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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/66—Non-ionic compounds
  • C11D1/662—Carbohydrates or derivatives
• • 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
  • C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/66—Non-ionic compounds
  • C11D1/83—Mixtures of non-ionic with anionic 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
  • C11D11/0082—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
  • C11D11/0088—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 the liquefied ingredients being sprayed or adsorbed onto solid particles
• • 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
  • C11D17/0034—Fixed on a solid conventional detergent ingredient
• • 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
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
  • C11D17/065—High-density particulate detergent 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
  • 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
  • C11D3/2082—Polycarboxylic acids-salts thereof
• • 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 process for the production of concentrated surfactant granules Active substance content of more than 45 wt .-%, based on the granules, which a low hygroscopicity, a significantly improved silage capacity and an increased Have bulk density.
• Granulation is an alternative to spray drying surfactant pastes describes EP-B-0 603 207 (Henkel) a process for the production of washing and cleaning active Surfactant granules with a bulk density above 500 g / l by simultaneous Granulation and drying in all devices where there is granulation can be carried out with simultaneous drying.
• a surfactant preparation form which is a non-surfactant liquid component (usually water) has, if desired granulated with the addition of a solid component and dried at the same time.
• the simultaneous spraying also provides of active substance and carrier component solution through one and the same nozzle here is a possible but not a mandatory process parameter.
• the object of the invention was to provide a method for producing heavy, free-flowing, to provide highly concentrated surfactant granules with bulk densities above 600 g / l, the granules obtained have advantages in terms of ensiling ability and Show hygroscopicity.
• the process according to the invention has the advantage that the resulting grain is conditional due to the inclusion of surfactant phases in phases of the carrier material, an increased mechanical Stability and an extremely reduced water absorption during storage.
• the granules obtained by the process according to the invention are accordingly very easy to pour and ensilage and stick together due to their low tendency to absorb water.
• the product is a carrier paste in the granulating unit even at low surfactant concentrations sticky and cakes on drying, adding the products are hygroscopic and stick in the course of heavy water absorption.
• the solutions of the active substance and the carrier substance are carried out according to the invention one and the same nozzle atomized.
• the solutions can only be in the nozzle with each other mixed, i.e. supplied to the nozzle via separate storage containers and feed lines but also a mixture of both solutions from a single storage container can be injected through a nozzle.
• the non-surfactant solvent which may contain one or more components, has a boiling point or boiling range preferably below normal pressure 250 ° C and especially below 200 ° C. With particular advantage, it contains components which boil between 60 and 180 ° C at normal pressure.
• Organic constituents of the non-surfactant solvent are preferably mono- and / or polyfunctional alcohols, for example methanol, ethanol, propanol, Isopropanol, butanol, secondary and tertiary butanol, pentanol, ethylene glycol, 1,2-propanediol, Glycerin or mixtures of these are used.
• an inorganic component of the non-surfactant Solvent water optionally together with organic components such as ethanol, 1,2-propanediol or glycerin.
• the share is of the water preferably 25 to 80 wt .-%, based on the total amount of non-surfactant solvent.
• the solutions of surfactants and carrier materials in Non-surfactant solvents can be used in a wide range of concentrations are taken into account, with only a viscosity that is still suitable for atomization got to.
• the proportion of the non-surfactant is Solvent 30 to 70 wt .-% and in particular 45 to 60 wt .-%.
• alkylbenzenesulfonates ABS
• alkylpolyglycosides APG
• surfactants Either alkylbenzenesulfonates (ABS) or alkylpolyglycosides (APG) or mixtures of these are used as surfactants.
• Advantageously used alkylbenzenesulfonates have a chain length of 9 to 13 carbon atoms, but almost pure C 12 -alkylbenzenesulfonate can also be used with preference.
• the alkyl or alkenylglycosides have the general formula RO- (G) x , in which R is one primary, straight-chain or in the 2-position methyl branched aliphatic radical having 8 to 22, preferably 12 to 18 carbon atoms, G is a symbol which represents a glucose unit having 5 or 6 carbon atoms, and the degree of oligomerization x between 1 and 10, preferably between 1 and 2 and in particular is significantly smaller than 1.4.
• ABS and / or APG surfactants in addition to the ABS and / or APG surfactants also other anionic, nonionic, cationic or amphoteric surfactants can be used in combination with the former. While the process is mainly used to manufacture ABS and / or APG compounds suitable are additions of up to 20% by weight of other surfactants, based on the total amount of surfactant, possible without losing the advantages of the method according to the invention.
• the carrier materials used in the process according to the invention can be inorganic and / or organic in nature.
• they consist of amorphous alkali silicates of the formula (SiO 2 ) m (M 2 O) n1 (so-called water glasses) and / or crystalline layered silicates of the formula (SiO 2 ) m ((M 2 O) n2 (H 2 O ) x , where M is lithium, sodium or potassium, m and n1 are integers or fractional numbers greater than 0, n2 is 1 and x is 0 or integers from 1 to 20.
• inorganic salts or organic polycarboxylates are used into consideration.
• sodium carbonate is among the inorganic salts preferred, while as polycarboxylates preferably citric acid / citrates and / or Acrylic acid / maleic acid copolymers are used.
• the detergent granules which are active in washing and cleaning, have, based on the finished granulate, Carrier material contents of 10 to 50 wt .-%. Because highly concentrated surfactant granules Preferred for economic reasons are carrier material contents from below 40, in particular below 30% by weight, is preferred. In addition to the so-called over-dried Water glasses can also be found in preferred embodiments of the invention Sodium carbonate, acrylic acid / maleic acid copolymers and trisodium citrate as carrier materials Use. Mixtures of the carrier substances are also preferred, in particular Carbonate / silicate mixtures as well as citrate / silicate mixtures.
• the surfactant preparation form is granulated and dried, according to the invention
• Process granulate particles are obtained in which the active substance is partially enclosed by the carrier. Under drying, this becomes partially or completely remove the non-surfactant solvent.
• the non-surfactant solvent is preferably removed almost completely.
• the preparation of the surfactant granules can be done in all devices take place in which a granulation under drying conditions can be carried out. Examples include heated mixers and granulators, especially high-speed ring mix dryers such as Turbo dryer® granulators (Device from Vomm, Italy). In a preferred embodiment, the Invention, however, that the combination of the two process steps in a batch or continuously running fluidized bed is carried out. It is special preferred to carry out the process continuously in the fluidized bed.
• the surfactant preparation form is introduced into the fluidized bed from a common nozzle. The mixture of the two liquid to pasty components of the surfactant preparation form can be done beforehand or only in the nozzle.
• Fluid bed apparatuses used have base plates with dimensions of at least 0.4 m.
• fluidized bed apparatuses which have a base plate are preferred have a diameter between 0.4 and 5 m, for example 1.2 m or 2.5 m.
• fluidized bed apparatuses are also suitable which have a base plate with a have a diameter greater than 5 m.
• a perforated base plate is preferably used as the base plate or a Conidur plate (commercial product from Hein & Lehmann, Federal Republic Germany).
• the method according to the invention is preferred at vortex air speeds between 1 and 8 m / s and in particular between 1.5 and 5.5 m / s performed.
• the granules are discharged from the fluidized bed advantageously via a size classification of the granules.
• This classification can for example with a screening device or through an opposed air flow (Classifier air), which is regulated so that only particles above a certain particle size removed from the fluidized bed and smaller particles retained in the fluidized bed will.
• Classifier air which is regulated so that only particles above a certain particle size removed from the fluidized bed and smaller particles retained in the fluidized bed will.
• the inflowing settles Air from the heated or unheated classifier air and the heated soil air together.
• the soil air temperature is preferably between 80 and 400 ° C, in particular between 90 and 350 ° C.
• the vortex air cools down due to heat loss and by the heat of vaporization of the components of the non-surfactant solvent from.
• the temperature of the fluidizing air is about 5 cm above the base plate 60 to 120 ° C, preferably 65 to 90 ° C and especially 70 to 85 ° C.
• the air outlet temperature is preferably between 60 and 120 ° C, especially below 100 ° C and with particular advantage between 70 and 85 ° C.
• the evaporate Parts or all of the non-surfactant solvent, the dried-on to dry germs with additional amounts of surfactant preparation are encased in such a way that the carrier substance is the active substance envelops.
• This special structure of the granulate, which can only be achieved by simultaneous injection Obtain active substance and carrier material solution through one and the same nozzle is the result of the evaporating non-surfactant solvent in the evaporation process
• Backing material from the freshly condensed layer on the grain contributes and deposits on the surface of the grain upon evaporation.
• a powdering agent preferably zeolite or sodium carbonate
• these powdering agents reduce the amount of granulation the stickiness of the moist granules and thus promote turbulence and drying to the desired product.
• this variant can be advantageous is, however, not absolutely necessary to carry out the invention.
• the process according to the invention results in surfactant granules which dissolve easily in cold water without being hygroscopic.
• the granules have high mechanical stability and thus excellent flow and silage properties. Leave with organic solvents that do not destroy the grain structure only small amounts of active substance dissolve from the uncrushed granules, while most of the active substance can be extracted from the ground granules is.
• the washing and cleaning active produced by the inventive method Surfactant granules have bulk densities above 600 g / l. They are ideal as components suitable for the production of detergents and cleaning agents, preferred Detergents and cleaning agents which are produced by the process according to the invention detergent granules active in washing and cleaning in amounts of more than 10% by weight, in particular in amounts above 20 wt .-%, based on the total washing and Detergent included.
• a bulk density according to the invention Process produced washing and cleaning active surfactant granules above of 700 g / l, in particular above 800 g / l, is preferred.
• the process according to the invention can advantageously be active in washing and cleaning Surfactant granules are produced, the total surfactant content, based on the total granulate is more than 40% by weight.
• Surfactant contents above 50% by weight and in particular above 60% by weight are preferred.
• ABS alkylbenzenesulfonate
• APG alkylpolyglycoside
• the process is suitable for the production of highly concentrated surfactant granules and has particular advantages if the surfactants to be processed are sticky per se Are natural, as is the case with alkylbenzenesulfonates and alkylpolyglycosides.
• the proportion of other surfactants is 20% by weight, based on the total surfactant content, does not exceed in the granules according to the invention.
• composition [% by weight] E1 E2 E3 E4 E5 E6 E7 E8 SECTION 45 - - - 60 50 - 61 APG - 67 80 50 - - 62 - silicate 21 22 17.5 10th 13 15 - - Sokalan CP5® - - - - - 33 - Sodium citrate - - - - - - - 14 sodium 28 - - 35 - - - - Zeolite - - - - 22 30th - 20th water 6 11 2.5 5 5 5 5 5 5
• Sokalan CP5 ® is an acrylic acid-maleic acid copolymer from BASF
• solubilities of E1 and E2 were determined by adding 5 g each of the agent to a 1 liter vessel containing 500 ml of demineralized water which was stirred by a propeller stirrer at 900 rpm. The conductivity was detected via a conductivity measuring cell and recorded on a recorder. The measurement was carried out until no increase was ascertainable. The time to reach the conductivity of the agent was set to 100%, the corresponding other dissolving times were calculated. Solubility test E1 E2 95% solved [min] 2.59 2.57 90% solved [min] 2.27 2.25 80% solved [min] 1.45 1.48 Residue after 1.5 min [% by weight] 2nd 5 Residue after 5 min [% by weight] 0 0 0
• All compounds E1 to E8 produced according to the invention can be stored in the air without sticking or losing their free-flowing properties.
• a comparison test between E5 and a commercially available comparable ABS compound with a bulk density of 400 g / l and an active substance content of 85% by weight gave the following values after 8 hours of storage (55% relative luminous humidity): Hygroscopicity (8-hour storage trial) E5 comparison Water absorption [% by weight] 5 20th Remarks free-flowing Bonding
• ABS / APG compounds produced according to the invention are ideal additives suitable for detergents because they give the detergents improved solubility.

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• Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
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• Oil, Petroleum & Natural Gas (AREA)
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• Organic Chemistry (AREA)
• Health & Medical Sciences (AREA)
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• Molecular Biology (AREA)
• Detergent Compositions (AREA)

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• 1997
  • 1997-01-27 DE DE19702845A patent/DE19702845A1/de not_active Withdrawn
• 1998
  • 1998-01-17 AT AT98100768T patent/ATE253107T1/de not_active IP Right Cessation
  • 1998-01-17 EP EP98100768A patent/EP0859048B1/fr not_active Expired - Lifetime
  • 1998-01-17 ES ES98100768T patent/ES2210601T3/es not_active Expired - Lifetime
  • 1998-01-17 DE DE59809988T patent/DE59809988D1/de not_active Expired - Lifetime

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