WO1998014548A2 - Procede de production d'un produit de nettoyage, notamment sous forme de poudre pour lave-vaisselle - Google Patents

Procede de production d'un produit de nettoyage, notamment sous forme de poudre pour lave-vaisselle Download PDF

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Publication number
WO1998014548A2
WO1998014548A2 PCT/DE1997/002254 DE9702254W WO9814548A2 WO 1998014548 A2 WO1998014548 A2 WO 1998014548A2 DE 9702254 W DE9702254 W DE 9702254W WO 9814548 A2 WO9814548 A2 WO 9814548A2
Authority
WO
WIPO (PCT)
Prior art keywords
soda
citric acid
detergent
polymer
reaction
Prior art date
Application number
PCT/DE1997/002254
Other languages
German (de)
English (en)
Other versions
WO1998014548A3 (fr
Inventor
Herbert Schmitz
Karl-Heinz Bonert
Frank Schneider
Original Assignee
Herbert Schmitz
Bonert Karl Heinz
Frank Schneider
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 claimed from DE1996140759 external-priority patent/DE19640759A1/de
Application filed by Herbert Schmitz, Bonert Karl Heinz, Frank Schneider filed Critical Herbert Schmitz
Priority to AU48619/97A priority Critical patent/AU4861997A/en
Publication of WO1998014548A2 publication Critical patent/WO1998014548A2/fr
Publication of WO1998014548A3 publication Critical patent/WO1998014548A3/fr

Links

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
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0052—Gas evolving or heat producing 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning 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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0073—Tablets
    • C11D17/0091—Dishwashing tablets
    • 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
    • C11D3/10—Carbonates ; Bicarbonates
    • 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
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2086—Hydroxy carboxylic acids-salts thereof

Definitions

  • the invention relates to a method for producing a cleaning agent, in particular a machine dish cleaner in powder form.
  • the method is also suitable, for example, for the production of a water softener, a stain remover or a detergent.
  • Dishwashers are now available in powder or tablet form as so-called "tabs". Modern machine dishwashers are low alkaline, chlorine-free and contain enzymes. To date, both phosphate-containing machine dish cleaners and phosphate-free machine dish cleaners are offered. Due to the risk of eutrophication of natural waters, there is a tendency towards phosphate-free machine dishwashers. Usual phosphate-free dishwashers contain 20 - 40% sodium citrate dihydrate, 10 - 30% soda, 0 - 40% bicarbonate, 0 - 20% silicate and 4 - 6% polymers. This
  • Components are also known as builders and represent about 85% of the detergent mass.
  • machine dishwashers contain 7-10% bleach, 1-2% TAED, 1-3% amylase, 1-3% protease, 1-3% nio-surfactants and 0-2% paraffin adducts.
  • the invention is based on the object of proposing a simple method for producing a cleaning agent, in particular a dishes cleaner.
  • This object is achieved with a process in which soda and citric acid are mixed intensively while removing heat in order to produce sodium hydrogen carbonate, sodium citrate and a portion of residual soda.
  • the reaction of the starting products with one another leads to a dust-dry product with a bulk density of about 700-900 g / 1, which is ideally processed with granulating aids to form a citrate compound granulate.
  • An advantageous procedure provides that the proportion of residual soda is kept below 20% GG, preferably below 15% GG.
  • the high conversion rate achieved thereby has a particularly advantageous effect on the cleaning agent produced.
  • Such a raw material compound can be classified as “non-irritating” since the sum of the "irritating" substances is less than 20%.
  • the batch process has the advantage that the combined quantities can be dosed precisely and the required quality aspect can thus be better taken into account.
  • citric acid When mixing soda and citric acid, it is suggested to add soda and spray in citric acid. It is advantageous if the citric acid is possibly injected through a nozzle on a moving mixing element, because this means that the mixing and addition of material take place at the optimum moment, both locally and in time.
  • a particularly good implementation is achieved when soda and citric acid are mixed with high shear forces, such as in a ploughshare mixer.
  • a ploughshare mixer with special cutter head inserts is particularly suitable.
  • the combination of batch process and ploughshare mixer makes it easier to maintain constant mixing ratios and defined bulk densities, since the components can be weighed precisely before mixing and the dwell time in the mixer has to be set according to the desired degree of conversion. The necessary parameters can therefore be varied slightly in order to achieve constant quality.
  • An advantageous way of temperature control in the reactor is that the heat is regulated or at least controlled by spraying in citric acid and / or cooling the reactor vessel.
  • the reaction be carried out in a container and the pressure in the container should be regulated. It has proven to be advantageous to apply a negative pressure in the container at the beginning of the reaction, which changes to an excess pressure during the reaction.
  • the resulting overpressure results from the resulting C0 2 .
  • the resulting C0 2 reacts with further mixing of the substances with the excess soda to bicarbonate, so that the pressure generated again decreases.
  • polymer is added when carrying out the process.
  • the polymer is preferably added in liquid form after the reaction between sodium carbonate and citric acid in order to agglomerate the resulting particles. If liquid polymer solutions are used during the process, a grain-stable, homogeneous detergent compound is created.
  • the polymer acts as a co-builder for the citrate-bicarbonate-soda builder system and bonds the dusting reaction product to particles of a defined particle size. These particles are so stable that separation of the cleaning agent produced is avoided even during transfer and transport processes.
  • Low molecular weight polymer is preferably used in a concentration which leads to 4-6% active polymer in the finished compound.
  • silicate is added after the reaction of soda with citric acid.
  • the silicate leads to a desired protective layer for sensitive decorations.
  • high silicate levels e.g. B. over 15% can, especially on glass, lead to an undesirable formation of deposits.
  • Silicate can be added dry after the reaction of soda with citric acid and, if necessary, after adding the polymer. This prevents a reaction between silicate and citric acid.
  • water glass ie a sodium silicate solution to the reaction mixture of citrate, bicarbonate and soda during the granulation, so that a granulate containing silicate is formed.
  • the builder system produced in this way is advantageously mixed with various other substances, such as bleach, TAED, amylase, protease, nonionic surfactants and paraffin adducts, and is marketed as a free-flowing powder or pressed into tabs.
  • the procedure for producing the builder system and a homogeneous mixture with the other substances leads to an easy-to-press product which is easy to tablet on the one hand and also easily soluble on the other.
  • the builder system is composed of a citrate compound and a silicate compound.
  • composition is suitable as a citrate compound (Citracomp plus):
  • Citracomp plus (copolymer) is created by granulating the base powder with a copolymer solution in a granulator.
  • a Lödige ploughshare mixer FKM 130 with knife head serves as the granulator.
  • 50 kg are introduced and 7.9 kg of copolymer H 40 (Stockhausen GmbH), 40%, are metered in over about 10 minutes.
  • the resulting product is dried in the fluidized bed at an air inlet temperature of 90 ° C for 13 minutes, taking care of a maximum product temperature of 60 ° C.
  • the resulting product has a sieve fraction of 5.9% above 1.7 mm, 93.5% between 0.2 and 1.7 mm and 0.6% below 0.2 mm.
  • a variant with disilicate is suitable as a silicate compound:
  • layered silicate e.g. SKS 6 from Hoechst AG
  • hydrogen carbonate bicarbonate
  • a polymer-free and silicate-free variant is particularly environmentally friendly.
  • the granulation is carried out, as in the other exemplary embodiments, in a Lödige ploughshare mixer FKM 130 with a knife head.
  • FKM 130 Lödige ploughshare mixer
  • 50 kg of base powder are introduced and then 8.65 kg of 20% aqueous solution of the base powder are metered in over about 10 minutes.
  • the resulting granulate is dried in the fluidized bed in a batch dryer at an air inlet temperature of 90 ° C for 20 minutes, taking care to ensure a maximum product temperature of 60 ° C.
  • a sieve fraction carried out resulted in 34% over 1.7 mm, 64% between 0.2 and 1.7 mm and 2% under 0.2 mm.
  • the granulation of the base powder with sodium silicate is carried out in a granulator.
  • a color protection polymer PVP polyvinyl pyrrolidone
  • PVP polyvinyl pyrrolidone
  • This PVP is added during granulation.
  • 15.7 kg of 30% PVP solution are added to 73.7 kg of base powder.
  • the granules are dried in the fluidized bed at an air inlet temperature of 90 ° C for 25 minutes, again ensuring a maximum product temperature of 60 ° C.
  • the resulting product has a composition of 52% sodium citrate dihydrate, 20% bicarbonate, 20% soda, 6% PVP and 2% residual moisture.
  • This special citrate compound with the color protection polymer PVP can be used 10 - 20% in color detergents.
  • Figure 1 schematically shows a mixer
  • FIG. 1 is a schematic of the method according to the invention.
  • the mixer 1 shown in FIG. 1 essentially consists of a mixer tank 2 with a tank 3 in which a ploughshare mixer 4 and special knife head inserts 5 are arranged (Lödige mixing reactor DVT 130).
  • Cutter head inserts 5 have nozzles 6 through which liquid can be sprayed into the mixer container 2 in the direction of the arrows 7, 8.
  • An air discharge 9 is arranged in the container wall 3, via which air 10 can be extracted from the mixing container 2.
  • the basic compound described is formed by the reactions in the reactor. This basic compound is removed from the reactor and in a granulator with granulating aids such. B. mixed liquid polymer without pressure and then dried on a fluidized bed. The dried granulate can be sold and transported.
  • the user can then mix this granulated compound with other additional ingredients such as bleach 15, enzymes 16, nonionic surfactants 17, TAED 18, etc., in order to ultimately press the product into so-called tabs 20 in a press 19.
  • additional ingredients such as bleach 15, enzymes 16, nonionic surfactants 17, TAED 18, etc.
  • the same machine dishwashing detergent can contain 10-17% disilicate bicarbonate polymer compound instead of the silicate and the compacted bicarbonate.
  • the described method is particularly inexpensive, since a large part of the cleaning agent is created directly from the particularly inexpensive raw materials, soda and citric acid, and the described method also offers the possibility of compiling different cleaning agent recipes according to individual requirements.

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

Abstract

On procède au mélange intensif de soude et d'acide citrique en évacuant la chaleur, selon un procédé discontinu, afin de produire du bicarbonate de sodium, du citrate de sodium et une partie de soude résiduelle, cette partie étant ensuite de préférence retraitée avec un polymère. On obtient ainsi un composé constituant un produit de nettoyage, pouvant être retraité d'une façon quelconque.
PCT/DE1997/002254 1996-10-02 1997-10-01 Procede de production d'un produit de nettoyage, notamment sous forme de poudre pour lave-vaisselle WO1998014548A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU48619/97A AU4861997A (en) 1996-10-02 1997-10-01 Method for producing a detergent, specially a powder detergent for dish washing machines

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE1996140759 DE19640759A1 (de) 1996-10-02 1996-10-02 Verfahren zur Herstellung eines Reinigungsmittels, insbesondere eines Maschinengeschirreinigers in Pulverform
DE19640759.1 1996-10-02
US6052797P 1997-09-30 1997-09-30
US60/060,527 1997-09-30

Publications (2)

Publication Number Publication Date
WO1998014548A2 true WO1998014548A2 (fr) 1998-04-09
WO1998014548A3 WO1998014548A3 (fr) 2000-08-24

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PCT/DE1997/002254 WO1998014548A2 (fr) 1996-10-02 1997-10-01 Procede de production d'un produit de nettoyage, notamment sous forme de poudre pour lave-vaisselle

Country Status (2)

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AU (1) AU4861997A (fr)
WO (1) WO1998014548A2 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0504091A1 (fr) * 1991-03-15 1992-09-16 Cleantabs A/S Composition pour le lavage machinal de la vaisselle sans phosphate
WO1992018596A1 (fr) * 1991-04-19 1992-10-29 The Procter & Gamble Company Compositions detersives granulaires pour lessive, presentant une solubilite amelioree
US5256327A (en) * 1991-08-01 1993-10-26 Shaklee Corporation Method of preparing a sequestering agent for a non-phosphate cleaning composition
EP0637628A2 (fr) * 1993-08-03 1995-02-08 Amway Corporation Procédé de mélange pour la formature de détergents
WO1997009411A1 (fr) * 1995-09-01 1997-03-13 Henkel Kommanditgesellschaft Auf Aktien Procede de preparation de produits granules precurseurs de detergents de faible alcalinite

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0504091A1 (fr) * 1991-03-15 1992-09-16 Cleantabs A/S Composition pour le lavage machinal de la vaisselle sans phosphate
WO1992018596A1 (fr) * 1991-04-19 1992-10-29 The Procter & Gamble Company Compositions detersives granulaires pour lessive, presentant une solubilite amelioree
US5256327A (en) * 1991-08-01 1993-10-26 Shaklee Corporation Method of preparing a sequestering agent for a non-phosphate cleaning composition
EP0637628A2 (fr) * 1993-08-03 1995-02-08 Amway Corporation Procédé de mélange pour la formature de détergents
WO1997009411A1 (fr) * 1995-09-01 1997-03-13 Henkel Kommanditgesellschaft Auf Aktien Procede de preparation de produits granules precurseurs de detergents de faible alcalinite

Also Published As

Publication number Publication date
AU4861997A (en) 1998-04-24
WO1998014548A3 (fr) 2000-08-24

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