JPH04503369A - Detergent additive granules and their manufacturing method - Google Patents

Abstract

The detergent additive granulate comprises a core with a primary detergent additive surrounded by a shell comprising a secondary detergent additive, a binder, and granulating agents, and optionally a filler, and a protective coating between the core and the shell, whereby the shell comprises cellulose fibres or artificial fibres, and whereby the core facultatively comprises cellulose fibres or artificial fibres. The detergent additive granulate exhibits a high physical strength, and the primary and secondary detergent additives are effectively separated from each other and/or from harmful environmental factors. The detergent additive granulate is produced by introduction of the components thereof into a granulating drum. This method of production is easily controllable and adapted for an industrial scale.

Description

[Detailed description of the invention] Detergent additive granules and their manufacturing method FIELD OF THE INVENTION The present invention relates to detergent additive granules and methods of making the same.

The granulate according to the present invention and its manufacturing method are carried out in a drum granulator, as disclosed in the Danish patent. This is a further development of the granular material and its manufacturing method described in Application No. 4368/8 B. be. Drum granulators come in a wide range of categories including, for example, bread granulators and granulator mixers. It should be understood that it represents a Lee granulation device.

The enzyme-containing granulate described in Danish patent application 4368/88 consists of granules excluding the core. Contains 1.5 to 40% by weight of cellulose fibers or artificial fibers based on the dry weight of the product. The core surrounded by a coating of binder, filler and one or more granulating agents in an amount of 5% by weight; The core and/or coating includes enzymes.

The present invention is based on Danish patent application No. This is a further development of a specific aspect of the invention described in No. 88.

However, the shell or enzyme in the detergent additive granules according to the present invention does not necessarily contain enzymes. Although it does not contain, the core is a kind of detergent additive (this may be an enzyme, hereinafter referred to as the present invention). In addition, the shell contains other detergent additives (referred to as the first detergent additive). may be another enzyme (hereinafter referred to as the second enzyme in the present invention). first In cases where the additive is to be protected against secondary additives and/or environmental factors. For example, enzymes are degraded by bleach and atmospheric moisture, or vice versa. In cases where there is a need for effective separation between the first and second detergent additives during storage, Exists. In addition, the granules have high physical strength and their manufacturing method (this is controllable and adaptable on a commercial scale).

It is therefore an object of the present invention to provide detergent additive granules with high physical strength. and the granulate has first and second detergent additives of the type described above; The first and second detergent additives are free from each other and/or from harmful environmental factors. Effectively separated. Furthermore, the purpose of the present invention is to provide a system that can be easily controlled on an industrial scale. It is an object of the present invention to provide a method for producing the additive which is compatible with the present invention.

The detergent additive granules according to the present invention contain a second detergent additive, a binder and a dusting agent. a first detergent additive surrounded by a shell comprising a filler and a desired filler; a protective coating between the core and the shell, wherein the shell preferably 1.5 to 40% by weight of the shell, more preferably 5 to 20% by weight of the shell. % of cellulose fibers or man-made fibers, the core optionally comprising Preferably, the separator is used in an amount of 1.5 to 40% by weight, more preferably 5 to 20% by weight of the core. It contains lurose fiber or man-made fiber.

Two detergent additives are added to the preserved tiles for a protective coating between the core and shell. The two detergent additives are brought into contact with each other only during application during cleaning. There will be. Also, due to the content of cellulose fibers or man-made fibers in the shell, the granularity The physical strength of objects is high. Furthermore, the following contents were surprisingly found. Sunawa U.S. Patent No. 4,106, shown in the earlier Danish Patent No. 4368/88, The granulator method of manufacture carried out according to the guidelines given in 991 also Easily controllable with two non-enzymatic detergents and more amenable to industrial scale. Easy to adapt.

European patent 0286773 describes encapsulated enzymes, which include several in the detergent additive granulate according to the invention in its widest aspect. deer However, prior art encapsulated enzymes are made of reinforced cellulose fibers or man-made fibers in the shell. containing no protected by the fluidized bed method, which is well suited for industrial scale production. It doesn't match.

The protective coating does not harm the first or second detergent additive or otherwise Any protective coating used in the industry that does not interfere with the manufacturing process or application of the product. Bye. Examples of protective coatings that can be used are: fatty acid esters, Lucoxylated alcohol, polyvinyl alcohol, ethoxylated alkyl Cyphenol, polyethylene glycol (MW1000-8000), linear alkyl Cole alkoxylate (MW26000-33000), high molecular weight nonilph phenyl ethoxylate (MW1975-4315), and dinonyl phenyl ethoxylate Toxilates (average MV/6900), R fatty acids such as palmitic acid, stear Phosphoric acid, and arachidonic acid, paraffin, beeswax, wax, monofatty acids or mixed fatty acids such as triglycerides, fatty alcohols, methane, etc. cellulose, ethyl cellulose, hydroxypropyl cellulose, and tips Coconut monoethanolamide.

Examples of combinations of first and second detergent additives are: (optical brightener) - ( enzyme), (enzyme) - (fluorescent brightener), (enzyme) - (bleach activator), (bleach activator) ) - (enzyme), (bleach activator) - (optical brightener), (optical brightener) - (bleach activity) agent), (enzyme - chlorine scavenger), (bleach activator - chlorine scavenger) ), (optical brightener - chlorine scavenger), (bleach) = (enzyme), and ( enzyme) - (bleach).

In a preferred embodiment of the granulate according to the present invention, the core is the smallest between the largest dimension and the smallest dimension. The shape corresponds to a major ratio of about 3, preferably about 2, more preferably 1.5. child In this embodiment, a satisfactory coating of carbon can be easily achieved.

In a preferred embodiment of the granulate according to the invention, the amount of cores is between 5 and 85% by weight of the granulate. %, preferably 10-50% by weight, most preferably 15-40% by weight. too When the amount of core is more than 85%, it is difficult to add a sufficient amount of the second detergent additive. and, if the amount of core is less than 5%, a sufficient amount of the first detergent additive. would be difficult to add.

In a preferred embodiment of the granulate according to the present invention, the core has an average particle size of 100 to 1000. μm, preferably 200 to 700 μm. These are the most often required particle size.

In a preferred embodiment of the granulate according to the invention, the core or shell contains an enzyme. . Enzymes are typical detergent additives that need protection from clumping detergent components.

In a preferable granule according to the present invention, the enzyme is protease, amylase, etc. , lipase, amidase, cellulase or oxidase.

These are the most common enzymes for industrial detergent purposes.

In a preferred embodiment of the invention, the filler consists of or contains an inorganic salt. It becomes. This results in inexpensive granules.

In a preferred embodiment of the invention, the shell is surrounded by a final dust suppression coating. It is rare. This seems to tend to cause the shell to produce an unacceptable amount of dust. This is advantageous in certain cases. Final dust suppression coating provides further protection if present Can serve as coaching.

In a preferred embodiment of the granulate according to the invention, the protective coating is a fatty acid monomer. and a mixture of diglycerides.

It has been found that in this manner a maximum satisfactory protection effect during storage is obtained. Ta. Advantageously, the mixtures described in Danish Patent No. 1377/88 can be used.

In preferred embodiments of the granules of the invention, suitable examples of protective coatings include: Thiosulfate, sulfite, bisulfite ascorbic acid, ascorbe or butyl hydroxyl toluene. Better storage stability in many cases Qualitative properties can be obtained due to the presence of antioxidants.

The present invention also includes a method for manufacturing the granulate of the present invention.

The method of manufacturing detergent additive granules of the present invention involves introducing the cores into a granulation drum and subsequently protecting them. coating agent, shell material, and desired final dust-suppressing coating agent as well as the cell Introducing loin fiber or artificial fiber into the granulation drum in an appropriate amount and in an appropriate process. It includes.

It is understood that any granulation drum can be used in connection with the method of the invention. whole pro The cess can be carried out in one type of these granulation drums. Also, understand as follows It should be.

That is, the core is coated with a protective coating in one granulation drum and then The coated core is isolated and then transferred to another granulation drum for application to the shell. The dust suppression coating can then be applied to the same or another granulation drum if desired. It will be held in

The method of the invention can be carried out batchwise or continuously.

The invention is illustrated by the following examples, in which the active units are defined as follows.

Upon request, AF Publications is pleased to announce that Novo Nordisk A/S (Novo PL, 2880, Available from Bazgbaert, Denmark). ″ Made by star■ Example 1 The following composition (15% cellulose fiber, Arbocel BC200, 15% fluorescent whitening agent, Tinopal DMS-Xcnc, Ciba Geigy, 4% kaolin smooth ECC (112% carbohydrate binder and 54% finely divided sodium sulfate) 15 kg of a powder composition having the composition as described in Example 1 of U.S. Pat. Using pure water as a granulating agent, the mixture is granulated in a Lodige mixer at FM50.

The granulate is dried in a fluidized bed to a moisture content of 1%, and then finally reduced to a particle size of 300 μm to 9 Palmitate sieved to obtain product XR of ゛00u'm Grindetake MS Coated with a layer of P90 (melting point 68℃) and bentonite ASB350ECC Ru.

Heat the granulate to 75-80°C in a Roedige mixer 201 with a heating jacket. However, this temperature is maintained during the coating process. Mix the heated granules and then sprayed with 700g molten MSP90 then 1000g bentonite powder, then sprayed with 210g MSP90, then 1000g MSP90. Powder with SP90 and then spray with 210 g of MSP90.

Finally, the granulate was cooled to room temperature in a fluidized bed and sieved to 300-1000 μm.

Example 3 an inner core containing fluorescent bleach and an outer core containing proteolytic enzymes and A granulate with shells separated by a protective layer is produced in the following manner.

The following composition (Savinase (registered trademark) with proteolytic activity 37 KNPU/g) cnc, 2.5kg, fiber cellulose 0.5kg Albocel BC200,0, 6 kg carbohydrate binder, 0.2 kg kaolin Supeswhite ECC, and and 1.2 kg of finely divided sodium sulfate); Next, Danish patent issued 1ie! Example in the manner described in Example 1 of 436 B/88 2 and then layered. edge However, in this example, the core has an optical brightener and a 501 Rhodigemix. Sir FM5 example 4 7 kg of granulate prepared as described in Example 3 was subjected to a conventional fluidized bed coating process. coat with a layer of sodium sulfate and kaolin.

280g Sodium Thiosulfate and 280g Kaolin Besu White ECC was dissolved/dispersed in 1000 g of water and then 7 kg of Spread onto the granulate to form a continuous coating and dry.

Air inlet temperature is 50°C. Air outlet temperature is 35°C.

The process ends with a drying period of 5 minutes at an air inlet temperature of 50°C.

The granulate has a proteolytic activity of 5.2 KNPU/g.

Example 5 7 kg of granulate prepared as described in Example 4 were added to 280 g of Grindetake MS. Coated with a protective coating of P90 and then coated with <875 g of film as described in Example 2. Coat 1:1 tanium dioxide to kaolin (Speth White), then 1:1 Coat with 40 g of Grindetake MSP90.

The granulate is cooled to room temperature in a fluidized bed and then sieved to 300-1000 μm.

The granulate has a proteolytic activity of 4.7 KNPU/g.

34 and 5 - '''' - Safe at a temperature of -37 degrees and 70% humidity. Conduct qualitative tests.

The above results demonstrate increased stability of the final dust suppression and protective coating.

Example 6 The following composition (2.2 kg of fibrous cellulose, 1.2 kg of Arbocel BC200, Bentonite, ASB350, ECC, 1°8kg carbohydrate binder, 9.5k TAED) of 14.7 kg of powder composition according to the example of U.S. Patent 4.106.991. Lodige using 3.0 kg of a 2% aqueous solution of carbohydrate binder as described in 1. Granulate in mixer FM50.

The granulate was dried in a fluidized bed to a moisture content of less than 1% and finally sieved to a particle size of 300 μm. A product with a diameter of m to 900 μm is obtained.

Subsequently, 10 kg of the dried 300-9001 Im product were treated in the manner described in Example 2. 8% hydrogenated beef tallow (m, p, 59°C) and 28% kaolin (Stes White Coat with ECC).

However, beef tallow is applied in one (first) step and then kaolin is sprinkled.

Has an inner core with TAED and an outer shell with proteolytically active enzymes The granular material, in which the core and shell are separated by a protective layer, is processed by the following method. Manufacture.

10 kg of TAED-containing granules coated with beef tallow were cooled to room temperature and then Transfer to Gemixer FM50 and spray with 200g PE0300 in the first step. However, the following composition (0.6 kg of Savinase® Concentrate) , 50KNPU/g, 0.5kg fiber cellulose, Arbocel BC200,0 , 2 kg titanium dioxide, 0.3 kg 0 kaolin, space white) EC 0% 0. shell with 2 kg carbohydrate binder, 2.8 kg finely divided sodium sulfate) Prelayer with 4.6 kg of material mixture.

In a method similar to that of Danish Patent No. 4368/88, 28. Treat the shell with a 5% aqueous solution.

However, in this example the core contains a perborate activator, TAED, and 501 A Lodige mixer was used.

Finally, the granules are dried to a moisture content of less than 1% and further sieved to 300μm to 11000a. did.

Example 7 A TAED-containing granulate coated with hydrogenated tallow was prepared as described in Example 6. However, and 20% kaolin was used in the wax coating process.

having an inner core containing TAED and an outer shell containing an optical brightener; A granulate in which the wells were separated by a protective layer was produced in the following manner.

10 kg of TAED-containing granules coated with beef tallow were cooled to room temperature and then Transfer to Gemixer FM50 and spray with 200g of PEG300 in step 10. Then, the following composition (0.75 kg of optical brightener, Cinovar DMS-X, Ciba - Geigy, 0.75 kg fiber cellulose, Arbocel BC200,0,20 kg titanium dioxide, 0.30 kg bentonite ASB350, ECC, 0, 20 kg of carbohydrate binder, 2゜40 kg of finely powdered sodium sulfate) shell material It was pre-layered with 4.6 kg of the raw material mixture.

Sheet with a powder feed rate of 20 kg/h using a continuous weight loss adjusted powder feeding system. Supply to Le. In total, 1.4 kg of 28° 5% aqueous carbohydrate binder solution was to bind the powder to the surface of the core particles. On the other hand, PCT WO39108 The front layer was applied as described in Example 1 of 695.

Finally, the granules are dried to a moisture content of less than 1% and then sieved to a particle size of 300 to 900 μm. A product of m was obtained.

Example 8 as described in Example 1 of U.S. Pat. No. 4,106.991, except that this 10 kg of Sebinase® with a particle size of 300 μm to 7001 Im The granulate was coated with 8% hydrogenated beef tallow and 26% kaolin as described in Example 6. did.

Inner core containing proteolytic enzyme Sabinase® and outer core containing optical brightener A granule having a shell, the core and the shell being separated by a protective layer, is prepared by the following method. Manufactured.

10 kg of Sabinase (registered trademark)-containing granules coated with beef tallow were cooled to room temperature. Next, it was transferred to a Lodige mixer FM50 and further added with 200 g of PEG3 in the first step. 00, followed by the following composition (1.5 kg of optical brightener, Tinopal DM S-X1 Civer Geigy, 1. 0kg fiber cellulose, Arbocel BC20 0,0,4 kg of titanium dioxide, 0. 6kg (7) Kaolin stes white, ECC, 0.40 kg carbohydrate binder, 5.3 kg finely divided sodium sulfate) The shell material mixture was pre-layered with 9.2 kg of shell material mixture.

Sheet with a powder feed rate of 20 kg/h using a continuous weight loss adjusted powder feeding system. Supply to Le. In total, 2.6 kg of 26°2% aqueous carbohydrate binder solution was and otherwise proceed as described in Example 1 of PCT WO39108695. It was.

Finally, the granules are dried to a moisture content of less than 1% and then sieved to a particle size of 300 to 900 μm. A product of m was obtained.

Example 9 As described in Example 1 of U.S. Pat. No. 4,106,991 (although this 10 kg of Savinase® with a particle size of 300 μm to 1000 μm The granulate was coated with 10% hydrogenated beef tallow and 30% kaolin as described in Example 6. I did it.

Inner core containing proteolytic enzyme Savinase® and chlorine scavenger - a granulate having a containing outer shell, said core and said shell being separated by a protective layer; It was manufactured by the following method.

10 kg of Sabinase (registered trademark)-containing granules coated with beef tallow were cooled to room temperature. Next, the mixture was transferred to a Lodige mixer FM50 at 60°C, and heated to 60°C in a mixer shear heating kerato. A separate layer process core temperature was maintained using 0°C hot water.

The following composition (6.8 kg ammonium sulfate, 1.0 kg fibrous cellulose, aluminum Bothell BC200, 0, 20kg titanium dioxide, 0.7kg0 kaolin base White, ECC, 0,5 kg carbohydrate binder) shell material mixture 9.2k g using a continuous weight loss-adjusted powder feeding system at a powder feeding rate of 50 kg/h. , in total, 2.1 kg of 34.7% aqueous carbohydrate binder solution (the binder solution was (slightly acidified with 0.7% citric acid to suppress ammonia generation/odor during granulation) supplied. On the other hand, as described in Example 1 of PCT WO39108695, Applied.

Finally, the granules are dried to a moisture content of less than 1% and then sieved to a particle size of 300-1000. A μm product was obtained.

Example 1O as described in Example 1 of U.S. Pat. No. 4,106.991, except that this 10 kg of Sabinase (based on Trademark) granulate with 5% hydrogenated beef tallow and 15% kaolin as described in Example 6. I coated it.

Inner core containing proteolytic enzyme Savinase® and chlorine scavenger - a granular material having a containing outer shell, said core and said L being separated by a protective layer; was prepared as described in Example 9.

Example 11 as described in Example 1 of U.S. Pat. No. 4,106.991, except that this Particle size: 300 μm to 10. O08m 10kg Sabinase (registered trademark) ) The granulate was co-coated with 3% hydrogenated beef tallow and 10% kaolin as described in Example 6. I started.

Example 12 as described in Example 1 of U.S. Pat. No. 4,106.991, except that this 10 kg of Savinase® with a particle size of 300 μm to 1000 μm The granulate was treated with 5% hydrogenated fatty acids (m, p, 58°C) and 1% as described in Example 6. Coated with 6% kaolin.

Inner core containing proteolytic enzyme Alcalase® and chlorine scavenger granulate having a carrier-containing outer shell, said core and said shell being separated by a protective layer; was produced by the following method.

Cool 10 kg of Alcalase (registered trademark)-containing granules coated with beef tallow to room temperature. Then, transfer to a Roedige mixer FM50 for 60" and place in the mixer heating jacket. A separate layer process core temperature was maintained using hot water at 60°C.

The following composition (7.0 kg ammonia sulfate, 1.0 kg fibrous cellulose, albo Cell BC200, 0.7kg kaolin, Supes White, ECC, 0.5kg 9.2 kg of a shell material mixture of (carbohydrate binder) was applied as described in Example 9. .

Finally, the granules are dried to a moisture content of less than 1% and then sieved to a particle size of 300-1100. A product of 0u was obtained.

PA eyebrow test for t of 910 and 11: Chlorine scavenger-containing Cleaning test principle using particulate matter: Torque autometer, 1000rpra water : 6°dH (33% tap water, 67% deionized water) Temperature: 40°C Time: 15 minutes, wash after 15 minutes, add Na, S, O, to all beers ( (over a period of 14 minutes) then rinse the swatch.

Detergent: Ig/IUs base powder p! (: Measured at 9.2 Textile/liquid Ratio: 8 swatches/800o+1 (dimensions of each swatch 7X7c+w) Rinse = 10 minutes + 15 minutes, running water Test material: pre-rinsed Nishikigami grass Enzyme: Sabinase (registered trademark) (control) 7. 04 KNPU(S)/g Sabinase Granules, Example 9 3. 84 KNPU(S)/g Savinase granules, Example 10 4.60 KNPU(S)/g Savinase Granules, Example 11 4. 61 KNPU(S)/g enzyme dose: O~0. 09KNPU/1 hypochlorite Dose: O ~ 4.5 ~ 9.0 ppm Na0C1 repetition: twice independently Eshi Comments: Dissolve the detergent and then heat to 40°C in a torque-automator.

Add Na0Cl, enzyme and test swatch in the order indicated within 60 seconds.

Boar training The doses of hypochlorite are actually not exactly the same, but Performance is observed and is measured by ΔR. 4.5 ppm of hypochlorite At doses, the performance of the control Sabinase® was reduced to half the performance (measured by Δ). decrease, while the three granules obtained from the examples still show the highest performance. high dose No significant enzyme performance is observed with respect to the control with hypochlorous acid. Obtained in Example 9 The particulate matter is approximately Shows 50% performance.

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Claims (11)

[Claims] 1. comprising a second detergent additive, binder and granules and desired fillers; a core having a first detergent additive surrounded by a shell and the core and the shell; a protective coating between the shells, wherein the shell preferably comprises a protective coating between the shells. ．． Cellulose fibers or fibers in an amount of 5 to 40% by weight, more preferably 5 to 20% by weight. the core optionally preferably has a content of 1.5 to 40% of the core. Contains cellulose fibers or man-made fibers in an amount of % by weight, more preferably 5-20% by weight. Detergent additive granules. 2. The core has a maximum ratio of the largest dimension to the smallest dimension of about 3, preferably about 2, more preferably The granule according to claim 1, having a shape corresponding to 1.5 mm. 3. The amount of core is 5 to 85% by weight of the granulate, preferably 10 to 50%, most preferably Granules according to claim 1 or 2, preferably from 15 to 40% by weight. 4. The core has an average particle size of 100 to 1000 μm, preferably 200 to 700 μm. The granular material according to any one of claims 1 to 3. 5. Claims 1 to 4, wherein the core or shell contains an enzyme. granular matter. 6. Enzymes include protease, amylase, lipase, acidase, cellulase, and The granular material according to any one of claims 1 to 5, which is iomosidase and/or omosidase. . 7. Claims 1 to 3, wherein the filler consists of or contains an inorganic salt. The granular material according to any of Item 6. 8. Claim 1, wherein the shell is surrounded by a final dust suppression coating. The granular material according to any one of items 1 to 7. 9. Claim wherein the protective coating is a mixture of mono- and diglycerides of fatty acids. The granule according to any one of items 1 to 8. 10. Any of claims 1 to 9, wherein the protective coating is an antioxidant. Particulate matter described in. 11. A method for producing a granule according to any one of claims 1 to 10, comprising: The core is introduced into the granulation drum, followed by the protective coating, shell material, and the desired final dust-suppressing coating, plus appropriate amounts of cellulose fibers or man-made fibers. and introducing it into a granulation drum in a suitable step.