Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
  • C11D17/065—High-density particulate detergent compositions
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
  • C11D11/04—Special methods for preparing compositions containing mixtures of detergents by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/128—Aluminium silicates, e.g. zeolites

Definitions

• the present invention relates to a process for preparing a high-bulk density detergent composition having excellent detergency, and a small average particle size.
• Japanese Patent Laid-Open No. Hei 3-33199 discloses a method of producing a detergent composition comprising the steps of dry-neutralizing components in a high speed mixer/granulator at a temperature of 55°C or less, and thereafter adding a liquid binder thereto to carry out granulation.
• Japanese Patent Laid-Open No. Hei 4-363398 discloses a method of producing a detergent composition comprising the steps of dry-neutralizing components in a high speed mixer/granulator at a temperature of 55°C or more, and then adding a liquid binder thereto to cany out granulation.
• an object of the present invention is to provide a process for preparing a high-bulk density detergent composition having excellent detergency, and a small average particle size.
• step (B) adding an inorganic powder to a neutralization mixture in step (A) after a point of initiation of formation of coarse grains of the neutralization mixture obtained during a course of a neutralization process in step (A) and mixing a resulting mixture; and [2] a process for preparing a high-bulk density detergent composition having a bulk density of 650 g/L or more, comprising the steps of: (a) blending a liquid acid precursor of an anionic surfactant with a water- soluble, alkali inorganic substance in an amount equal to or exceeding in an amount necessary for neutralizing the liquid acid precursor, in a substantial absence of an alkali metal aluminosilicate, thereby neutralizing the liquid acid precursor; and (b) adding an alkali metal aluminosilicate to a neutralization mixture obtained in step (a) and mixing a resulting mixture.
• the process for preparing a high-bulk density detergent composition of the present invention is roughly classified into the following two embodiments.
• a process for preparing a high-bulk density detergent composition having a bulk density of 650 g/L or more comprising the steps of:
• step (B) adding an inorganic powder to a neutralization mixture in step (A) after a point of initiation of formation of coarse grains of the neutralization mixture obtained during a course of a neutralization process in step (A) and mixing a resulting mixture.
• step (b) adding an alkali metal aluminosilicate to a neutralization mixture obtained in step (a) and mixing a resulting mixture.
• Step (A) or step (a) is a step in which essentially the same operations are carried out.
• the liquid acid precursor of an anionic surfactant usable in step (A) or step (a) refers to those anionic surfactants in the form of acids in a liquid or pasty state at room temperature or with heating, which are formed into salts by neutralization reaction.
• the liquid acid precursor of an anionic surfactant includes linear alkylbenzenesulfomc acids (LAS), ⁇ -olef ⁇ n sulfonic acids (AOS), alkyl sulfuric acids (AS), internal olefin sulfonic acids, sulfonic acids of fatty acid esters, alkylether sulfuric acids, dialkyl sulfosuccinic acids, and the like.
• the liquid acid precursors may be used in a combination of two or more components.
• the amount of the liquid acid precursor of an anionic surfactant can be appropriately set depending upon the composition of the desired detergent composition.
• the amount of the liquid acid precursor of an anionic surfactant, as an anionic surfactant formed by the neutralization reaction is preferably from 5 to 55% by weight, more preferably from 5 to 45% by weight, still more preferably from 10 to 40% by weight especially preferably from 20 to 40% by weight, of the final high-bulk density detergent composition.
• the present invention is effective also in a case where the main surfactant is supplied in another form in the detergent composition.
• the water-soluble, alkali inorganic substance usable in step (A) or step (a) exhibits an alkaline property which can neutralize the liquid acid precursor of an anionic surfactant.
• the water-soluble, alkali inorganic substance described above includes sodium carbonate, sodium hydrogencarbonate, sodium silicate, potassium carbonate, calcium carbonate, and the like.
• preference is given to sodium carbonate because the sodium carbonate can act as a detergent builder and an alkalizing agent in the final detergent composition. Therefore, it is preferable to add the water-soluble, alkali inorganic substances in step (A) or step (a) in an amount equal to or exceeding in an amount necessary for neutralizing the liquid acid precursor of an anionic surfactant.
• the water-soluble, alkali inorganic substance is added in an amount of preferably from 1 to 20 times the equivalent amount required for neutralization of the liquid acid precursor of an anionic surfactant, more preferably from 2 to 15 times the equivalent amount required for neutralization, especially preferably from 3 to 15 times the equivalent amount required for neutralization.
• the water-soluble, alkali inorganic substance is preferably granular, and its average particle size is preferably 30 ⁇ m or more, more preferably from 40 to 200 ⁇ m, most preferably from 50 to 100 ⁇ m, from the viewpoints of the yield improvements and the storage stability.
• the average particle size of the granular, water-soluble, alkali inorganic substance is evaluated based on volume, wherein the average particle size is measured by using a laser diffraction particle size distribution analyzer ("LA-700," commercially available from HORIBA Ltd.).
• LA-700 laser diffraction particle size distribution analyzer
• the phrase "the substantial absence of the alkali metal aluminosilicate” refers to a case where the content of the alkali metal aluminosilicate in step (A) or step (a) is preferably 5% by weight or less, more preferably 3% by weight or less, of the neutralization mixture in step (A) or step (a).
• the alkali metal aluminosilicate exists in a large amount in step (A) or step (a)
• the deterioration and the aggregation of the alkali metal aluminosilicate by the contact with a liquid acid precursor of an anionic surfactant in an acid form take place, so that the detergency performance in the resulting detergent composition is likely to be lowered thereby. Therefore, the above problem can be eliminated by carrying out the mixing operation under specified conditions of the substantial absence of the alkali metal aluminosilicate.
• Embodiment 1 also encompasses an embodiment where the addition of the alkali metal aluminosilicate of step (B) is initiated at during the course of the neutralization process of step (a), or at a point where the amount of the liquid acid precursor of an anionic surfactant added exceeds a certain level.
• step (A) or step (a) besides the water-soluble, alkali inorganic substance and the liquid acid precursor of an anionic surfactant, a part or all of optional ingredients can be added.
• Optional ingredients which can be blended at this step include, for instance, fluorescers, pigments, anti-redeposition agents (polycarboxylate polymers, sodium salt of carboxymethyl cellulose, and the like); surfactants (fatty acids or salts thereof, linear alkylbenzenesulfonates, alkyl sulfates, and the like); diatomaceous earth, calcite, kaolin, bentonite, tripolyphosphates, sodium sulfate, sodium sulfite, and the like.
• the average particle size of the tripolyphosphates is not particularly limited, and the average particle size is preferably from 1 to 30 ⁇ m, more preferably from 5 to 20 ⁇ m, still more preferably from 6 to 15 ⁇ m. From the viewpoint of inhibiting the aggregation of the detergent granules, the smaller the average particle size of the tripolyphosphate, the smaller the average particle size of the detergent granules.
• the average particle size of the tripolyphosphate is preferably 1 ⁇ m or more, and from the viewpoint of inhibiting the aggregation of the detergent granules, the average particle size is preferably 30 ⁇ m or less.
• the average particle size of the tripolyphosphate as referred to in the present specification is evaluated based on volume, wherein the average particle size is measured by using a laser diffraction particle size distribution analyzer ("LA-700," commercially available from HORIBA Ltd.).
• the optional ingredients which are added in step (A) or step (a) are preferably those in a granular or powdeiy state, and those prepared by pulverizing a lumpy mass, or those which are separately granulated may be used.
• the average particle size of the optional ingredients is preferably 200 ⁇ m or less.
• the optional ingredients may be added as an aqueous solution, paste or slu ⁇ y. However, in order to prevent excessive aggregation, when water is contained, its amount is preferably adjusted so as not to exceed the water content described below.
• step (A) or step (a) When the above optional ingredients are added, it is preferable that the optional ingredients are previously blended with the water-soluble, alkali inorganic substance before neutralizing in step (A) or step (a).
• the extent of mixing is preferably such that each of the ingredients is uniformly mixed.
• the operation conditions for the agitation granulator are, for instance, a mixing time period of within 5 minutes.
• water may be added for the purpose of accelerating the neutralization reaction.
• the amount of water added is preferably from 0.2 to 3 parts by weight, more preferably from 0.5 to 1.5 parts by weight, based on 100 parts by weight of the water-soluble, alkali inorganic substance (and in a case where optional ingredients are added, their weights on dry basis are added) in step (A) or step (a).
• the amount of water is preferably 0.2 parts by weight or more, from the viewpoint of initiating the neutralization reaction, and the amount is preferably 3 parts by weight or less, from the viewpoint of suppressing the aggregation of the detergent granules.
• the amount of water to be added may be determined in consideration of these water contents.
• an aqueous alkali solution or an alkali slurry solution (hereinafter simply referred to as "alkali solution”) can be preferably used in place of water mentioned above.
• alkali solution By using the alkali solution, not only the neutralization reaction can be more accelerated as compared to the case of using water, but also the particle size of the resulting detergent granules can be made small, whereby the bulk density can be markedly increased.
• the alkali solution is added in an amount of preferably from 0.05 to 0.5 times the equivalent amount required for neutralization of the liquid acid precursor of an anionic surfactant, more preferably from 0.10 to 0.45 times the equivalent amount required for neutralization, especially preferably from 0.10 to 0.40 times the equivalent amount required for neutralization.
• the amount is preferably 0.05 times or more the equivalent amount required for neutralization, and from the viewpoint of suppressing the aggregation of the detergent granules, the amount is preferably 0.5 times or less the equivalent amount required for neutralization.
• the concentration of the alkali solution is preferably from 20 to 50% by weight, more preferably from 30 to 50% by weight, especially preferably from 40 to 50% by weight.
• the kinds of the alkalizing agent used in the alkali solution include strongly alkali aqueous solutions, such as aqueous sodium hydroxide and aqueous potassium hydroxide, which can readily cause the neutralization reaction with the liquid acid precursor of an anionic surfactant.
• the aqueous sodium hydroxide is favorably used from the viewpoint of costs.
• the alkali aqueous solution more preferably has a pH of 12 or more, and it is preferable that the alkali solution is added by spraying or dropping to an extent that the alkali solution uniformly disperses when added. It is preferable that the alkali solution is added to a mixture of a water-soluble, alkali inorganic substance and other optional ingredients before blending with the liquid acid precursor of an anionic surfactant.
• step (A) or step (a) it is preferable to previously add an inorganic acid, for example, sulfuric acid, and the like, to the liquid acid precursor of an anionic surfactant.
• an inorganic acid for example, sulfuric acid, and the like
• the resulting granules have low adhesiveness and small particle sizes, whereby the granules having a high surfactant content can be prepared without causing the aggregation of the granules.
• the granules obtainable in the manner described above have a large number of micropores
• the granules having a high content of liquid ingredients, such as a nonionic surfactant can be prepared.
• the inorganic acid is added in an amount of preferably from 0.1 to 1.0 moles, more preferably from 0.1 to 0.8 moles, still more preferably from 0.15 to 0.75 moles, especially preferably from 0.2 to 0.7 moles, most preferably from 0.25 to 0.65 moles, per one mol of the liquid acid precursor of an anionic surfactant.
• the inorganic acid is added in an amount of 0.1 moles or more, per one mol of the liquid acid precursor, from the viewpoint of suppressing the formation of coarse grains of the detergent granules, and that the inorganic acid is added in an amount of preferably 1.0 mole or less, per one mol of the liquid acid precursor, from the viewpoint of securing the degree of freedom in the formulation composition of the concentrated detergent.
• the order of adding the liquid acid precursor of an anionic surfactant and the water-soluble, alkali inorganic substance is not particularly specified. It is preferable that the liquid acid precursor is added to the water-soluble, alkali inorganic substance.
• the method of adding the liquid acid precursor of an anionic surfactant may be carried out continuously or in a plurality of batches, and the plural addition means may be provided.
• step (A) or step (a) is carried out by using an agitation granulator.
• the agitation granulators are equipped with agitation blades and a chopper for disintegration and dispersion (or those replaced with a functionally equivalent means).
• agitation granulators usable in the present invention for a batch process include Vertical Granulator (commercially available from Powrex Corp.); High-Speed Mixer (commercially available from Fukae Powtec Kogyo Corp.); Lodige Mixer (commercially available from Matsuzaka Giken Co., Ltd.); and PLOUGH SHARE Mixer (commercially available from PACIFIC MACHINERY & ENGINEERING Co., LTD.); Gericke Mixer (commercially available from Meiji Machine Co., Ltd.), and the like, and the Lodige Mixer and the PLOUGH SHARE Mixer are especially preferable.
• Vertical Granulator commercially available from Powrex Corp.
• High-Speed Mixer commercially available from Fukae Powtec Kogyo Corp.
• Lodige Mixer commercially available from Matsuzaka Giken Co., Ltd.
• PLOUGH SHARE Mixer commercially available from PACIFIC MACHINERY & ENGINEERING Co., LTD
• CB recycler commercially available from Lodige
• Turbilizer commercially available from Hosokawa Micron Corporation
• Shugi Mixer commercially available from Powrex Corp.
• Flow Jet Mixer commercially available from Funken Powtechs, Inc.
• the above mixers may be appropriately used in combination.
• the neutralization reaction by the blending of the water-soluble, alkali inorganic substance and other optional ingredients and the neutralization reaction by the addition of the liquid acid precursor of an anionic surfactant may be treated in different agitation granulators.
• the agitation granulator used in the present invention is equipped with a jacket for adjusting the internal temperature of the granulator or is equipped with a nozzle for blowing a gas into the agitation granulator.
• Concrete examples of the more preferable agitation granulators include those mixers disclosed in Japanese Patent Laid-Open Nos. Hei
• step (A) or step (a) it is preferred that the neutralization is carried out while blowing a gas into an agitation granulator.
• a gas By blowing a gas into the agitation granulator, the excess water produced in the neutralization reaction can be evaporated and the resulting granular product can be cooled with the gas, to thereby inhibit the granular product from forming into a doughy mass.
• the gases which may be usable include an N 2 gas, air, and the like.
• the amount of gas blown (amount of gas flow) is not particularly limited. The gas is blown at a rate of preferably equal to or greater than 0.002 parts by weight per minute, more preferably equal to or greater than 0.02 parts by weight per minute, based on 100 parts by weight of the granular product.
• neutralization mixture Especially when a detergent containing a surfactant in a ratio exceeding 20% by weight to the final detergent composition is prepared, the detergent granules are likely to form coarse grains or become lumpy, so that it is preferable to provide a disintegration process for the purpose of obtaining a detergent composition having a small particle size.
• the disintegration process when the content of the anionic surfactant is 30% by weight or more, of the neutralization mixture, it is preferable to provide the disintegration process.
• the method for disintegration may be carried out subsequently to step (A) or step (a) in the agitation granulator equipped with agitation blades and a chopper for disintegration and dispersion, or the method may be earned out by a separate disintegrator.
• the disintegrator include Fitz Mill (commercially available from Hosokawa Micron Corporation), Speed Mill (commercially available from Okada Seiko K.K.), and the like.
• Step (B) comprises adding an inorganic powder to a neutralization mixture in step (A) after a point of initiation of formation of coarse grains of a neutralization mixture obtained during a course of a neutralization process in step (A) and mixing a resulting mixture.
• the addition of the inorganic powder is initiated at any time after a point when the liquid acid precursor of an anionic surfactant is added in an amount exceeding a weight ratio of 0.25, preferably an amount exceeding a weight ratio of 0.3, to the water-soluble, alkali inorganic substance. This is because the formation of coarse grains of the neutralization mixture is initiated at this point. Further, from the viewpoint of suppressing the compactification and the formation of coarse grains of the neutralization mixture by the progress of the granulation after the termination of the neutralization, it is desired that the inorganic powder is added within a short time period from the termination of addition of an entire amount of the liquid acid precursor of an anionic surfactant, for instance, within 5 minutes. Within the above range, the disintegration of the neutralization mixture can be facilitated by initiating the addition of the inorganic powder within this range.
• the inorganic powder usable in step (B) has an average particle size of 30 ⁇ m or less, preferably 20 ⁇ m or less, from the viewpoint of suppressing the aggregation of the detergent granules.
• the average particle size of the inorganic powder is evaluated based on volume, wherein the average particle size is measured by using a laser diffraction particle size distribution analyzer ("LA-700," commercially available from HORIBA Ltd.).
• LA-700 laser diffraction particle size distribution analyzer
• examples of the inorganic powder include inorganic powdery builders and fine granular components generally usable in detergent compositions.
• alkali metal aluminosilicates examples thereof include alkali metal aluminosilicates, tripolyphosphates, crystalline silicates, sodium sulfate, calcite, diatomaceous earth, silica, and the like.
• the inorganic powders may be used in combination of two or more kinds.
• the alkali metal aluminosilicate is especially preferable.
• the alkali metal aluminosilicate may be either amorphous or crystalline, and those having a metal ion capturing ability as a detergent aid are preferable, and especially those generally so-called "synthetic zeolite" in the field of detergent are preferable.
• the alkali metal aluminosilicate has an average particle size of preferably from 1 to 30 ⁇ m, more preferably from 10 ⁇ m or less.
• the alkali metal aluminosilicate is added at any point after the termination of the addition of an entire amount of the liquid acid precursor of an anionic surfactant, preferably after any point between a point where the agitation granulator is operated for additional 30 seconds or more, more preferably 1 minute or more, and a point up to 5 minutes from the termination of addition of an entire amount of the liquid acid precursor of an anionic surfactant.
• the neutralization reaction can be favorably completed.
• the liquid acid precursor of an anionic surfactant since the liquid acid precursor of an anionic surfactant is already neutralized, its deterioration and aggregation would not take place even if the alkali metal aluminosilicate were added. Therefore, the lowering of the detergency performance of the resulting detergent composition can be suppressed, so that there can be sufficiently exhibited an effect by the addition of the alkali metal aluminosilicate, namely the effect of improving the metal ion capturing ability and the supporting ability of the liquid ingredients.
• Step (b) comprises adding an alkali metal aluminosilicate to a neutralization mixture obtained in step (a) and mixing a resulting mixture.
• the neutralization mixture obtained in step (a) referred to herein is a mixture in which an entire amount of the liquid acid precursor of an anionic surfactant is added, and it is preferable those in which the neutralization is terminated.
• the alkali metal aluminosilicate usable in step (b) may be the same ones as those of step (B).
• step (b) it is preferable that the addition of the alkali metal aluminosilicate is initiated in step (b) at any time within 5 minutes from the teirnination of the addition of an entire amount of the liquid acid precursor of an anionic surfactant, from the viewpoint of suppressing the compactification and the formation of coarse grains of the neutralization mixture by the progress of the granulation after the termination of the neutralization process.
• the alkali metal aluminosilicate is added at any point after the termination of the addition of an entire amount of the liquid acid precursor of an anionic surfactant, preferably after any point between a point where the agitation granulator is operated for additional 30 seconds or more, more preferably
• the neutralization reaction can be favorably completed. According to the above process, since the liquid acid precursor of an anionic surfactant is already neutralized, its deterioration and aggregation would not take place even if the alkali metal aluminosilicate were added.
• the lowering of the detergency performance of the resulting detergent composition can be suppressed, so that there can be sufficiently exhibited an effect by the addition of the alkali metal aluminosilicate, namely the effect of improving the metal ion capturing ability and the supporting ability of the liquid ingredients.
• the amount of the inorganic powder usable in step (B) or the alkali metal aluminosilicate usable in step (b) is preferably from 5 to 50% by weight, more preferably from 8 to 40% by weight, especially preferably from 10 to 36% by weight, of the high-bulk density detergent composition, which is the final product. From the viewpoint of suppressing the aggregation of the neutralization mixture, the amount is preferably 5% by weight or more, and from the viewpoint of securing the degree of compositional freedom of the resulting detergent composition, the amount is preferably 50% by weight or less.
• a method of adding an inorganic powder or alkali metal aluminosilicate includes adding it at once or in a plurality of divided portions.
• Embodiments for adding in a plurality of divided portions include (i) an embodiment of adding an inorganic powder or alkali metal aluminosilicate for the pmpose of facilitating disintegration when the neutralization mixture obtained in step (A) or step (a) is formed into coarse grains or lumpy masses (addition as a disintegration aid); (ii) an embodiment of adding an inorganic powder or alkali metal aluminosilicate for the purpose of adjusting the granulation property when adding the liquid binder described below (addition as a granulation adjustment agent); and (iii) an embodiment of adding an inorganic powder or alkali metal aluminosilicate before the surface modification of the finally obtained detergent granules (addition as a surface modifier).
• step (B) or step (b) from the viewpoints of the reduction of fine powder and the improvements in the detergency and the metal ion capturing ability, it is desirable to formulate a liquid binder.
• the neutralization mixture can be made to have a small particle size, so that greater amounts of the liquid binder can be formulated.
• the term "liquid binder" in the present invention refers to a substance imparting a property of increasing the bulk density of the detergent composition by collectively assembling the granules by the formulation of the liquid binder.
• the liquid binder includes, for instance, optional liquid ingredients in the detergent composition such as water, liquid nonionic surfactants, aqueous solutions of water-soluble polymers (polyethylene glycols, acrylic acid-maleic acid copolymers, and the like), and fatty acids.
• liquid binders may be used in combination of two or more kinds, and embodiments of such addition methods include (1) adding after previously mixing two or more liquid binders; (2) simultaneously adding each of the liquid binders; and (3) alternately adding each of the liquid binders. In any of these methods, from the viewpoints of cost reduction, it is preferable to use water in combination.
• the amount of the liquid binder formulated is preferably 20 parts by weight or less, more preferably 15 parts by weight or less, based on 100 parts by weight of the neutralization mixture, from the viewpoint of suppressing the aggregation of the detergent composition.
• the method of adding the liquid binder may be carried out continuously or in a plurality of batches. It is preferable that the liquid binder is added to the neutralization mixture obtained in step (A) or step (a) before or after the addition of the inorganic powder. By the addition of the liquid binder at this stage, the adhesiveness of the granular surface by the liquid binder can be reduced, whereby the granulation can be suppressed.
• the optional ingredients can also be formulated in step (B) or step (b).
• the optional ingredients can also be formulated in step (B) or step (b).
• the aqueous solution in step (B) or step (b) rather than in step (A) or step (a), from the viewpoint of granulation property.
• the inorganic powder can be added in plural batches as shown in the above embodiments (i) to (iii), so that the granulation property is not greatly affected by the water content carried by the optional ingredients into the neutralization mixture.
• a surface-modifying step as shown in the above embodiment (iii).
• the surface modification step can be also carried out by using the inorganic powder such as an alkali metal aluminosilicate.
• the inorganic powder such as an alkali metal aluminosilicate.
• the amount of the surface modifier is from 2 to 15% by weight, preferably from 4 to 12% by weight, of the detergent composition after the surface modification.
• such components may be added after at a point where at least the first batch of the inorganic powder or alkali metal aluminosilicate is added in step (B) or step (b) in the present invention, and the particle sizes are evenly sized, or these components may be after-blended by mixing the granules finally treated with a surface-coating agent by using a mixer such as a rotary mixer.
• the high-bulk density detergent composition obtained by the process of the present invention may be used as ingredients for constituting other detergent compositions.
• the process of the present invention can be earned out by a continuous process.
• step (A) or step (a) can be carried out using, for instance, a high-speed mixer such as CB recycler, and thereafter, step (B) or step (b) can be carried out using, for instance, a moderate-speed mixer such as continuous Lodige Mixer.
• a high-bulk density detergent composition comprising a granular mixture having a bulk density of 650 g/L or more, the detergent composition having excellent detergency and a small average particle size, can be obtained.
• the high-bulk density detergent composition obtained by the process of the present invention has the following properties.
• Average particle size Measured by vibrating a sample with each of standard sieves according to JIS Z 8801 for 5 minutes, and thereafter determining from a weight percentage depending upon the size openings of the sieves.
• the average particle size is preferably 700 ⁇ m or less, more preferably 650 ⁇ m or less.
• Bulk density Preferably from 650 to 950 g/L, more preferably from 700 to 900 g/L.
• the bulk density is measured by a method according to JIS K 3362.
• the flowability of the detergent composition in the present specification is expressed as flow time which is defined as a time period required for dropping 100 mL of a powdery detergent composition from a hopper used in the determination of the bulk density according to JIS K 3362.
• the flow time is preferably 8 seconds or shorter, more preferably 7 seconds or shorter.
• the detergency is expressed a relative detergency ratio.
• the relative detergency ratio is preferably 0.95 or more, more preferably 0.98 or more. The more the relative detergency ratio approximates 1, the less the affect of the process to individual ingredients.
• the relative detergency ratio is obtained as follows.
• a detergent composition to be tested is dissolved in water, to give an aqueous solution of the detergent composition. This solution is refened to as
• test detergent aqueous solution an aqueous solution having the same composition as the test detergent aqueous solution is obtained by adding and mixing the individual ingredients constituting the detergent composition with water. This aqueous solution is refened to as "control detergent aqueous solution.”
• control detergent aqueous solution The detergency of the test detergent aqueous solution and the detergency of the control detergent aqueous solution are obtained by the following detergency test. Thereafter, the relative detergency ratio is obtained by: Detergency of
• An artificially stained cloth is prepared by smearing an artificial soil solution having the composition shown in Table 1 to a cloth.
• the smearing of the artificial soil solution to a cloth is carried out in accordance with Japanese Patent Laid-Open No. 7-270395 wherein the artificial soil solution was printed on a cloth by a gravure staining machine equipped with a gravure roll coater.
• the conditions for smearing the artificial soil solution to a cloth to prepare an artificially stained cloth are a cell capacity of a gravure roll of 58 cm /cm , a coating speed of 1.0 m/min, a drying temperature of 100°C, and a drying time of one minute.
• #2003 calico manufactured by Tanigashira Shoten
• Pentadecanoic Acid 2.31% by weight
• washing conditions are concretely as follows: the washing time: 10 minutes, the detergent concentration: 0.083% by weight; water hardness: 5°DH; water temperature: 20°C; rinsing: with tap water for 5 minutes.
• the detergency was evaluated by measuring the reflectance at 550 nm of the original cloth before staining and those of the stained cloth before and after washing by an automatic recording colorimeter (manufactured by SHIMADZU CORPORATION), and the detergency (%) was calculated by the following equation. The average value determined of 5 pieces was expressed as the detergency (%).
• Zeolite 4A manufactured by Tosoh Corporation
• nonionic surfactant there was used a polyoxyethylene alkyl ether (prepared by adding ethylene oxide in an average of 8 moles to a primary alcohol of which alkyl moiety has 12 to 14 carbon atoms (average being 12.8)); as a fatty acid, there was used palmitic acid; and as the acrylic acid-maleic acid copolymer, there was used one having a weight-average molecular weight of about 70000 as determined by gel permeation method using a polyethylene glycol as a standard.
• a detergent composition having a composition shown in Table 2 was prepared in an amount of 35 kg for each unit, using a Lodige Mixer "FKM-130D" (manufactured by Matsubo Co., Ltd.). This mixer was equipped with agitator blades; a shearing device conesponding to a chopper for disintegration and dispersion; and a jacket for adjusting the temperature within the mixer. The operations were carried out as follows. ⁇ Powder Blending>
• Solid ingredients comprising 13.19 parts by weight of sodium carbonate ("LIGHT ASH,” manufactured by Central Glass Co., Ltd.; average particle size: 56.1 ⁇ m), and 0.11 parts by weight of a fluorescer, were blended for one minute with the above Lodige Mixer under the conditions of a rotational speed of agitator blades of 130 rotations/min (peripheral speed: 3.4 m/s) and a rotational speed of a shearing device of 2850 rotations/min (peripheral speed: 27 m/s).
• LIGHT ASH sodium carbonate
• a rotational speed of agitator blades of 130 rotations/min
• a rotational speed of a shearing device 2850 rotations/min
• a zeolite (5.00 parts by weight) having an average particle size of 4 ⁇ m was added, while the mixer was operated under the same conditions as above, and mixing was carried out for 5 minutes.
• the resulting mixture was subjected to a surface modification treatment by adding the zeolite (3.50 parts by weight) having an average particle size of 4 ⁇ m to the mixer as a surface modifier, and operating the mixer for additional one minute.
• the granules of the resulting detergent composition had an average particle size of 640 ⁇ m, a bulk density of 795 g/L, and a flowability of 7.1 seconds, whereby showing excellent powder properties.
• the granules had a relative ratio for the detergency rate of 0.998, whereby showing excellent detergency.
• Example 2 Using a rotary mixer, an enzyme (0.18 parts by weight) and the detergent composition obtained above were mixed, and a perfume (0.07 parts by weight) was further sprayed thereto, to give a final powder of the high-bulk density detergent composition.
• an enzyme (0.18 parts by weight) and the detergent composition obtained above were mixed, and a perfume (0.07 parts by weight) was further sprayed thereto, to give a final powder of the high-bulk density detergent composition.
• a detergent composition having a composition shown in Table 2 was prepared in an amount of 35 kg for each unit, using a Lodige Mixer "FKM-130D” (manufactured by Matsubo Co., Ltd.). This mixer basically had the same construction as that described in Example 1.
• Example 1 (the same “LIGHT ASH” as in Example 1), and 0.11 parts by weight of a fluorescer, were blended for one minute with the above Lodige Mixer under the same conditions as in Example 1.
• Example 2 In the same manner as in Example 1, a zeolite (5.00 parts by weight) having an average particle size of 4 ⁇ m was added, and mixing was carried out for 5 minutes.
• Example 2 In the same manner as in Example 1, the nonionic surfactant (0.98 parts by weight), the zeolite (2.00 parts by weight) having an average particle size of 4 ⁇ m, and the 40% by weight aqueous solution of acrylic acid-maleic acid copolymer (effective ingredient: 1.49 parts by weight) were added to the mixer, and the ingredients were blended. Subsequently, the resulting mixture was subjected to the same surface modification treatment as in Example 1.
• the granules of the resulting detergent composition had an average particle size of 565 ⁇ m, a bulk density of 776 g/L, and a flowability of
• the granules had a relative ratio for the detergency rate of 0.988, whereby showing excellent detergency.
• Example 2 In the same manner as in Example 1, the enzyme and the perfume were added thereto, to give a final powder of the high-bulk density detergent composition.
• Example 3 A detergent composition was obtained by using the same composition and the operations as employed in Example 2, except for changing the amount of LIGHT ASH used to 12.73 parts by weight, adding 0.23 parts by weight of a 48%o by weight aqueous NaOH solution as a reaction initiating agent before neutralization to the mixture of LIGHT ASH and a fluorescer, and thereafter adding a process for blending for 1 minute and 30 seconds under the same conditions as those for the process of powder blending.
• the granules of the resulting detergent composition had an average particle size of 550 ⁇ m, a bulk density of 780 g/L, and a flowability of 7.3 seconds, whereby showing excellent powder properties.
• the granules had a relative ratio for the detergency rate of 0.990, whereby showing excellent detergency.
• Example 4 A detergent composition having a composition shown in Table 2 was prepared in an amount of 35 kg for each unit, using a Lodige Mixer "FKM-130D" (manufactured by Matsubo Co., Ltd.). This mixer basically had the same construction as that described in Example 1.
• Solid ingredients comprising 12.22 parts by weight of sodium carbonate (the same "LIGHT ASH" as in Example 1), and 0.11 parts by weight of a fluorescer, were blended for one minute with the above Lodige Mixer under the same conditions as in Example 1.
• the granules of the resulting detergent composition had an average particle size of 510 ⁇ m, a bulk density of 778 g/L, and a flowability of 6.5 seconds, whereby showing excellent powder properties.
• the granules had a relative ratio for the detergency rate of 0.988, whereby showing excellent detergency.
• Example 5 A detergent composition having a composition shown in Table 2 was prepared in an amount of 35 kg for each unit, using a Lodige Mixer "FKM-130D" (manufactured by Matsubo Co., Ltd.). This mixer basically had the same construction as that described in Example 1.
• Solid ingredients comprising 11.00 parts by weight of sodium carbonate (the same "LIGHT ASH" as in Example 1), and 0.11 parts by weight of a fluorescer, were blended for one minute with the above Lodige Mixer under the same conditions as in Example 1.
• Example 1 While the disintegrated mixture was stirred in the above Lodige Mixer under the same conditions as above, the nonionic surfactant (0.70 parts by weight) was added to the mixer and blended for one minute. Next, a zeolite (2.00 parts by weight) having an average particle size of 4 ⁇ m was added thereto, and blended for additional 5 minutes. Thereafter, a 40% by weight aqueous solution of acrylic acid-maleic acid copolymer (effective ingredient: 1.49 parts by weight) was added to the mixer, and the ingredients were blended for 1 minute and 30 seconds. Subsequently, the resulting mixture was subjected to the same surface modification treatment as in Example 1.
• the granules of the resulting detergent composition had an average particle size of 560 ⁇ m, a bulk density of 780 g/L, and a flowability of 7.4 seconds, whereby showing excellent powder properties.
• the granules had a relative ratio for the detergency rate of 0.994, whereby showing excellent detergency.
• Example 2 In the same manner as in Example 1, the enzyme and the perfume were added thereto, to give a final powder of the high-bulk density detergent composition.
• a detergent composition having a composition shown in Table 2 was prepared in an amount of 35 kg for each unit, using a Lodige Mixer "FKM-130D” (manufactured by Matsubo Co., Ltd.). This mixer basically had the same construction as that described in Example 1.
• Solid ingredients comprising 13.19 parts by weight of sodium carbonate (the same "LIGHT ASH" as in Example 1), 7.00 parts by weight of a zeolite having an average particle size of 4 ⁇ m, and 0.11 parts by weight of a fluorescer, were blended for one minute with the above Lodige Mixer under the same conditions as in Example 1.
• the nonionic surfactant (0.98 parts by weight) was added to the mixer and blended for one minute, and thereafter a 40% by weight aqueous solution of acrylic acid- maleic acid copolymer (effective ingredient: 1.49 parts by weight) was added to the mixer, and the ingredients were blended for 1 minute and 30 seconds. Subsequently, the resulting mixture was subjected to the same surface modification treatment as in Example 1.
• the granules of the resulting detergent composition had an average particle size of 650 ⁇ m, a bulk density of 770 g/L, and a flowability of 6.9 seconds, whereby showing excellent powder properties.
• the granules had a relative ratio for the detergency rate of 0.902, whereby showing notably poorer detergency.
• Example 2 In the same manner as in Example 1, the enzyme and the perfume were added thereto, to give a final powder of the detergent composition.
• composition (% by weight) LAS-Na 28.00 28.00 28.00 28.00 22.00 35.00 28.00
• a detergent composition having a composition shown in Table 3 was prepared in an amount of 35 kg for each unit, using a Lodige Mixer "FKM-130D" (manufactured by Matsubo Co., Ltd.). This mixer basically had the same construction as that described in Example 1. The operations were carried out as follows (the amount of each raw material formulated in each step is shown in Table 4). ⁇ Powder Blending>
• Solid ingredients comprising sodium carbonate ("LIGHT ASH,” manufactured by Central Glass Co., Ltd.; average particle size: 56.1 ⁇ m), sodium tripolyphosphate (STPP; average particle size: 11.2 ⁇ m), and a fluorescer, were blended for one minute with the above Lodige Mixer under the conditions of a rotational speed of agitator blades of 130 rotations/min (peripheral speed: 3.4 m s) and a rotational speed of a shearing device of 2850 rotations/min (peripheral speed: 27 m s).
• a 48%o by weight of NaOH aqueous solution was added to the contents in the mixer as a reaction initiating agent, and the blending was canied out for 1 minute and 30 seconds under the same conditions as above.
• the nonionic surfactant (0.98 parts by weight) was added to the mixer and blended for one minute.
• a zeolite (2.00 parts by weight) having an average particle size of 4 ⁇ m was added thereto, and blended for additional 5 minutes.
• a 40% by weight aqueous solution of acrylic acid-maleic acid copolymer was added to the mixer, and the ingredients were blended for 1 minute and 30 seconds.
• the resulting mixture was subjected to a surface modification treatment by adding the zeolite (2.20 parts by weight) having an average particle size of 4 ⁇ m to the mixer as a surface modifier, and operating the mixer for additional one minute.
• Example 6 after 30 seconds from the termination of addition of the LAS, STPP or zeolite (1.75 parts by weight) was added as an inorganic powder.
• Example 8 the addition of STPP, an inorganic powder was canied out during the course of the neutralization process, and the mixture was continued to be blended for 5 minutes after termination of the addition of the LAS.
• the addition of STPP was canied out at a point where a weight ratio of the LAS added to sodium carbonate reached 0.6.
• Example 2 the mixture was blended for 5 minutes after the termination of the addition of LAS, without adding an inorganic powder during the course of the neutralization process or immediately after the neutralization process.
• composition (% by weight)
• a detergent composition having a composition shown in Table 3 was prepared in an amount of 35 kg for each unit, using a Lodige Mixer "FKM-130D" (manufactured by Matsubo Co., Ltd.). This mixer basically had the same construction as that described in Example 1. The operations were carried out as follows (the amount of each raw material formulated in each step is shown in Table 4). ⁇ Powder Blending>
• Solid ingredients comprising sodium carbonate (the same LIGHT ASH as in Example 1), sodium tripolyphosphate (the same STPP as in Example 6), and a fluorescer, were blended for one minute with the above Lodige Mixer under the same conditions as in Example 1.
• Example 1 While the mixer was operated under the same conditions as in Example 1, a mixture comprising a 40% by weight aqueous solution of acrylic acid-maleic acid copolymer and water was added to the mixer and blended for 1 minute and 30 seconds. Subsequently, the resulting mixture was subjected to a surface modification treatment in the same manner as in Example 1.
• Example 2 In the same manner as in Example 1, the enzyme and the perfume were added thereto, to give a final powder of the high-bulk density granular detergent composition.
• a high-bulk density detergent composition having excellent detergency and a small average particle size can be obtained.

Landscapes

• Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Detergent Compositions (AREA)

Applications Claiming Priority (3)

Publications (2)

Family

ID=16966523

Family Applications (1)

Country Status (4)

Families Citing this family (2)

Family Cites Families (7)

• 2000
  • 2000-08-17 DE DE60016428T patent/DE60016428T2/de not_active Expired - Lifetime
  • 2000-08-17 EP EP00953448A patent/EP1212399B1/de not_active Expired - Lifetime
  • 2000-08-17 CN CNB00814267XA patent/CN100419056C/zh not_active Expired - Fee Related
  • 2000-08-17 WO PCT/JP2000/005487 patent/WO2001014511A1/en active IP Right Grant

Non-Patent Citations (1)

Also Published As

Similar Documents

Legal Events