EP0560799A1 - Solid washing agents. - Google Patents

Solid washing agents.

Info

Publication number
EP0560799A1
EP0560799A1 EP19910920111 EP91920111A EP0560799A1 EP 0560799 A1 EP0560799 A1 EP 0560799A1 EP 19910920111 EP19910920111 EP 19910920111 EP 91920111 A EP91920111 A EP 91920111A EP 0560799 A1 EP0560799 A1 EP 0560799A1
Authority
EP
European Patent Office
Prior art keywords
weight
sodium
parts
paste
wt
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.)
Granted
Application number
EP19910920111
Other languages
German (de)
French (fr)
Other versions
EP0560799B1 (en
Inventor
Guenther Panthel
Karl-Heinz Linde
Hermann Anzinger
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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 DE4038476 priority Critical
Priority to DE19904038476 priority patent/DE4038476A1/en
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Priority to PCT/EP1991/002212 priority patent/WO1992009676A1/en
Publication of EP0560799A1 publication Critical patent/EP0560799A1/en
Application granted granted Critical
Publication of EP0560799B1 publication Critical patent/EP0560799B1/en
Anticipated expiration legal-status Critical
Application status is Expired - Lifetime legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials characterised by their shape or physical properties
    • C11D17/06Powder; Flakes; Free-flowing mixtures; Sheets
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/146Sulfuric acid esters
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/0082Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste, melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials characterised by their shape or physical properties
    • C11D17/0047Detergents in the form of bars or tablets
    • C11D17/0065Solid detergents containing builders
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/12Water-insoluble compounds
    • C11D3/124Silicon containing, e.g. silica, silex, quartz, glass beads
    • C11D3/1246Silicates, e.g. diatomaceous earth
    • C11D3/128Aluminium silicates, e.g. zeolites

Abstract

On produit des détergents solides en mélangeant 100 parties en poids d'une pâte aqueuse contenant 40 à 60 % en poids de pâte de sulfate d'alkyle, à une température comprise entre 20 et 80 °C, avec: (a) 15 à 100 parties en poids d'un sel de sodium sélectionné dans le groupe formé par le sulfate, le carbonate et le silicate de sodium, et/ou avec (b) 10 à 300 parties en poids de silicate d'aluminium. of solid detergent is produced by mixing 100 parts by weight of an aqueous paste containing 40 to 60% by weight alkyl sulfate paste at a temperature between 20 and 80 ° C, with: (a) 15 to 100 parts by weight of a sodium salt selected from the group consisting of sulfate, carbonate and sodium silicate, and / or with (b) 10 to 300 parts by weight of aluminum silicate. Ensuite, on fragmente et/ou on pulvérise le produit solide ainsi obtenu, à une température comprise entre 20° et 60 °C. Then, fragments and / or pulverized solid product thus obtained, at a temperature between 20 ° and 60 ° C.

Description

solid detergent

Field of the Invention

The invention relates to solid detergent containing anion surfactants, sodium salts and / or aluminosilicates and a Ver¬ drive for their preparation.

S and the art

Alkyl sulfates (AS), which are industrially produced by sulfation pri¬ märer alcohols represent anionic surfactants which th Owing to their excellent Detergenseigenschaf- and their high biodegradability particularly for the production of detergents and cleaning agents are suitable.

Solid, ie, lumpy or pulverulent detergents, the alkyl sulfates, sodium sulfate and / or aluminosilicates th enthal¬ are, for. Example, from Japanese Patent Application JP 62/273 300 known.

They are prepared usually starts from aqueous alkyl sulphate dispersions ( "AS-pastes") having a solids content zwi¬'s 40 and 60 wt .-%, optionally from in admixture with other detergent ingredients, such as sodium sulphate, soda or aluminosilicates that be converted by spray drying into a solid, anhydrous, erförmige usually pul form. It is of particular importance that not only the processing but also the storage of the AS pastes at temperatures between 60 and 80 ° C must be carried out because the pastes solidify at lower temperatures and are no longer pumpable. Storage at higher temperatures Tempera¬ is connected to the serious disadvantage that partial hydrolysis of alkyl sulfates can take place to give alcohol and sulfuric acid, whereby the content of washing-active substance significantly reduced as a function of storage time.

Furthermore, an almost complete dewatering is erfor¬ sary for the production of powder-form detergents based on alkyl sulfates according to the methods of the prior art, which is associated with a high expenditure of energy and time. Finally, the narrow Temperaturinter¬ vall, the AS-pastes can be stored and processed within which a serious disadvantage with respect to the processing of most other anionic surfactant pastes are.

The object of the present invention was to develop solid washing agent based on alkyl sulfates, which are free of the disadvantages. Description of the Invention

The invention relates to solid detergent containing anionic surfactants, sodium salts and / or alumosilicates, the da¬ be obtained by that one at 20 to 80 ° C 100 parts by weight of a ring wä߬ 40 to 60 wt .-% by weight alkyl sulfate paste with

a) 15 to 100 parts by weight of a sodium salt selected from the group consisting of sodium sulfate, Natriu carbonate and sodium silicate is formed, and / or

b) 10 to 300 parts by weight of aluminosilicate

mixed and the solid obtained is then brought from 20 to 60 ° C in particulate form and / or pulverized.

Another object of the invention relates to a process for preparing solid detergent composition which characterized characterized aus¬ in that 100 parts by weight of an aqueous 40 to 60 wt .-% by weight alkyl sulfate paste at 20 to 80 ° C with

a) 15 to 100 parts by weight of a sodium salt selected from the group formed by sodium sulfate, sodium carbonate and sodium silicate, and / or

c) 10 to 300 parts by weight of aluminosilicate

mixed and the solid obtained is then brought from 20 to 60 ° C in particulate form and / or pulverized. It has surprisingly been found that leave the gelled plastic alkyl sulfate pastes even at room temperature over lead defined by the addition amounts of the above sodium salts and / or aluminosilicates in solid mixtures that be comminuted mechanically in spite of their high water content of up to 40 wt .-% and in bring particulate form or can be processed into free flowing powders. thus the erfindungsge¬ Permitted method has, in particular with regard to energy saving to a particular advantage over the spray technology of the prior art.

Alkyl sulfates are known substances which may be obtained by the üb¬ modern methods of preparative organic chemistry. The preferred method for their preparation starts from primary alcohols of natural or synthetic origin, which initially sulfated in known manner with gaseous sulfur trioxide and subsequently neutralized with aqueous bases. In this way is alkyl sulfate pastes have solids contents between 40 and 60 wt .-% was obtained, which have a gel-like consistency or solid are [J. Falbe (ed.), "Surfactants in Consumer Products", Springer Verlag, Berlin 1986 , p.67].

For the production of solid detergents alkyl sulfate pastes may preferably be used, in which the fat Alkylsul¬ 12 to 22, in particular 16 to 18 carbon atoms in the Älkylrest. Particularly preferred alkyl sulfate pastes are Cig / ig alkyl sulfate Na salt paste based on gehär¬ tetem tallow alcohol, the solid content of 40 to 60, more particularly sondere 50 to 55 wt .-% by weight. Under aluminosilicates, which can be used in the inventive process, compounds with unterschied¬ union proportions of AI2O3, and Si are (_2 to understand, in which the silicon is always surrounded tetrahedrally by 4 oxygen atoms, while aluminum is vor¬ in octahedral coordination. Come particular zeolites of this into consideration, the general formula (I)

M 2 / z O A1 2 0 3 x Si0 2 (I)

follow, in which M represents a mono- or polyvalent metal, z is the valence of the metal M and x is a number from 1.8 to 12. Preferred aluminosilicates are the zeolites of the type X, Y or L; particularly preferred is the use of zeolite A [DE-A-24 12 837] is. The zeolites may be aqueous slurries having a solids content of at least 50 wt .-% or in dry state are used in the form. By "dried zeolite" Such aluminosilicates are to be understood here that, although present as a dry powder, but still 20 to 50 wt .-% contain water of crystallization. For the purposes of the inventive mixtures verschie¬ Dener zeolites can be employed. For constitution of said compounds 117 (1986) is on ChiuZ, 2 i, verwie-

* • sen.

For the preparation of solid detergents according to the invention the liquid alkyl sulfate paste is initially mixed at temperatures of 20 to 80 ° C with the additives. based on 100 parts by weight of the aqueous alkyl sulfate paste of this 15 to 100, preferably 10 to 300, preferably 30 to 100 and in particular 50 to 75 parts by weight of the aqueous Alumosili cats admixed with 20 to 50 parts by weight of said sodium salts, and / or.

In the event that especially dry powder would receive should, it has been found advantageous to mix the Alkylsul¬ fat paste with sodium sulfate and aluminosilicate. In this case, it is optimal when the total amount of materials set Zu¬ 100 parts by weight - based on the alkyl sulfate paste - is not exceeded. The ratio of sodium sulfate and aluminosilicate is freely selectable within the specified limits.

The resulting solid can be mechanically comminuted at temperatures from 20 to 60 ° C, that is brought into particulate form, and / or- are pulverized. For this purpose are particularly crushers, mills, pelleting or extrusion machines costume in Be¬. In a preferred embodiment of the invention, the additives are first dispersed at 60 to 80 ° C in the liquid alkyl sulfate paste which was then transferred into a cooled extruder in which they temperatures to Tem¬ cools from 20 to 60 ° C. The solidified mixture may then be crushed easily.

The following examples are intended to illustrate the invention without limiting it. Examples

Example 1:

100 g of an aqueous 57 wt .-% strength Ci6 / 18 "Alk Y LSU lf at" Natr: L ~ to-salt paste (Cιs: Cιg ratio = 1: 1) were mixed at 80 ° C with 50 g of sodium sulfate , Then the Mi¬ was research in a screw press crushed with perforated front cover lens. In spite of the high water content of a solid, dry granulate was obtained.

Composition of the product; Alkyl sulfate Na salt: 38 wt .-% of sodium sulfate: 33 wt .-% water: 29 wt .-%

Example 2:

In 100 g of the aqueous alkyl sulfate paste from Example 1 75 g of zeolite A (Wessalith (R) P, a product of Messrs. Degussa, water content ca. 20 wt .-%) were stirred at 80 ° C. The liquid Michung was transferred to a water-cooled extruder in which it was cooled to solidification and brought into particulate form simultaneously. In spite of the high water content of a solid, dry granulate was obtained.

Composition of the product; Alkyl sulfate sodium salt; 33 wt .-% of zeolite A; 32 wt .-%

Water ; 35 wt .-% Example 3;

In 100 g of the aqueous alkyl sulfate paste of Example 1 were reacted at 80 ° C 50 g of zeolite A (Sasil (R), a product of Messrs. Henkel KGaA, water content ca. 50 wt .-%) is stirred and 75 g sodium sulfate. The mixture was cooled to 20 ° C where it solidified, and crushed into a powder mill. Despite the high water content was obtained .a dust-dry, non-tacky, free-flowing powder.

Composition of the product;

Alkyl sulfate Na salt: 25 wt .-%

Zeolite A: 11 wt .-%

Sodium sulfate: 33 wt .-%

Water: 31 wt .-%

Claims

claims
1. Solid detergents containing anionic surfactants, sodium salts and / or alumosilicates obtainable by mixing 100 parts by weight of an aqueous 40 to 60 wt .-% strength also alkyl sulfate paste at 20 to 80 ° C with
a) 15 to 100 parts by weight of a sodium salt ausge¬ selects the group of carbonate, sodium sulfate, sodium carbonate and sodium silicate is formed, and / or
b) 10 to 300 parts by weight of aluminosilicate
mixed and the solid obtained is then brought from 20 to 60 ° C in particulate form and / or pulveri¬ Siert.
2. A process for the preparation of pulverulent detergents comprising licate anionic surfactants, sodium salts and / or Alumosi¬, characterized in that 100 parts by weight of an aqueous 40 to 60 wt .-% by weight alkyl sulfate paste at 20 to 80 ° C and v
a) 15 to 100 parts by weight of a sodium salt ausge¬ selects the group of carbonate, sodium sulfate, sodium carbonate and sodium silicate is formed, and / or
b) mixing 10 to 300 parts by weight of alumosilicate and the solid obtained is then brought from 20 to 60 ° C in particulate form and / or pulveri¬ Siert.
3. A method according to claim 2, characterized in that ~ / Alkysulfat used as paste, an aqueous 40 to 60 wt .-% strength Cι i8-tallow alkyl sulfate Na salt paste.
4. The method according to at least one of claims 2 and 3, characterized in that is used as the aluminosilicate-containing zeolite A wasser¬.
5. A method according to any one of claims 2 to 4, characterized in that the additives are dispersed at 60 to 80 ° C in the alkyl sulfate paste which flüs¬ SiGe über¬ mixture into a water-cooled extruder, cooled therein until it solidifies and simultaneously crushed.
EP19910920111 1990-12-03 1991-11-25 Solid washing agents Expired - Lifetime EP0560799B1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE4038476 1990-12-03
DE19904038476 DE4038476A1 (en) 1990-12-03 1990-12-03 Prepn. of solid washing compsn. - by mixing aq. alkyl sulphate paste with sodium sulphate and/or aluminosilicate and shaping or grinding
PCT/EP1991/002212 WO1992009676A1 (en) 1990-12-03 1991-11-25 Solid washing agents

Publications (2)

Publication Number Publication Date
EP0560799A1 true EP0560799A1 (en) 1993-09-22
EP0560799B1 EP0560799B1 (en) 1995-05-31

Family

ID=6419459

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19910920111 Expired - Lifetime EP0560799B1 (en) 1990-12-03 1991-11-25 Solid washing agents

Country Status (8)

Country Link
US (1) US5399297A (en)
EP (1) EP0560799B1 (en)
JP (1) JPH06503107A (en)
AT (1) AT123300T (en)
DE (1) DE4038476A1 (en)
ES (1) ES2072629T3 (en)
MY (1) MY135771A (en)
WO (1) WO1992009676A1 (en)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6689305B1 (en) 1993-05-05 2004-02-10 Ecolab Inc. Process for consolidating particulate solids and cleaning products therefrom II
US5858299A (en) * 1993-05-05 1999-01-12 Ecolab, Inc. Process for consolidating particulate solids
DE4403323A1 (en) * 1993-09-23 1995-08-10 Henkel Kgaa Extruded detergents or cleaners with improved release properties
DE4415369C1 (en) * 1994-05-02 1995-08-31 Henkel Kgaa Heterogeneous surfactant granulate useful in washing powder and detergent
JP2958506B2 (en) * 1994-06-15 1999-10-06 花王株式会社 Method for producing a fine solid builder
DE19831707A1 (en) * 1998-07-15 2000-01-20 Henkel Kgaa Production of detergent or washing agent combining high hardness with rapid disintegration in use by method involving pre-mixing a fatty alcohol sulfate paste with the surfactant component in a granulator
DE19847280A1 (en) * 1998-10-14 2000-04-20 Henkel Kgaa Washing and cleaning tablets with Zeolithcompound
DE19909230A1 (en) * 1999-03-03 2000-09-07 Wolff Walsrode Ag A process for producing compacted free-flowing varnish raw materials
EP2154235A1 (en) * 2008-07-28 2010-02-17 The Procter and Gamble Company Process for preparing a detergent composition

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US2382165A (en) * 1945-08-14 Detergent briquette
US2382163A (en) * 1945-08-14 Detergent briquette
GB557593A (en) * 1942-06-18 1943-11-26 Ernst Stern A process of manufacturing detergents in cake or tablet form
US2412819A (en) * 1945-07-21 1946-12-17 Mathieson Alkali Works Inc Detergent briquette
BE498392A (en) * 1945-11-09
NL269436A (en) * 1960-09-23
AT330930B (en) * 1973-04-13 1976-07-26 Henkel & Cie Gmbh A process for the preparation of solid detergents or cleaners schuttfahigen with a content of calcium-binding substances
US4097418A (en) * 1975-10-06 1978-06-27 The Procter & Gamble Company Granular colored speckles
IN160448B (en) * 1982-12-07 1987-07-11 Albright & Wilson
JPS62273300A (en) * 1986-05-21 1987-11-27 Kao Corp Detergent composition
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US5152932A (en) * 1989-06-09 1992-10-06 The Procter & Gamble Company Formation of high active detergent granules using a continuous neutralization system
CA2017921C (en) * 1989-06-09 1995-05-16 John Michael Jolicoeur Formation of detergent granules by deagglomeration of detergent dough
US5045238A (en) * 1989-06-09 1991-09-03 The Procter & Gamble Company High active detergent particles which are dispersible in cold water
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Non-Patent Citations (1)

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Title
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Also Published As

Publication number Publication date
DE4038476A1 (en) 1992-06-04
AT123300T (en) 1995-06-15
WO1992009676A1 (en) 1992-06-11
EP0560799B1 (en) 1995-05-31
US5399297A (en) 1995-03-21
MY135771A (en) 2008-06-30
ES2072629T3 (en) 1995-07-16
JPH06503107A (en) 1994-04-07

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