlaurelsulfat-Lösung, um das Natriumlaurelsulfat auszufällen,
    (iii) Abtrennen des resultierenden Niederschlags und schließlich
    (iv) Trocknen des Produktes.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß wenigstens ein wasserlösliches Salz ausgewählt wird aus der Gruppe, die aus Kaliumnitrat, Kaliumchlorid, Kaliumacetat, Natriumacetat, Natriumchlorid oder irgendeiner Kombination davon besteht.
  3. Verfahren nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, daß wenigstens ein wasserlösliches Salz ein Meersalz ist.
  4. Verfahren nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, daß der Niederschlag in Schritt (iii) mit einer Filtrationsvorrichtung oder Zentrifuge abgetrennt wird.
  5. Verfahren nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, daß das Produkt in Schritt (iv) in einem Fließbetttrockner, Trommelvakuumtrockner, Hordentrockner oder irgendeiner Kombination davon getrocknet wird.
  6. Verfahren nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, daß es weiter den Schritt umfasst, daß ein oder mehrere Zusatzstoffe zum abgetrennten Niederschlag vor dem Trocknen hinzugefügt werden.
  7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß der eine oder die mehreren Zusatzstoffe ausgewählt werden aus der Gruppe, die aus Reinigungsmittel-Buildern, Füllstoffen, sauren Pulvern, alkalischen Pulvern, Bindemitteln, Bleichmitteln, Bleichaktivatoren, Aufhellern, Mitteln zur Verhinderung des Anlaufens, Mitteln zur Verhinderung der Korrosion, Mitteln zum Suspendieren von Schmutz, Mitteln zum Freisetzen von Schmutz, Germiziden, pH-Einstellungsmitteln, Chelatbildnern, Tonen, Beschichtungsmitteln, Enzymen, Enzymstabilisierungsmitteln oder irgendeiner Kombination davon besteht.
  8. Verfahren nach Anspruch 7, dadurch gekennzeichnet, daß die Zusatzstoffe ein saures Pulver und ein alkalisches Pulver einschließen.
EP03019852A 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden Expired - Lifetime EP1491619B1 (de)

Priority Applications (8)

Application Number Priority Date Filing Date Title
PT03019852T PT1491619E (pt) 2003-09-01 2003-09-01 Processo para preparar um detergente
EP03019852A EP1491619B1 (de) 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden
DE60300259T DE60300259T2 (de) 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden
DK03019852T DK1491619T3 (da) 2003-09-01 2003-09-01 Fremgangsmåde til fremstilling af en detergent
ES03019852T ES2238657T3 (es) 2003-09-01 2003-09-01 Proceso de preparacion de un detergente.
EP04024858A EP1586630A1 (de) 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden
SI200330025T SI1491619T1 (en) 2003-09-01 2003-09-01 Process for preparing a detergent
AT03019852T ATE286531T1 (de) 2003-09-01 2003-09-01 Verfahren zur herstellung von tensiden

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP03019852A EP1491619B1 (de) 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden

Related Child Applications (2)

Application Number Title Priority Date Filing Date
EP04024858A Division EP1586630A1 (de) 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden
EP04024858.5 Division-Into 2004-10-19

Publications (2)

Publication Number Publication Date
EP1491619A1 EP1491619A1 (de) 2004-12-29
EP1491619B1 true EP1491619B1 (de) 2005-01-05

Family

ID=33395901

Family Applications (2)

Application Number Title Priority Date Filing Date
EP03019852A Expired - Lifetime EP1491619B1 (de) 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden
EP04024858A Withdrawn EP1586630A1 (de) 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP04024858A Withdrawn EP1586630A1 (de) 2003-09-01 2003-09-01 Verfahren zur Herstellung von Tensiden

Country Status (7)

Country Link
EP (2) EP1491619B1 (de)
AT (1) ATE286531T1 (de)
DE (1) DE60300259T2 (de)
DK (1) DK1491619T3 (de)
ES (1) ES2238657T3 (de)
PT (1) PT1491619E (de)
SI (1) SI1491619T1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8080512B2 (en) 2004-12-23 2011-12-20 J P Laboratories Pvt. Ltd. Process for preparing a detergent

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2337552A (en) * 1940-08-15 1943-12-28 Du Pont Purification of saturated hydrocarbon sulphonic acids
DE1131662B (de) * 1960-12-23 1962-06-20 Leuna Iawalter Ulbrichtia Veb Verfahren zur Gewinnung fremdsalzarmer, oberflaechenwirksamer Alkylbenzolsulfonate
JPS62220597A (ja) * 1986-03-24 1987-09-28 花王株式会社 α−スルホ脂肪酸エステル塩の高濃度中和物の製造方法
JP2000109895A (ja) * 1998-10-01 2000-04-18 Futaba Kagaku:Kk 洗浄剤組成物

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8080512B2 (en) 2004-12-23 2011-12-20 J P Laboratories Pvt. Ltd. Process for preparing a detergent

Also Published As

Publication number Publication date
EP1586630A1 (de) 2005-10-19
DE60300259D1 (de) 2005-02-10
DE60300259T2 (de) 2005-12-15
ATE286531T1 (de) 2005-01-15
EP1491619A1 (de) 2004-12-29
SI1491619T1 (en) 2005-06-30
ES2238657T3 (es) 2005-09-01
PT1491619E (pt) 2005-05-31
DK1491619T3 (da) 2005-05-17

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