MXPA99011782A - Production of detergent granulates - Google Patents

Abstract

A process of forming granular detergent products, the process comprising, in a gas fluidisation granulator, contacting a fluidised particulate solid material with a spray of liquid binder, whilst fluidising the solids in the granulator with at least one gas stream, wherein the gas temperature is controlled so as to be increased and/or reduced during at least one stage of the process.

Description

PRODUCTION OF GRANULATED DETERGENTS DESCRIPTION OF THE INVENTION I ^ The present invention is related to? ! a process for the production of detergent composition in granules. It is well known in the art to obtain powders of tertiles by spray drying. However, the spray drying process consumes a lot of money and energy and consequently the resulting product is expensive. More recently, there has been a lot of interest in production. or granular detergent through the process _ which mainly use mixing, without. the use of spray drying. These mixing techniques can offer great flexibility to produce powders of several different compositions in a single plant post-dosing several components after an initial granulation step. A known type of mixing process that does not involve spray drying, uses moderate speed granulldor (a common example very often colloquially called "plowing"), optionally preceded by a mixer = -_ Although the fluidization granulators of __ - | Gas can give good volume density control, there is still a need for greater flexibility and in particular, to produce powders of lower volume density. The processes that involve the granulation of cutting at low speed are very varied. *: For example, WO96 / 04359 (Unilever) discloses a process in which low volume density powders are prepared by contacting a neutralizing agent such as an alkaline builder and a liquid acid precursor. an anionic surfactant in a fluid zone to form detergent granules. However, as indicated in the Indian Patent No. 166307 (Unilever), the use of a conventional liquid gas process can lead to the formation of sticky lumps and granules. This problem is solved by using an internal recirculation gas fluidization granulator I. However, the present invention solves this problem more simply and effectively by controlling the temperature of the gas.Therefore, the present invention goes on to provide a process for forming products of gas. granular detergents, the process comprises, in a gas fluidization granulator, contacting a solid fluidized particulate material with a liquid binder spray, while fluidizing the solids in the granulator with at least one gas stream. , wherein the gas temperature is controlled in such a way that it can be increased and / or reduced during a process step. The temperature of the gas according to the present invention leads to an increase and / or reduction in the temperature of the solid material in n fluidized particles during at least one stage of the process. In other words, the temperature of the gas is controlled not simply to maintain a constant "bed" temperature, for example by removing the heat from the reaction, but to increase and / or decrease the current temperature of the solids. _ The baking granulation and gas granulation apparatus? It includes a camera in which 1 utna 1"L gas stream, usually air, is used to cause a turbulent flow of particulate solids to form a" cloud "of solids and 1 liquid binder is sprayed on or inside, the cloud to come into contact with the individual particles f. As the process progresses, the individual particles of the solid materials ~ -? initials agglomerate, due to the liquid binder, to form granules. | The process of the present invention resolves t the stickiness of the granules as they are formed. In many cases, it is believed that this may occur as a result of the transformation of liquid constituent messes into a more solid state or a state having a higher viscosity, due to the temperature variation ^ of the process. J * The increase and / or reduction of temperature must occur during the stage of a process, that is, at least one stage when fluidization and sprinkling are in progress. The process can be operated with a gas temperature below the ambient temperature during at least one stage (or all stages -) of the process. Preferably, a higher gas temperature is operated chronologically during a first stage of the process than during a second stage, before or after the first stage. The gas fluidization granulator is typically operated at a surface air velocity of approximately 0.1-1.2 ms' either low positive or negative relative pressure. | The temperature of the gas, and thus preferably the temperature of the bed, can rise during a prime. For example, up to 80 ° C or even up to 200 ° C, and then in a nail or fights from the other "stages" (before then), it can be reduced to just above, in, or . below room temperature, for example at 30 ° C or less, preferably 25 ° C or less or even as low as 5 ° C or -10 ° C or less. In a preferred embodiment, the temperature of the. gas, and preferably also the temperature of 1 ... ll, rises by means of a prime period.; and subsequently decreases in a second period. ? : - When, the process is a proc: e "s - '" or., ".-By lot, •?" - "- ~' -: i ''! The temperature change will be - e faith ct uada with 1 time.If -it is a continuous process, it will vary to. The length of the "course" of the ho ho anuíador In this last case, this is carried out with the use of a granulator of the type "aradp grating", that is to say in one in .. which materials flow through the reactor, from the beginning to the end ... In a batch process, the temperature of the gas can: reduce over a period of time. relatively short, for example 10 to 50% of the time of the process. Typically, the gas temperature can be reduced by 0.5 to 15 minutes. In (a continuous process, the temperature of the gas can be reduced over a relatively short length of the "course" of the granulator bed, for example over 10 to 50% of the course. It can be pre-cooled. Preferably, the temperature of the gas, and preferably also the temperature of the bed, is not decreased until the granulation of the fluidized particulate solids is substantially c omp. * C orno is used here, the term "bed temperature" does not refer to the temperature of the fluidized solid particulate material The temperature of the fluidized solid particulate material can be measured, for example, by using a probe te rmoe st Whether there is a discernible bed of dust or there is no discernible bed of powder (ie because the mixer is being operated with a gas velocity so high that the fluid bed is not formed). "bubbly" classic), the "bed temperature" is taken as the temperature measured at a point 1 inside the fluidization chamber approximately cm from the gas distributor plate. In the context of the present invention, the term "granular detergent product" includes granular products finished for sale, as well as granular or auxiliary components for "finished products," eg by post-dosing to or with any other product. In this way, a granular detergent product as defined herein may or may not contain detergent material such as a "synthetic surfactant and / or soap. The minimum requirement is that it should contain at least "one material of a general type of the conventional component of granulare Is detergent products, How is it a surfactant agent (including jabob), a better b 1 a n than a a __ c e enzyme, n fluoresc-corro s_? or n coló rali t -_ "hace .re e consist of grains of individual materials and me z c 1 alir of the grains. The term "granule" refers to a small particle of agglomerated powder materials. The final product of the process [according to the present invention consists of, comprises a high percentage of granules. However, the additional granulator and / or powder materials may optionally be applied to the product. On the other hand, as will be explained in more detail below, the initial solid materials of the present invention are in particles and can be in powder form and / or be 1-. granular = When the gas fluidization graululation process of the present invention is a batch process or a continuous process, the initial solid particulate material can be introduced at what time during the time when the liquid binder is being sprayed. . In the simplest form of the process, the initial solid material is first introduced into the gas fluidization register and then sprayed with the liquid binder. I However, part of the particulate solid material (- initi-1 can be introduced at the beginning of the process in the gas fluidization apparatus and the remaining initial solid materials, when reference is made to an average particle size | say the average particle diameter d 3, 2 The "gas fluidization null" graph can be adapted to recycle "fines" ie material [in 1 powder or partially granular or a very small particle size, so that it can be returned "to two at a time. entrance of the gas fluidization apparatus and / or the entry of a pre-metered clutch.

Preferably, the fine particles are elutriated material, ie they are present in the air exiting a gas fl uxation chamber. ['The gas fluidization granulator can optionally be of the type provided with In I vibrating bed, particularly that is used in continuous mode. In a preferred class of processes according to the present invention, the liquid binder comprises an acid precursor of an age ammonium surfactant and the solid material in the initial particles comprises an inorganic alkaline material. The process of the present invention is especially suitable for this type of granulation, especially when the temperature rises, in the first part of the process. In this way, the neutralization reaction can be performed much closer to completion, before the end of the granulation operation, which otherwise would be the case. In this way it is preferred that the bed temperature be increased by increasing the temperature of the gas during any nitrification reaction, preferably during a substantial part of the neutralization reaction, the acid precursor may be example is the acid precursor of an ammonium surfactant such as linear a1-quilbenzene sulfonate (LAS) or primary alkyl sulfate (PAS) or any other type of ammonium surfactant. Suitable materials that can be used as the inorganic alkaline material include alkali bicarbonates and carbonates, for example, sodium salts thereof. The neutralizing agent is most preferably present at a level sufficient to completely neutralize the acidic component. If desired, an excess of this tri-agent agent can be used to ensure complete neutralization or provide an alternative function, for example as a builder, for example if the neutralizing agent comprises sodium carbonate. . i i The liquid binder can be an alternative! or additionally contain one or more other liquid materials such as surfactants, non-liquid and organic solvents. The total amount of acid precursor is usually as high as possible, subject to the presence of any other component in the liquid and subjected to ^ p) other considerations to which will be made later on. In this way, the acid precursor can constitute 98% (for example at least 95%) by weight of the liquid binder, but it can be at least 75%, at least 50%, or at least 25% by weight of the binder.

To constitute, for example, 5% or less by weight of the binder. Of course, the acid precursor can be completely replaced if required. When the liquid nonionic surfactant I 20 is present in the liquid binder together with an acidic cursor of an anionic surfactant, then the weight ratio of the precursor or precursors to the non-anionic surfactants jormalmente will be 20: 1 to 1:20. However, this ratio can be, for example, inorganic alkaline to react with the fatty acid to produce the soap. The liquid binder will very often be total or non-aqueous non-aqueous, that is, any amount of water present does not exceed 25% by weight of the liquid binder, but preferably not more than 10% by weight. However, if desired, a controlled amount of water can be added to facilitate neutralization Typically, the water can be added in a quantity of 0.5 to 2% by weight of the final detergent product. Any amount of water can be added conveniently before or together or alternatively with the addition of the acid precursor. Alternatively, a liquid aqueous binder can be employed. This is especially for the manufacture of products which are auxiliaries that can be subsequently mixed with other components to form a fully formulated detergent product. Such auxiliaries usually, apart from the components resulting from the liquid binder, mainly consist of one, or a small number of components normally found in the detergent compositions, for example a surfactant or, an enhancer such as zeollta otr ipo 1 if Sodium fato.

However, this does not mean that the use of liquid binders speaks form 11 qui of a cr 11 Sokal The initial preset can come into contact and be mixed with a first portion of the liquid binder, for example in a high or low speed blender (ie a pre-blender) to form a partially granulated material. then it can be sprayed with a second portion of the bound binder in the gas fluidization granulator, to form the granulated detergent product.In the two-stage granulation process, it is preferred, but not absolutely necessary, The total amount of the liquid binder is metered into the fluidization and partial granulation pre-mixing steps Conceivably, part can be dosed during or after the fluidization and / or partial granulation pre-mixing. Also, the content of the binder may vary between this first and second stage.The extent of granulation in the pre-mixer (i.e. al) and J the amount of granulation in the gas fluidization granulator is preferably determined b [according to the density of the desired final product. t The preferred amounts of liquid binder to be dosed in each of the two stages can be divided as follows: __ (i) If a higher density of powder is desired - f low, -that is to say 350-650 g / l, I (a) 5-75% by weight of the total liquid binder is preferably added in the pre-mix; and (b) the remaining 95-25 by weight of the total liquid binder is preferably added in the gas-fumidifier granulator - (n) If a more high powder density is desired, " ie 550-1300 g / 1,, (a) 75-95% by weight of the liquid binder -? Total ~ is preferably added in the pre-mixer; and, (b) the remaining "25-5% in" ~ p is or total liquid binder is preferably added in the Ide gas fluidization granulator. _ If an initial starter is used for partial granulation, an appropriate mixer for this step is a high-speed cutter or low-speed mixer, or a low-speed mixer. KM. Other suitable equipment includes the Dra? SRT160 manufactured by Drais Werke GmbfH, Germarfy; the Littleford mixer with blades. cut _? t e rna s and a turbine type mill mixer that has several blades on one axis of rotation. A high-speed or high-speed mixer granulator has a mixing action and / or a cutting action which are operated independently of one another. The types of granulators of granulators, mixed with cutters, at high low speed are mixers of the series.

Fukae FS Dio s na V series ex Dierks S ohne, Germany; Pharma MatpxR ex T.K. Fielder Ltd; Englañd. Other mixers which are believed to be used for use in the process of the invention are Fuji • VG-C series ex Fu j i. Sangyo C q. , Japan; lthe Roto ex Zanchetta & Co. asi, Italy and SchugilR Flexomix granulator. ": Yet another suitable mixer that can be used. In the pregranulation stage is 1st series Lodig (Mark, registered) FM (plow mixers plowed) 'batch mixer -Mor ton Machine Co. Ltd., S Optionally, a "layer forming agent" or "auxiliary" flow agent "1 may enter at any appropriate stage." This is. .to improve. | the granularity of the product, for example by avoiding aggregation 'and / or the formation of plast of the g ruli s. Layer forming agent is suitably present in an amount of 0.1 to 15%; in weight of the granular product and more. preferably in a quantity of 0.5 to 5%. "Suitable flux auxiliaries / coating agents," include amorphous alkali metal silicates or crystalline silicates, aluminum, which includes ze.oli.Las, D leamol, calcite, diatomaceous earths. s, silica, for example if precipitated, chlorides, sodium chlorides, sulfates such as sulfates of magnesium, carbonates such as calcium carbonate, and phosphates. "how" sodium tripolyphosphate. Mixtures of these materials can be used as desired. In general, the additional components can be: included in a liquid agglutinant or can be mixed with the solid neutralizing agent at any appropriate stage of the process. However, the solid components can be "post-dosed to the pro du ct or granular detergent!" In addition to: ... what 1 r agent is a surfactant that is optionally available can produce by means of a neutralization step, "- other" agents "t in s io.a tio ns ammonic agents t in sioa ct i vo s. no ion i cois", as was mentioned ternary, Also, agents in themselves are cationic, zwitterionic, amido or semi-polar, and mixtures of them. They can be added at an appropriate time. In general, the. "Suitable surfactants include those generally described in" Sur face active agents nd detergents "Vol by Sc Arts nd Perry. Co.,."? e. mentioned earlier, yes; it is desired, the j a-b or n zi derived from unsaturated O-unsaturated fatty acids having, for example, an average C 1 to C 8 carbon atoms may also be present.

If present, the active detergent is suitably incorporated at a level of 5 to 40% preferably 10 to 30% ~ by weight of the product < final granular detergent. T A very often complete detergent composition contains a builder. Such an improver can be introduced with the solid material. and / or subsequently added as desired. The improver may also constitute a neutralizing agent, for example, sodium carbonate, in which case sufficient material will be used for higher functions. Generally speaking, the total amount of detergency better in the appropriate granular product is 95% by 10 80%, preferably 15% to 65%, more preferably 15% to 50% by weight. "" "The inorganic builders that may be present include sodium carbonate, if any, in combination with a crystallization seed for calcium carbonate as described in GB-Al 437 950. Any sodium carbonate it will need to be in excess of that used to neutralize, the anionic acid precursor if the latter was added during the process. layer forming silicates as described in EP-B-164 514. Inorganic phosphate builders, for example sodium, orthophosphate, pyrophosphate, and tripolyphosphate, may also be present, but for environmental reasons these are already - f are not preferred. The 1% if 1, whether they are used as coating and / or ncorporate forming agents in the volume of the particles may be suitably present in a total amount of [10 to 60% and preferably an amount of 15 to 50% by weight. The zeolite used in most of the commercial particulate detergent compositions is zellite A. Advantageously, however, the maximum aluminum P zeolite (zeolite MAP) disclosed and claimed in EP-A-384 07D can be used. [MAP zeolite is an alkaline metal with luminescence of the zj type? which has a proportion of silicone "- for other purposes. The improver is preferably present in the form of" metal salt! alkaline, especially sodium salt. Suitably, the enhancer system can also comprise a crystalline cap-forming silicone, for example, SKS-6 ex Hoechst, a zeolite, for example, zeolite A and optionally an alkali metal citrate. The granular composition resulting from the process of the present invention may also comprise a particulate filler (or any other component that does not contribute to the washing process) which suitably comprises an inorganic salt, for example sodium sulfate and chlorine [ of sodium. The filler may be present at a level of 5 to 70% by weight of the granular product. The present invention also includes an i. granular detergent product resulting from the process of the invention (before any post-dosing or the like). This product will have a volume density determined by the exact nature of the process. If he. process does not involve pre-mixing to effect partial granulation, a final volume density of 350-750 g / 1, can normally be expected. As mentioned earlier, the use of a pre-metering device allows 1 of the final volume of volume to be "350-650 g / 1 ° ~ of 550-1300 g / 1, respectively, in accordance with option (i) or (ii) is used, however, the granular detergent products resulting from the present invention are also characterized by their ranges of particle size. Preferably, not more than 10% by weight has a diameter of > 1.4 mm and more preferably, no more than 5% by weight of the granules are above this limit. It is also preferred that no more than 20% by weight of the granules have a diameter > lmm Finally, granules can be "distinguished from granules produced by other methods by mercury porosimetry.

This last technique can not reliably determine the porosity of the particles (not individual agglomerates but it is ideal for characterizing the granules. A fully formulated detergent composition produced according to the invention can, for example, comprise the active and improver. of detergent and optionally one or more auxiliary fluids, a filler and other minor ingredients such as dye, perfume, fluorescer, bleach, dyes, etc. The invention will now be illustrated by means of the following non-limiting examples: The following formulation was made: Sodium-LAS 24% by weight Sodium-Carbonate 32% by weight STPP 32% by weight Zeolite 4A _ 10% by weight water 2% by weight: In Examples I to IV, the temperature of fluidisation air varied from 20 ° C to 80 ° C in the first stage followed by a second stage at 20 ° C.

A Spraying Sy s_t em SUE 25 i nozzle was operated with an air pressure of at least 5 tbar. The following influence on the powder is a sticky measurement, the higher the value, the product is more sticky. Examples I and II are examples in which there was no temperature variation.

Claims (17)

1. Process for forming a granular detergent product, the process comprises, in a fluidization granulator or gas, contacting a solid particulate material with a liquid binder spray, while the solids are fluidized in the granulator with at least one I run on gas, where the gas temperature is controlled to increase and / or decrease during a phase of the process when fluidization and sprinkling are in progress.

2. Process according to claim 1, wherein the gas temperature is controlled to increase and / or reduce the temperature of the fluidized solid particulate material during at least one step of the process.

, 3. Process according to the claim 2, in "where the temperature of the solid material | in partí c" u the fluidized ones is -reduce below or room temperature during at least one stage •

4. Process according to the claim 2, wherein the temperature of the solid material in fluidized particles is greater during a first stage of the process than during a second stage of the process after the first stage.

5. Process according to claim [4, wherein the process is a batch process and 'the temperature change between the first and second • stage is done on time

. 6. Process according to claim 4, wherein the process is a continuous process and the temperature change between the first and second 15 stage is done throughout the course of granulation

7. Process according to claim 5, which is carried out in a plug flow granulator

8. Process according to any of claims 4 to 7, wherein the temperature at the first stage is controlled to be up to 200 ° C, preferably up to 80 ° C. t

9. Process according to any of claims 4 to 7, wherein the temperature in the second stage is controlled to be 30 ° C, or less, preferably 25 ° C or less, or 5 ° C or less or - 10 ° C or less. ___! f -_ l -

10. Process according to the claim " 1, wherein the gas temperature is reduced due to or at ambient temperature at least at the stage.

11. Process according to the claim 1, wherein the gas temperature is more a during a first stage of the process than during a second stage of the process, "before or after the first stage.

12. Process according to the claim 11, where the process is a batch process and the temperature change between the first and second stage is done over time.

13. Process according to claim 11, where "the process is a continuous process and the temperature change between the first and second stage is done along the granulation course."

14. Process according to the claim 13, when done in a plug flow granulator &

15. Process according to any of the steps 11 to 14, wherein the temperature t in the first stage is controlled to be "up to 200 ° C, preferably up to 80 ° C.

16. Process according to any of claims 10 to 14, wherein the temperature in the second stage is controlled to be at 30 ° C or less, preferably 25 ° C or less, or 5 ° C or less or -10 ° C or less .

17. Process according to claim 1, wherein the liquid binder comprises an acid precursor of an ammonium surfactant and the particulate solids comprise an inorganic alkaline material.