ES2263162T3 - PROCEDURE FOR MANUFACTURING A HIGH DENSITY DETERGENT COMPOSITION FROM A TENSIOACTIVE PASTE CONTAINING A NON-WATER BINDER. - Google Patents

Abstract

THE INVENTION REFERS TO A PROCEDURE FOR PREPARING DETERGENT AGLOMERATES WITH A DENSITY OF AT LEAST 650 G / L. SUCH PROCEDURE INCLUDES THE FOLLOWING PHASES: (A) CONTINUOUSLY MIX A DETERGENT TENSIOACTIVE PASTE AND A DRY INITIATION DETERGENT MATERIAL, INSIDE A HIGH SPEED MIXER / DENSIFIER, TO OBTAIN THANK YOU, APPROX. 0.1 AND 50% P / P OF A NON-WATER BINDER, BETWEEN APPROX. 70 AND 95% P / P OF A DETERGENT VOLTAGE, BEING THE REST WATER, (B) MIXING THE DETERGENT AGLOMERATES IN A MODERATED SPEED MIXER / DENSIFIER, TO DENSIFY AND AGLOMER AGAINLY AGGREGATE THOSE; AND (C) DRY THESE DETERGENT AGLOMERATES, FORMING THE DETERGENT COMPOSITION OF HIGH DENSITY. SUCH PROCEDURE MAY INCLUDE ONE OR MORE ADDITIONAL PHASES, HOW TO ADD A COATING AGENT AFTER THE MODERATED SPEED MIXER / DENSIFIER PHASE, TO FACILITARY TO CONTROL THE AGLOMERATION.

Description

Procedure to manufacture a composition high density detergent from a surfactant paste that It contains a non-aqueous binder.

Field of the Invention

The present invention relates in a manner general to a process for manufacturing a detergent composition of high density. More particularly, the invention relates to a continuous process during which detergent agglomerates are manufactured high density feeding a surfactant paste with a non-aqueous binder and a dry adjuvant detergent material Initial to two mixers / densifiers positioned in series. He process produces a high density detergent composition with surprisingly improved flow properties that can be marketed as a "compact" or low detergent composition dosage.

Background of the invention

Recently there has been an interest considerable in the detergent industry by detergents for laundry "compact" and therefore low volume of dosage. To facilitate the production of these so-called Low dosage detergents numerous attempts have been made aimed at producing detergents of high apparent density of, for example, 650 g / l or higher. Low detergents Dosage is currently in great demand since they save resources and can be sold in small packages that result more comfortable for the consumer.

Basically there are two types of processes to manufacture granules or detergent powders. The first type of process consists of spray drying an aqueous detergent suspension in a spray drying tower to obtain granules high porosity detergents. In the second type of process the different detergent components are mixed dry and, at then, they agglomerate with a binder such as, e.g. eg a nonionic or anionic surfactant. In both types of processes the main factors that control the density of the granules resulting detergents are density, porosity and area surface of the different initial materials as well as their chemical composition. However, these parameters can only Modify within a limited range. Therefore, you can only achieve a significant increase in bulk density if additional steps are included in the process to densify the detergent granules.

Numerous attempts have been made in the art to provide processes that increase the density of the granules or detergent powders. Special attention has been given to the densification of spray-dried granules by post-tower treatment. Thus, for example, an attempt refers to a discontinuous process in which spray-dried powder detergents or granules containing sodium tripolyphosphate and sodium sulfate are densified and spheronized in a Marumerizer®. This apparatus comprises a practically horizontal, rough and rotating table that is located at the inner base of a practically vertical cylinder with smooth walls. This process, however, is practically a discontinuous process and, therefore, is less suitable for large-scale production of powder detergents. More recently, other attempts have been made to provide continuous processes that increase the density of the "post-tower" or spray-dried detergent granules. Typically, these processes require the use of a first apparatus for spraying or crushing the granules and a second apparatus for increasing the density of the granules pulverized by agglomeration. These processes only achieve the desired increase in density by treatment or densification of the "post-tower" or spray-dried granules.
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However, all processes previously mentioned refer basically to densification or to a Processing of other types of spray-dried granules. Currently, quantities and types of materials have been limited subjected to spray drying processes in the production of detergent granules. So, for example, it turns out difficult to achieve high levels of surfactant in the resulting detergent composition, characteristic that facilitates production of low dosage detergents. Thus, it would be desirable. have a production process for detergent compositions that did not have the limitations imposed by the techniques Conventional spray drying.

To this end, there are numerous process descriptions in the art that include the agglomeration of detergent compositions. Thus, for example, attempts have been made to agglomerate detergency builder additives by mixing zeolite and / or layered silicates in a mixer to obtain fluid agglomerates. Although such attempts suggest that their process can be used to manufacture detergent agglomerates, they do not provide a mechanism by which initial detergent materials in the form of pastes, liquids or dry materials can be agglomerated effectively to obtain fluid and friable high detergent agglomerates. density. In this sense, in the previous agglomeration processes there is ample room for improvement of the flow properties of the agglomerates produced. These flow properties, such as fluidity, friability, narrow particle size distribution and the like, are necessary in today's low-dose compact detergent products. In addition, the above agglomeration processes do not adequately take into account nor are they aimed at minimizing the need for recycling of excess size or insufficient size agglomerates obtained in the
process.

Therefore, there is still a need in the technique of having a continuous manufacturing process of a high density detergent composition from directly from initial detergent ingredients. Likewise there is still the need to have a process to produce a composition high density detergent of this type with flow properties improved and that minimizes the need for recycling. Finally, there is still a need for such a process make it more efficient and economical to facilitate production at Large scale of low dosage or compact detergents.

Prior art

The following references refer to the Densification of spray dried granules: Appel et al., US 5,133,924 (Lever); Bortolotti et al., US 5,160,657 (Lever); Johnson et al., GB-1,517,713 (Unilever); and Curtis, EP-451,894. The following references refer to the production of detergents by agglomeration: Beerse et al., US 5,108,646 (Procter &Gamble); Capeci et al., US 5,366,652 (Procter &Gamble); Hollingsworth and col., EP-351,937 (Unilever); and Swatling et al., US 5,205,958. In application WO 93/25378, describes an agglomeration process for numerous high granules Density for detergents.

Summary of the invention

The present invention covers the needs previously mentioned in the art providing a process that produces a high density detergent composition in the form of agglomerated directly from a surfactant paste and from Initial dry adjuvant detergent ingredients. Pasta surfactant contains a relatively low amount of water but maintains its transportability and processability properties at include a sufficient amount of non-aqueous polyethylene glycol that it has a melting temperature of 35 to 70 ° C, to which the formation of agglomerates with surprisingly flowing properties improved. By having these improved flow properties, the agglomerates produced by the process of the invention are less sticky and avoid having to recycle again in the process the agglomerated particles of excessive size as in the case of previous processes Once the process of the invention is finished the agglomerated particles of excessive size can be reduced by proper size using crushing processes more economical

Here, the expression "agglomerates" refers to particles formed by agglomeration of more porous initial detergent ingredients (particles) that typically have a median size of particles smaller than formed agglomerates. The percentages and the relationships used in the present invention are expressed as weight percentages (calculated as anhydrous substance) unless Specify otherwise. All viscosities mentioned in the This memory is measured at 70 ° C (± 5 ° C) and with a speed of friction of about 10 to 100 sec. -1.

According to one aspect of the invention, it is provided a process to prepare a friable and fluid detergent composition high density The process includes the steps of: (a) mixing of continuously form a detergent surfactant paste and a material initial dry detergent in a high mixer / densifier speed to obtain detergent agglomerates, where the paste surfactant includes, by weight of the surfactant paste, of about 0.1% to about 50% polyethylene glycol which it has a melting temperature of 35 to 70 ° C, introduced as non-aqueous polyethylene glycol; from about 30% to about 95% of a detersive surfactant, and water for equilibrium; (b) mix the detergent agglomerates in a mixer / densifier moderate speed to densify and agglomerate additionally detergent agglomerates; and (c) dry the detergent agglomerates to form the high density detergent composition.

In an especially preferred embodiment of the Invention, the process comprises the steps of:

(a) continuously mixing a detergent surfactant paste and an initial dry detergent material comprising a detergency builder additive selected from the group consisting of aluminosilicates, crystalline layered silicates, sodium carbonate, Na 2 Ca (CO 3) ) 2, K 2 Ca (CO 3) 2, Na 2 Ca 2 (CO 3) 3, NaKCa (CO 3) _ { 2}, NaKCa 2 (CO 3) 3, K 2 Ca 2
(CO 3) 3 and mixtures thereof, in a high speed mixer / densifier to obtain detergent agglomerates, wherein said surfactant paste includes, by weight of said surfactant paste, about 0.1% to about 50% polyethylene glycol having a melting temperature of 35 to 70 ° C, introduced as non-aqueous polyethylene glycol; from about 30% to about 95% of a detersive surfactant and water for equilibrium, the weight ratio between the surfactant paste and the dry detergent material being from about 1:10 to about 10: 1; (b) mixing the detergent agglomerates in a moderate speed mixer / densifier to densify and further agglomerate the detergent agglomerates; (c) drying the detergent agglomerates; and (d) adding a coating agent to obtain a high density detergent composition with a density of at least 650 g / l.

The invention also provides a composition. high density detergent prepared according to the process of invention and its different embodiments.

Therefore, it is an object of the present invention provide a process to continuously produce a high density detergent composition directly from a surfactant paste and dry adjuvant detergent ingredients initials. Another object of the invention is to provide a process of this type that produces a composition with flow properties improved. Another object of the invention is to provide a process of this type that is more efficient and economical to operate at large scale. These and other objects, features and possible advantages of the present invention will be clear to the expert in the technique after reading the following drawings, the detailed description of the preferred embodiment and the appended claims.

Detailed description of the preferred embodiment

The present process is used to produce low dosage detergent agglomerates directly from of initial detergent ingredients instead of granules conventional "post-tower" detergents. The "post-tower" detergent granules expression means detergent granules that have been processed in a tower of conventional spray drying or in a similar apparatus. The process of the invention allows to manufacture low detergents Dosing in an environmentally friendly way by avoiding use of spray drying techniques or the like that typically emit pollutants into the atmosphere through their towers or chimneys This feature of the process of the invention is extremely desirable in especially sensitive geographical areas to the emission of pollutants into the atmosphere.

Process

In the first stage of the process of the invention are mixed continuously in a high mixer / densifier speed 10 several streams of detergent ingredients initials, including a stream of surfactant paste 12 and a initial dry detergent material stream 14. Paste surfactant 12 comprises from about 30% to about 95%, preferably from about 60% to about 85% and most preferably from about 70% to about 75%, by weight of a detergent surfactant in the form of paste.

The surfactant paste 12 includes polyethylene glycol having a melting temperature of 35 to 70 ° C to facilitate the production of high detergent agglomerates density with improved flow properties. It has been observed that at include non-aqueous polyethylene glycol in surfactant paste 12, thus replacing at least partially the water in the paste, surprisingly achieves the formation of agglomerates with basically improved flow properties. The non-aqueous binder in the paste not only improves the agglomerates formed in the process of the invention but also retains the properties of paste processability and portability while maintaining viscosity at a sufficiently low level for these tasks. Without pretend to impose any theory, it is believed that partial replacement of the water in the paste by the non-aqueous binder causes the agglomeration occurs at a higher temperature and so more controllable, allowing the formation of fluid agglomerates more friable

Therefore, the surfactant paste comprises also from about 0.1% to about 50%, more preferably from about 1% to about 15% and with highest preference of about 2% to about 8%, in weight of non-aqueous polyethylene glycol and water for equilibrium and, optionally, other conventional detergent ingredients. He polyethylene glycol improves agglomeration by acting as an agent "binder" or "adherent" of detergent components of process. The polyethylene glycol preferably has a viscosity of approximately 0.1 Pa.s (100 cP) at approximately 100 Pa.s (100,000 cP) and most preferably about 1 Pa.s (1000 cP) at approximately 25 Pa.s (25,000 cP). Also has preferably a melting point of about 40 ° C at approximately 60 ° C, so that it can operate effectively maximum in the process of the invention.

Preferably, the dry detergent material initial 14 comprises from about 20% to about 50%, preferably from about 25% to about 45% and with highest preference of about 30% to about 40%, of a detergent reinforcing additive of the aluminosilicate type or zeolite, and from about 10% to about 40%, preferably from about 15% to about 30% and with highest preference of about 15% to about 25%, of a sodium carbonate. Most preferably the reinforcing additive of the detergency is selected from the group consisting of aluminosilicates, crystalline laminar silicates, carbonate sodium, Na 2 Ca (CO 3) 2, K 2 Ca (CO 3) 2, Na 2 Ca 2 (CO 3) 3, NaKCa (CO 3) 2, NaKCa 2 (CO 3) 3, K 2 Ca 2 (CO 3) 3 and mixtures of the same. It should be understood that in the high mixer / densifier speed 10 other detergent ingredients can be mixed initials, some of which are described below, without therefore, leaving the scope of the invention.

Preferably, the relationship between the paste surfactant 12 and the initial dry detergent material 14 is of about 1:10 to about 10: 1, more preferably of approximately 1: 4 to approximately 4: 1 and most preferably from about 2: 1 to about 2: 3.

It has been observed that the first stage of the process can be done successfully, using the process parameters described herein, in a mixer / densifier of high speed which is preferably a Lödige CB mixer or other of similar brand. These types of mixers practically consist of a hollow horizontal static cylinder that has a rotating shaft centrally mounted around which several are fixed Blades with a plow configuration. The shaft rotates at a speed from about 10.5 rad / s (100 rpm) to about 261.8 rad / s (2500 rpm) and more preferably about 31.4 rad / s (300 rpm) at approximately 167.6 rad / s (1600 rpm). Preferably, the average residence time of the ingredients detergents in the high speed mixer / densifier 10 is preferably about 2 sec. at approximately 45 sec. and most preferably about 5 sec. to approximately 15 sec

Next the detergent agglomerates resulting formed in the high speed mixer / densifier they are fed to a lower speed mixer / densifier or moderate 16 where agglomeration and densification is performed additional. This moderate speed mixer / densifier used in this process should include tools for liquid distribution and agglomeration so that both techniques can be done simultaneously. It is preferable that the moderate speed mixer / densifier 16 be, for example, a  Lödige KM mixer (Plowshare), Drais® K-T 160 u another similar brand. The residence time in the moderate speed mixer / densifier is preferably of approximately 0.5 minutes to approximately 15 minutes and with highest preference from about 1 to about 10 minutes The distribution of the liquid is done by blades, generally of a smaller size than the rotating shaft, the which preferably operate at approximately 377 rad / s (3600 rpm).

According to the present process, the combination of high speed mixer / densifier and mixer / densifier of moderate speed provide the amount of energy needed to form the desired agglomerates. The mixer / densifier of Moderate speed generates approximately 5000 J / kg (5 \ times 10 10 erg / kg) at about 2 x 10 5 J / kg (2 x 10 12 erg / kg) at a speed of approximately 30 J / kg-sec. (3 x 10 8 erg / kg-sec.) to approximately 300 J / kg-sec. (3 x 10 9 erg / kg-sec.) to form detergent agglomerates high density fluids. The energy input and the speed of input can be determined from the power readings at moderate speed mixer / densifier with and without granules, the residence time of the granules in the mixer / densifier and the mass of granules in the mixer / densifier. These calculations are They are clearly available to the subject matter expert.

The density of detergent agglomerates resulting from the mixer / speed densifier moderate 16 is at least 650 g / l and more preferably it is in the range from about 700 g / l to about 875 g / l. TO then the detergent agglomerates are dried in a dryer fluid bed or similar apparatus to obtain a composition high density granulated detergent that is already at this point ready for packaging and sale as a compact detergent product of Low dosage Detergent agglomerates obtained through process preferably have a surfactant concentration of about 25% to about 55%, more preferably of approximately 35% to approximately 55% and most preferably from about 45% to about 55%. The porosity of particles of the detergent agglomerates resulting from the composition is preferably about 5% at about 20% and more preferably about 10%. As one skilled in the art will easily appreciate, a agglomerate low porosity detergent provides a product dense or low dosage detergent, to which it refers Mainly the present process.

In addition, an attribute of the agglomerates Dense or densified detergents is particle size relative. The present process typically provides agglomerates with a median particle size of about 400 µm to about 700 µm and more preferably from about 400 µm to about 500 \ mum. Here, the expression "median size of particle "refers to individual agglomerates and not to individual detergent particles or granules. The combination of the porosity and particle size mentioned above produces agglomerates with densities of 650 g / l and higher. This feature is especially useful in making laundry detergents of low dosage as well as other granulated compositions such as washing compositions of dishes.

Optional stages of the process

At an optional stage of the present process the detergent agglomerates leaving the fluid bed dryer are conditioned additionally by cooling them in a refrigerator fluid bed or in a similar apparatus known in the art. Other Optional stage of the process involves adding an agent coating to improve fluidity and / or minimize over agglomeration of the detergent composition at one or more points of the following process of the invention: (1) the agent of coating can be added directly after the refrigerator of fluid bed as the coating agent stream shows (favorite); (2) the coating agent can be added between the fluid bed dryer and fluid bed refrigerator as shows the coating agent stream; (3) the agent of coating can be added between the fluid bed dryer and the moderate speed mixer / densifier as shown in the stream; and / or (4) the coating agent can be added directly to the moderate speed mixer / densifier and to fluid bed dryer as current shows. Must be understood that the coating agent can be added in any stream or in any combination of currents. The agent stream of Coating is the most preferred in the process of the invention. He coating agent is preferably selected from the group that It consists of aluminosilicates, silicates, carbonates and mixtures of same. The coating agent not only improves the fluidity of the resulting detergent composition, made desired by the consumers by allowing easy detergent dosing during use, it also serves to control the agglomeration by avoiding or minimizing over agglomeration, especially when it is added directly to the moderate speed mixer / densifier. As is known by the person skilled in the art, over agglomeration can lead to flow properties and aesthetics of the detergent product Very undesirable end.

Other optional stages contemplated by the This process includes the screening of detergent agglomerates oversized in sieves of different shapes, including but not limited to conventional sieves chosen according to the Desired particle size in the finished detergent product. Other Optional stage includes conditioning the detergent agglomerates subjecting these to an additional drying. Optionally, the process  may comprise the step of spraying an additional binder in one or both mixers / densifiers. The binder can comprise the same non-aqueous binder material used in the surfactant paste as described above.

Another optional stage of the process of the invention consists in finishing the resulting detergent agglomerates using different processes, including spraying and / or mixing of other conventional detergent ingredients, mentioned from collective form as the final stage. So, for example, the stage final covers the spraying of perfumes, brighteners and enzymes on the finished agglomerates to obtain a composition more complete detergent. These techniques and these ingredients are well known in the art.

Detergent surfactant paste

As briefly described above, The detergent surfactant paste used in the process is preferably found in the form of a non-aqueous viscous paste. The so-called viscous surfactant paste has a viscosity of approximately 5 Pa.s (5,000 cP) to approximately 100 Pa.s (100,000 cP) and more preferably about 10 Pa.s (10,000 cP) at approximately 80 Pa.s (80,000 cps). Viscosity it is measured at 70 ° C with friction speeds of approximately 10 to 100 sec. -1.

The surfactant of the surfactant paste itself viscose is preferably selected from those of the anionic type, non-ionic, hybrid, ampholytic and cationic ion and mixtures compatible of them. Detergent surfactants useful in The present invention is described in the patent US 3,664,961, issued to Norris on May 23, 1972, and in US Patent 3,919,678, granted to Laughlin et al. on December 30, 1975. Surfactants Useful cationics also include those described in the patent US-4,222,905, granted to Cockrell on the 16th of September 1980, and in US Patent 4,239,659, granted to Murphy on December 16, 1980. Among the surfactants, the most preferred are anionic surfactants and Nonionics

Non-limiting examples of the preferred anionic surfactants useful in the surfactant paste include conventional C 11 -C 18 alkyl benzene sulphonates ("LAS"), the C 10 -C 20 alkyl sulfates ("AS ") Branched chain and random primary, C 10 -C 18 alkyl secondary sulfates (2.3) of the formula CH 3 (CH 2) x (CHOSO 3 ^ ^ {-} M +) CH 3 and CH 3
(CH 2) y (CHOSO 3 ^ - M +) CH 2 CH 3 where xe (y + 1) are integers of at least about 7 and preferably of at least about 9, and M is a hydro-soluble cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and C 10 -C 18 alkylalkoxy sulfates ("AE x S"; especially EO 1-7 ethoxy sulfates).

Optionally, other illustrative surfactants useful in the pulp of the invention may include alkylalkoxy C 10 -C 18 carboxylates (especially EOs 1-5 ethoxycarboxylates), glycerol C 10-18 ethers, the alkyl C 10 -C 18 polyglycosides and their corresponding sulfated polyglycosides, and esters C 12 -C 18 alpha-sulphonates of fatty acid. If desired, they can also be included in the general non-ionic and amphoteric surfactant compositions conventional such as alkyl C_ {12} -C_ {18} ethoxylates ("AE"), included the so-called narrow-peak alkyl ethoxylates and the alkyl C 6 -C 12 phenol alkoxylates (especially ethoxylates and mixed ethoxy / propoxy), C 12 -C 18 betaines and sulfobetains ("sultaines"), amine oxides C 10 -C 18, and the like. Can also be use N-alkyl C 10 -C 18 fatty acid polyhydroxyamides. Typical examples include N-methyl C 12 -C 18 glucamides (see application WO 9,206,154). Other sugar-derived surfactants include acid N-alkoxy polyhydroxyamides fatty like N- (3-methoxypropyl) C 10 -C 18 glucamide. You can use the N-propyl to N-hexyl C 12 -C 18 glucamides to achieve a low foaming Soaps can also be used C 10 -C 20 conventional. If you want one high foaming, chain soaps can be used branched C 10 -C 16. Result especially useful mixtures of anionic surfactants and nonionic surfactants. Other useful conventional surfactants They are described in the standard texts.

Dry detergent material

The initial dry detergent material of the present process preferably comprises a reinforcing additive of the aluminosilicate type detergency, mentioned as ion exchange aluminosilicate, and sodium carbonate. The ion exchange aluminosilicate materials used in the present invention as a detergency builder preferably they have a high ion exchange capacity calcium and a high exchange rate. Without pretending impose any theory, it is believed that these high speeds and calcium ion exchange capabilities depend on several interrelated factors that derive from the method of Production of ion exchange aluminosilicate material. TO In this regard, exchange aluminosilicate materials ionic used in the present invention are manufactured preferably according to Corkill et al., patent US-4,605,509 (Procter & Gamble).

Preferably, the aluminosilicate material ion exchange is in its "sodium" form, since the potassium and hydrogen forms of the aluminosilicate of the invention they do not have a speed and an exchange capacity so high as those of the sodium form. In addition, the material of ion exchange aluminosilicate is preferably a form excess drying to facilitate the obtaining of agglomerates friable detergents such as those described herein. The ion exchange aluminosilicate materials used in the present invention preferably have size diameters of particles that optimize their effectiveness as reinforcing additives of the detergency The expression "particle size diameter" in the present specification means the average size diameter of particles of a certain aluminosilicate material of ion exchange determined by analytical techniques conventional such as microscopic determination and scanning electron microscopy (MEB). The size diameter of Preferred particles for aluminosilicate is approximately 0.1 µm to about 10 µm and more preferably of about 0.5 µm to about 9 µm. With maximum Preferably, the particle size diameter is about 1 µm to about 8 µm.

Preferably, the aluminosilicate material ion exchange has the formula

Na_ {z} [(AlO_2) {z} \ cdot (SiO 2) y] xH 2 O

where z and y are whole numbers of at least 6, the molar ratio between z and y is about 1 to about 5, and x is about 10 to about 264. More preferably, the aluminosilicate has the formula

Na 12 [(AlO 2) 12 \ cdot (SiO 2) 12] xH 2 O

where x is about 20 to about 30, preferably about 27. These Preferred aluminosilicates are marketed, for example, under the names Zeolita A, Zeolita B and Zeolita X. Alternatively, the natural ion exchange aluminosilicate materials or Synthetics suitable for use in the present invention may be manufactured as described in the patent US 3,985,669 granted to Krummel and cabbage.

The aluminosilicates used herein invention are also characterized by their exchange capacity ionic, which is at least about 200 mg equivalent of CaCO 3 hardness / gram, calculated as anhydrous substance, and that preferably it is about 300 to 352 mg equivalents of CaCO_ {3} hardness / gram.

Preferably, a water-soluble cation selected from the group consisting of hydrogen, water-soluble metals, hydrogen, boron, ammonium, silicon and mixtures thereof, more preferably, sodium, potassium, hydrogen, lithium, ammonium and mixtures thereof, is present. the most preferred sodium and potassium. Non-limiting examples of anions that are not carbonate include those selected from the group consisting of chloride, sulfate, fluoride, oxygen, hydroxide, silicon dioxide, chromate, nitrate, borate and mixtures thereof. Preferred detergency builders of this type in their simplest form are selected from the group consisting of Na 2 Ca (CO 3) 2,
K 2 Ca (CO 3) 2, Na 2 Ca 2 (CO 3) 3, NaKCa (CO 3) 2, NaKCa 2 (CO 3) 3, K 2 Ca 2 (CO 3) 3 and combinations thereof. An especially preferred material for the detergency builder additive described herein is Na 2 Ca (CO 3) 2 in any of its crystalline modifications.

Reinforcing additives of the detergency of the above defined type suitable including the natural or synthetic forms of one or combinations of the following minerals: Afghanite, Andersonite, Ashcroftine, and Beyerite, Borcarita, Burbankita, Butschliita, Cancrinita, Carbocernaita, Carletonita, Davyne, DonnayiteY, Fairchildita, Ferrisurita, Franzinita, Gaudefroyita, Gaylussita, Girvasita, Gregoryita, Jouravskita, KamphaugiteY, Kettnerita, Khanneshita, LepersonniteGd, Liottite, MckelveyiteY, Microsommita, Mroseita, Natrofairchildita, Nyerereita, RemonditeCe, Sacrofanita, Schrockingerita, Shortita, Surita, Tunisita, Tuscanita, Tyrolita, Vishnevita and Zemkorita. The Preferred mineral forms include Nyererita, Fairchildita and Shorty

Adjuvant detergent ingredients

The initial dry detergent material in the This process may include other detergent ingredients and / or additional ingredients can also be incorporated into the detergent composition during later stages of the present process. These adjuvant ingredients include other additives detergency builders, bleaches, activators bleach, foaming enhancers or defoamers, anti-fogging and anti-corrosion agents, suspensions stains, stain repellent agents, germicides, agents pH adjusters, alkalinity sources without reinforcing additive of detergency, chelating agents, smectite clays, enzymes, enzyme stabilizing agents and perfumes. See the US Patent 3,936,537, issued February 3, 1976 to Baskerville, Jr. et al.

Other detergency builders they can generally be selected from different phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxy sulfonates, polyacetates, carboxylates and water-soluble alkali metal, ammonium or ammonium polycarboxylates replaced. Among the above, metal salts are preferred alkaline, especially sodium. Preferred for use in The present invention is phosphates, carbonates, fatty acids C 10-18, polycarboxylates and mixtures of the same. More preferred are sodium tripolyphosphate, the tetrasodium pyrophosphate, citrate, tartrate mono-succinates and tartrate di-succinates and mixtures thereof (see more ahead).

Crystalline lamellar sodium silicates they have a calcium and magnesium ion exchange capacity clearly superior to amorphous sodium silicates. In addition, the Sodium laminar silicates show greater preference for magnesium ions than calcium ions, characteristic that is necessary to ensure the elimination of virtually all of the "hardness" of the wash water. These layered silicates of crystalline sodium, however, are generally more expensive than amorphous silicates and other reinforcing additives of the detergency Therefore, to provide a washing detergent of economically feasible clothing, it is necessary to determine carefully the proportion of layered sodium silicates crystals used.

Crystalline lamellar sodium silicates suitable for use in the present invention preferably They have the formula:

NaMSi_ {x} O_ {2x + 1} \ cdot and H2O

where M is sodium or hydrogen, x is about 1.9 to about 4, and y is of about 0 to about 20. More preferably, the crystalline laminar sodium silicate has the formula:

NaMSi_ {2} O_ {5} \ cdot and H2O

where M is sodium or hydrogen, and and is from about 0 to about 20. These and others crystalline lamellar sodium silicates are described in the patent US-4,605,509, granted to Corkill and cabbage.

Specific examples of inorganic phosphate type detergency builders are tripolyphosphates, pyrophosphates, polymeric sodium and potassium metaphosphates with a polymerization degree of about 6 to 21 and orthophosphates. Examples of polyphosphonate-type detergency builders are the sodium and potassium salts of ethylenediphosphonic acid, the sodium and potassium salts of ethane-1-hydroxy-1, 1-diphosphonic acid and the sodium and potassium salts of ethane acid -1,1,2-triphosphonic. Other phosphorus-type detergency builder additives are described in US Pat. Nos. 3,159,581; US 3,213,030; US 3,422,021; US 3,422,137; US-3,400,176 and
US 3,400,148.

Examples of phosphorus-free inorganic builder detergents are tetrahydrate decahydrate and silicates with a weight ratio SiO2: alkali metal oxide of about 0.5 to about 4.0 and preferably about 1.0 to about 2.4. Hydro-soluble phosphorus-free organic detergency builder additives useful in the present invention include alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxysulfonates. Examples of detergency builders of the polycarboxylate and polyacetate type are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylenediaminetetraacetic, nitrilotriacetic, oxydisuccinic, melitic, polycarboxylic benzene and
citric.

Additives strengthening detergency Polymeric polycarboxylate type are described in the patent US 3,308,067, granted to Diehl on March 7, 1967. These materials include water soluble salts of homopolymers and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, acid fumaric, aconitic acid, citraconic acid and acid methylenemalonic Some of these materials are useful as the water-soluble anionic polymer described below, but only if is intimately mixed with the anionic surfactant without soap.

Other polycarboxylates suitable for use in The present invention is the polyacetal carboxylates described in US Patent 4,144,226, issued March 13, 1979 to Crutchfield et al., And the patent US 4,246,495, issued March 27, 1979 to Crutchfield et al. These polyacetal carboxylates can be prepared by mixing an acid ester under polymerization conditions glyoxylic and a polymerization initiator. Then the resulting carboxylate polyacetal ester binds to groups chemically stable terminals to stabilize the polyacetal carboxylate versus rapid solution depolymerization alkaline, after which it becomes the corresponding salt and add to a detergent composition. The reinforcing additives of the Especially preferred polycarboxylate detergency are the carboxylate ether detergency builder additives that comprise a combination of tartrate monosuccinate and tartrate disuccinate described in US Patent 4,663,071, granted to Bush et al. May 5, 1987.

Bleaching agents and activators of bleach are described in US Pat. No. 4,412,934, granted to Chung et al. on November 1, 1983, and in the patent US 4,483,781, granted to Hartman on November 20 of 1984. Chelating agents are also described in the patent. US 4,663,071, issued to Bush et al., Column 17, line 54 to column 18, line 68. The training modifiers foam are also optional ingredients and are described in the US Patent 3,933,672, issued January 20, 1976 to Bartoletta et al., And US 4,136,045, granted on January 23, 1979 to Gault et al.

Smectite type clays suitable for your use in the present invention are described in the patent US-4,762,645, granted to Tucker et al. the 9 of August 1988, column 6, line 3 to column 7, line 24. Other detergency builder additives suitable for use in the The present invention are listed in the Baskerville patent, column 13, line 54 to column 16, line 16 and in the patent US 4,663,071, granted to Bush et al. May 5th of 1987.

In order for the present invention to result more easily understandable include the following examples, which They are only intended to be illustrative and not limiting the scope of the invention.

Example I

This example illustrates the process of the invention for producing a fluid and friable high density detergent composition in the form of agglomerates. In a Lödige CB-30 mixer / densifier, two feed streams with different initial detergent ingredients are continuously introduced, at a speed of 1270 kg / h, one of them comprising a surfactant paste containing surfactant and the non-aqueous binder polyethylene glycol, and the other the initial dry detergent material containing aluminosilicate and sodium carbonate. The rotation speed of the shaft in the Lödige CB-30 mixer / densifier is approximately 146.6 rad / s (1400 rpm) and the average residence time is approximately 10 sec. The contents of the Lödige CB-30 mixer / densifier are continuously fed to a Lödige KM 600 mixer / densifier for further agglomeration with an average residence time of approximately 6 minutes. Next, the resulting detergent agglomerates are fed to a fluid bed dryer and then to a fluid bed refrigerator, the average residence times being approximately 10 minutes and 15 minutes, respectively. Approximately halfway after a moderate speed mixer / densifier, a coating agent, aluminosilicate, is fed to control and prevent over agglomeration. Next, the detergent agglomerates are passed through a conventional sieving apparatus to obtain a uniform particle size distribution. The composition of the detergent agglomerates leaving the fluid bed refrigerator is shown in Table I
next:

TABLE I

Component % by weight of the load total Rent C_ {14-15} sulfate 22.5 C 12 alkyl benzene sulfonate linear 2.5 Aluminosilicate 35.2 Carbonate sodium 21.0 Polyethylene Glycol (PM 4000) 1.5 Various (water, etc.) 12.3 \ overline {100.0}

In the final stage the ingredients are pulverized additional detergents, including perfumes, enzymes and others minor components, on the described agglomerates above to obtain a finished detergent composition that is mixing with spray dried granules in a ratio of 60:40 weight (agglomerates: spray dried granules). In the Table II below shows the relative proportions of the finished total detergent composition obtained by the process of the invention:

TABLE II

Component (% in weight) Rent C 14-15 sulfate / C 12.3 alkyl benzene linear sulphonate 16.3 Neodol 23-9.51 1.8 Polyacrylate (PM = 4500) 3.2 Polyethylene glycol (PM = 4000) 1.7 Sulfate sodium 5.7 Aluminosilicate 26.3 Carbonate of sodium 33.1 Enzyme protease 0.4 Enzyme amylase 0.1 Enzyme lipase 0.2 Enzyme cellulase 0.1 Components minorities (water, perfume, etc.) 11.1 \ overline {100.0} 1 Alkyl C 12-13 ethoxylate (EO = 9) marketed by Shell Oil Company

The density of the detergent composition Totally formulated result is 561 g / l and the median size of particles is 450 µm. The density of the agglomerates alone it is 810 g / l.

Example II

This example illustrates another process according to invention in which the steps described in Example I are performed except that the coating agent, aluminosilicate, is added after the fluid bed cooler instead of in the moderate speed mixer / densifier. In Table III The composition of the detergent agglomerates is shown below leaving the fluid bed cooler after the addition of coating agent:

TABLE III

Component % by weight of the load total Rent C_ {14-15} sulfate 22.7 Rent C 12-13 benzene sulfonate linear 7.6 Aluminosilicate 34.5 Carbonate sodium 21.2 Polyethylene Glycol (PM 4000) 1.5 Various (water, perfume, etc.) 12.5 \ overline {100.0}

In the final stage the ingredients are pulverized additional detergents including perfumes, brighteners and enzymes, on the agglomerates described above to obtain a finished detergent composition that is mixed with granules spray dried in a 60:40 weight ratio (agglomerates: spray dried granules). In Table IV Following are the relative proportions of the composition finished total detergent obtained by the process of invention:

TABLE IV

Component (% in weight) Rent C 14-15 sulfate / C 12.3 alkyl benzene linear sulphonate 16.3 Neodol 23-9.51 1.8 Polyacrylate   (PM = 4500) 3.2 Polyethylene glycol (PM = 4000) 1.7 Sulfate sodium 5.7 Aluminosilicate 26.3 Carbonate of sodium 33.1 Enzyme protease 0.4 Enzyme amylase 0.1 Enzyme lipase 0.2 Enzyme cellulase 0.1 Components minorities (water, perfume, etc.) 11.1 \ overline {100.0} 1 Alkyl C 12-13 ethoxylate (EO = 9) marketed by Shell Oil Company

The density of the detergent composition resulting is 560 g / l and the median particle size is 450 µm. The density of the agglomerates is only 860 g / l

Once the invention has been described in detail, it is obvious to the person skilled in the art that it is possible to perform different changes without abandoning the scope of the invention and that, in addition, the invention should not be considered limited to described in the specification.

Claims (8)

1. A process for continuously preparing a high density detergent composition characterized by the steps of:

(to)

continuously mix a paste detergent surfactant and an initial dry detergent material in a high speed mixer / densifier that has an axis with a rotation speed of 10.5-261.8 rad / s (100-2500 rpm) to obtain detergent agglomerates, wherein said surfactant paste includes, by weight of said paste surfactant, from 30 to 95% by weight of detersive surfactant; of 0.1 at 50% by weight of polyethylene glycol having a temperature of melting at 35 to 70 ° C fed as non-aqueous polyethylene glycol; and the water for balance,

(b)

mix said detergent agglomerates in a moderate speed mixer / densifier that generates from 5000 J / kg (5 x 10 10 erg / kg) at 2 x 10 5 J / kg (2 x 10 12 erg / kg) at a speed of 30 J / kg.sec. (3 x 10 8 erg / kg.sec.) A 300 J / kg. Sec. (3 x 10 9 erg / kg.sec.) To densify and agglomerate additionally said detergent agglomerates; Y

(C)

dry said detergent agglomerates to form said high density detergent composition.

2. A process according to claim 1, in the that the surfactant paste includes from 60% to 95% by weight of detersive surfactant and from 1% to 15% by weight of polyethylene glycol 3. A process according to any of the previous claims, wherein the polyethylene glycol is 4000 polyethylene glycol. 4. The process according to any of the previous claims, wherein said initial dry material it is a detergent builder additive selected from the group consisting of aluminosilicates, crystalline laminar silicates, sodium carbonate, Na 2 Ca (CO 3) 2, K 2 Ca (CO 3) 2, Na 2 Ca 2 (CO 3) 3, NaKCa (CO 3) 2, NaKCa 2 (CO 3) 3, K 2 Ca 2 (CO 3) 3 and mixtures of the same. 5. The process according to any of the preceding claims, which is also characterized by including the step of adding a coating agent after said moderate speed mixer / densifier, the coating agent being selected from the group consisting of aluminosilicates, carbonates, silicates and mixtures thereof. 6. The process according to any of the previous claims, wherein the average residence time of said detergent agglomerates in said mixer / densifier of High speed is in the interval of 2 sec. at 45 sec. 7. The process according to any of the previous claims, wherein the average residence time of said detergent agglomerates in said mixer / densifier of Moderate speed is in the range of 0.5 minutes to 15 minutes 8. A process for continuously preparing a high density detergent composition characterized by the steps of:

(to)

continuously mixing a detergent surfactant paste and an initial dry detergent material characterized by comprising a detergent builder additive selected from the group consisting of aluminosilicates, crystalline layered silicates, sodium carbonate, Na 2 Ca (CO 3) ) 2, K 2 Ca (CO 3) 2, Na 2 Ca 2 (CO 3) 3, NaKCa (CO 3) _ { 2}, NaKCa 2 (CO 3) 3, K 2 Ca 2 (CO 3) 3 and mixtures thereof, in a high speed mixer / densifier having an axis with a rotation speed of 10.5-261.8 rad / s (100-2500 rpm) to obtain detergent agglomerates, wherein said surfactant paste includes, by weight of said surfactant paste, from 70% to 95 % of a detersive surfactant and from 0.1% to 50% of polyethylene glycol having a melting temperature 35 to 70 ° C, introduced as non-aqueous polyethylene glycol, and water for equilibrium, the weight ratio being between said surfactant paste and said material dry detergent from 1:10 to 10: 1; mixing said detergent agglomerates in a moderate speed mixer / densifier that generates from 5000 J / kg (5 x 10 10 erg / kg) to 2 x 10 5 J / kg (2 x 10 12) erg / kg) at a speed of 30 J / kg.sec. (3 x 10 8 erg / kg.sec.) At 300 J / kg.sec. (3 x 10 9 erg / kg.s) to further densify and agglomerate said detergent agglomerates,

(b)

drying said detergent agglomerates; Y

(C)

add a coating agent to obtaining said high density detergent composition with a density of at least 650 g / 1.