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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/04—Water-soluble compounds
  • C11D3/06—Phosphates, including polyphosphates
• • 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

Definitions

• the present invention relates to a detergent composition and a method for producing the same.
• Heavy-duty detergents are used for washing in a washing machine, but may be used for hand-washing when there is a heavy load of stains on fibers.
• hand-washing it has been empirically known that the washing efficiency is good if a heavy detergent solution is applied to the soil and the heavy-duty detergent is sprinkled directly on the part to be washed wet with water and then used. ing. In this case, sufficient lathering is required to improve slippage between the fibers in order to rub the parts to be washed with each other or the other textile parts by hand.
• a heavy powder detergent having a large amount of water-soluble components is preferable.
• the powder has high fluidity, foams quickly, is easy to wash, and the agglomeration of detergent particles disappears.
• a detergent with a high dissolution rate that contains a phosphate builder that is fast.
• the gist of the present invention is:
• the weight frequency W i of each classified particle group obtained by classifying the detergent particles by using a classifier consisting of: and the dissolution rate V i of each classified particle group measured under the following measurement conditions.
• a detergent composition in which the sum of the products satisfies the following formula (1), and the weight frequency of the classified particles having a particle size of less than 125 / m is 0.10 or less:
• FIG. 1 (1) and (2) are diagrams showing the steps of a classification operation in the production method of the present invention.
• the content of the phosphate builder in the present invention is from 5 to 60% by weight, preferably from 10 to 50% by weight of the detergent composition, from the viewpoint of the slipperiness of the laundry to be washed during hand washing. %, More preferably 15 to 45% by weight.
• the phosphate builder one or more selected from tripolyphosphate, orthophosphate, pyrophosphate and the like are preferable.
• the content of triphosphate in the total phosphate builder is 80 to 97% by weight
• the content of orthophosphate is 1 to 10% by weight
• the content of pyrophosphate is 2 to 10% by weight.
• an alkali metal ion is preferable, and particularly, a sodium ion and a potassium ion are preferable.
• the content of sodium ions and potassium ions in all the counter ions is preferably at least 70% by weight, more preferably at least 85% by weight.
• the surfactant content in the present invention is preferably from 10 to 60% by weight, more preferably from 20 to 50% by weight, and still more preferably from the viewpoint of obtaining detergency and desired powder properties. Or 27-45% by weight.
• the surfactant contains an anionic surfactant and / or a non-ionic surfactant, and may contain a cationic surfactant and an amphoteric surfactant as necessary.
• anionic surfactants alkyl benzene sulfonate, alkyl or alkenyl ether sulfate, alkyl or alkenyl sulfate, hypoolefin sulfonate, hysulfo fatty acid salt or ester thereof, alkyl or alkenyl ether carboxylate And fatty acid salts.
• the content of the anionic surfactant is preferably 1 to 50% by weight, more preferably 5 to 30% by weight of the detergent composition in terms of detergency.
• an alkali metal ion is preferable in terms of improving the detergency.
• potassium ions are preferable, and the content of potassium ion in all the counter ions is preferably 5% by weight or more, more preferably 20% by weight or more, and particularly preferably 40% by weight or more.
• polyoxyalkylene alkyl ethers polyoxyalkylene alkyl phenyl ethers, polyoxyalkylene fatty acid esters And polyoxyethylene polyoxypropylene alkyl ethers, polyoxyalkylene alkylamines, glycerin fatty acid esters, higher fatty acid alcohol amides, alkyl glycosides, alkyl glucose amides, and alkylamine oxides.
• polyoxyethylene polyoxypropylene polyoxyethylene alkyl ether is preferred.
• the compound can be obtained by reacting an ethylene oxide adduct of an alcohol having 10 to 18 carbon atoms, preferably 12 to 14 carbon atoms, with propylene oxide and further ethylene oxide.
• polyoxyethylene alkyl ethers those having a narrow distribution of the alkylene oxide chain length are preferred.
• the content of the nonionic surfactant is preferably 1 to 50% by weight, more preferably 5 to 30% by weight of the detergent composition from the viewpoint of detergency.
• Examples of the cationic surfactant include alkyltrimethylammonium salts and the like, and examples of the amphoteric surfactant include carbobetaine-type and sulfobetaine-type surfactants.
• the content of each of the positive surfactant and the amphoteric surfactant is preferably 0.1 to 5% by weight, more preferably 0.5 to 3% by weight of the detergent composition.
• the detergent composition of the present invention may contain water-soluble inorganic salts such as carbonates, bicarbonates, silicates, sulfates, sulfites, and phosphates.
• an alkali metal ion such as a sodium ion and a potassium ion is particularly preferable.
• the salts, especially carbonates are preferably 40% by weight or less, more preferably 5 to 3% by weight of the detergent composition in terms of anhydride. 0% by weight, more preferably 5 to 25% by weight.
• the detergent composition of the present invention may contain a crystalline silicate.
• the Si 0 2 ZM 20 molar ratio (M is an alkali metal atom) is preferably 0.5 or more, and preferably 2.6 or less from the viewpoint of alkali ability. 5 to 2.2 are particularly suitable.
• the crystalline silicate preferably has an average particle size of about 1 to 40 m from the viewpoint of high-speed dissolution and powder physical properties. The content of the crystalline silicate is 0. It is preferably from 5 to 40% by weight, more preferably from 1 to 25% by weight. In particular, a combination with sodium carbonate is preferred.
• the detergent composition of the present invention is preferably blended with a cation exchange polymer having a carboxylic acid group and a Z or sulfonic acid group in terms of sequestering ability and dispersing ability of solid particle stains.
• a cation exchange polymer having a carboxylic acid group and a Z or sulfonic acid group in terms of sequestering ability and dispersing ability of solid particle stains.
• salts of acrylic acid-maleic acid copolymers having a molecular weight of 1,000 to 100,000, polyacrylates and molecular weights described in JP-A No. 54-52196 of 8 to 1 million, preferably 5,000 to 200,000 polyacetate carboxylate such as polyglyoxylic acid is blended.
• the cation exchange polymer is preferably contained in an amount of 0.5 to 12% by weight, more preferably 1 to 7% by weight, particularly preferably 2 to 5% by weight of the detergent composition from the viewpoint of detergency.
• the detergent composition of the present invention may contain a crystalline aminosilicate such as A-type, X-type, or P-type zeolite.
• the average primary particle diameter is preferably from 0.1 to 1.
• the content of the crystalline aluminosilicate is preferably 3 to 15% by weight of the detergent composition.
• Preferred as the crystalline aluminosilicate is A-type zeolite (for example, trade name "Toyovirda-1": manufactured by Tosoichi Co., Ltd.), which is also preferable in terms of sequestering ability and economy.
• the value of the oil absorption capacity of the A-type zeolite according to the JISK 5101 method is preferably at least 4 OmL / 100 g.
• P type for example, trade name “Doucil A24J,“ ZSE064 ”, etc.); all manufactured by Crosfie 1d; oil absorption capacity 60 to 15 OmLZl 00 g
• X type for example, trade name“ We ssa 1 It hXDj.; manufactured by Degu ssa; oil absorption capacity 8 O l O OmLZl OO g
• suitable zeolite described in WO9842622 is also suitable crystallinity. Examples include aluminosilicates.
• an amorphous aluminosilicate having an oil absorption capacity of at least 8 OmL / 100 g according to the JISK 5101 method can be blended.
• S i 0 2 A 1 2 0 3 ( molar ratio) is 4.0 or less, Preferably, it is 3.3 or less, and JP-A-5-501 publication, column 4, line 34 to column 6, line 16 (especially column 4, line 43 to 49) (Oil-absorbing carrier) ⁇ Japanese Patent Application Laid-Open No.
• the crystalline a which is a water-insoluble inorganic salt in the present invention, is preferred.
• the total amount of the minosilicate, the amorphous aluminosilicate and the crystalline silicate having a low dissolution rate in water is preferably less than 25% by weight of the detergent composition in view of the ease of hand washing and washing. It is preferably less than 20% by weight, more preferably less than 15% by weight, and less than 200% by weight, preferably less than 100% by weight with respect to phosphate builder. Desirably.
• the detergent composition of the present invention includes organic acid salts such as citrate and ethylenediaminetetraacetate; dispersants or color transfer inhibitors such as carboxymethylcellulose, polyethylene glycol, polyvinylpyrrolidone and polyvinyl alcohol; Bleaching agents such as salts, compounds described in JP-A-6-31670 and bleaching activators such as tetraacetylethylenediamine, enzymes such as proteases, cellulases, amylases and lipases; A stilbene-type fluorescent dye, an antifoaming agent, an antioxidant, a bluing agent, a fragrance, and the like can be appropriately compounded.
• organic acid salts such as citrate and ethylenediaminetetraacetate
• dispersants or color transfer inhibitors such as carboxymethylcellulose, polyethylene glycol, polyvinylpyrrolidone and polyvinyl alcohol
• Bleaching agents such as salts, compounds described in JP-A-6-31670 and bleaching activators such as te
• the bulk density of the detergent composition measured by JISK 3362 is 600 to 1200 gZL, and from the viewpoint of improving transport efficiency and user convenience, is 600 g / L or more, preferably 6 g / L or more. 5 O gZL or more, more preferably 70 O gZL or more, and 1200 gZL or less, preferably 1 g, from the viewpoints of securing voids between particles and improving dispersibility by suppressing the increase in the number of contact points between particles. It is at most 5,000 gZL, more preferably at most 850 g / L.
• the detergent composition of the present invention is excellent in solubility per detergent particle and prevention of aggregation between detergent particles.
• agglomeration between detergent particles means that under the conditions of low mechanical force and cold water, a surfactant capable of forming liquid crystals and a part of inorganic salts that form hydrated crystals such as carbonates and sulfates are dissolved.
• This is a phenomenon in which high-viscosity liquid crystals are formed between the detergent particles or recrystallized into hydrates earlier than the remainder is dissolved after the start. Therefore, in the particle size of the detergent composition of the present invention, the weight frequency of the classified particles having a particle size of less than 125 / m is 0.10 or less from the viewpoint of preventing aggregation between the detergent particles.
• the weight frequency of the classified particles having a particle diameter of less than 125 / m is 0.10 or less, preferably 0.08 or less, more preferably 0.06 or less, and particularly preferably 0.04 or less.
• the weight frequency of the classified particles having a particle diameter of 125/111 or more and less than 180 / m is preferably 0.20 or less, more preferably 0.10 or less, and particularly preferably 0.05. It is as follows.
• each weight frequency has a relationship of [classified particle group having a particle size of less than 125 m] ⁇ [classified particle group having a particle size of from 125 m to less than 180 m].
• the content of coarse particles in the detergent composition is small in view of the high-speed solubility per particle.
• the weight frequency of the classified particle group having a particle diameter of 1000 / zm or more is preferably not more than 0.03, more preferably not more than 0.01, and particularly preferably substantially not included.
• the weight frequency of the classified particle group having a particle diameter of 7100 m or more and less than 1000 zm is preferably 0.10 or less, more preferably 0.05 or less, and particularly preferably 0.03 or less.
• the weight frequency of the classified particle group having a particle diameter of 500 / m or more and less than 710 m is preferably 0.10 or less, more preferably 0.05 or less, and even more preferably 0.03 or less. .
• the weight frequency is accumulated in order from fine particles to coarse particles, the opening of the first sieve at which the cumulative frequency becomes 50% or more is am, and is larger than a ⁇ .
• the mesh size of the sieve is b / m and the integration of the weight frequency from the saucer to the sieve of a is c%, and the weight frequency on the sieve of azm is d%, the following formula (3) is used. You can ask.
• Filter (mesh size: 74 m) (Use a sieve having a sieve area of 35 cm 2 or more and a weight of 10 g or less, and measure the weight in advance.) Subsequently, the residue of each classified particle group remaining on the sieve was dried together with the sieve in an electric dryer at 105 ° C for 1 hour, and desiccated with silica gel with enhanced activity. Allow to cool for 30 minutes at (25 ° C), then weigh. By subtracting the weight of the sieve from this weight, the dry weight of the residue of each classified particle group can be derived. Specific measurement conditions are the same as the dissolution measurement conditions described above. Under these conditions, the powder detergent composition having a dissolution rate of 90% or more was found to be very easy to dissolve and lose particles even at the time of manual washing at room temperature or lower, and to have a high foaming rate. Was.
• the solubility of the detergent composition of the present invention is represented by the sum of the products of the weight frequency W i of each classified particle group and the solubility V i of each classified particle group (that is, ⁇ (Wi ⁇ Vi)). .
• the solubility of the detergent composition of the present invention is 90% or more, preferably 94% or more, more preferably 97% or more.
• the dissolution rate Vi of the classified particles is calculated by the following equation (2).
• i means each classified particle group.
• the detergent composition of the present invention is easy to sprinkle a desired amount on an object to be washed in hand-washing, has a fast dissolution of particles, has an excellent foaming rate, and has a phosphate builder as a main builder. Can be done efficiently.
• irrigation using a washing machine since it has extremely high solubility even in cold water conditions, it not only has the effect of eluting the washing components into the washing bath more quickly to improve the washing power, but also has an extremely low Even under laundry conditions, the probability of remaining undissolved is extremely low.
• a specific measuring method is a polypropylene basin with a maximum opening diameter of 31 cm, a bottom part of 24 cm, and a height of 13 cm (for example, KW-30 type washing tub manufactured by YA ZAKI, content volume 8.2 L) ), Add 5.0 L of tap water at 25 ° C. Then, spray 15 g of the detergent composition to be tested uniformly and quickly (within 3 seconds as a guide) over the entire surface of the water so that it does not solidify in one place. From that point, a skilled panelist spreads five fingers with one hand (dominant arm) and gently strokes the bottom of the basin with his fingertip while sensing detergent particles present at the bottom of the basin with his fingertip (ventral side of the finger) Start the stirring).
• the panelists will be conducted by 10 or more persons.
• the average value of the panelists' hand-washing dissolution times in the middle 60% excluding the top 20% and bottom 20% panelists shall be used as the hand-washing dissolution time of the tested detergent composition.
• the flow time (the time required for the powder of 10 OmL to flow out of the hopper for bulk density measurement specified by JISK 3362) is 10 seconds or less, preferably 8 seconds or less, more preferably Is less than 6.5 seconds.
• the detergent composition of the present invention comprises an unclassified detergent particle group containing 5 to 60% by weight of a phosphate builder and 10 to 60% by weight of a surfactant (hereinafter, also referred to as a base detergent particle group.
• the base detergent particle group includes a classification particle group obtained by performing a classification operation and a particle size adjustment operation a plurality of times.) The production process can be performed by performing a classification operation and a particle size adjustment operation.
• the mixture of the acid precursor of the nonionic surfactant and the anionic surfactant capable of lamellar orientation described in Japanese Patent Publication No. 0 is tumbled by a stirring granulator at a temperature not lower than the neutralizable temperature.
• a method of granulating while performing the method can be used.
• the detergent composition of the present invention can be obtained by classifying and adjusting the particle size of the base detergent particles.
• the classification method include a method using a circular / rectangular vibrating sieve, an ultrasonic vibrating sieve having an ultrasonic vibrator attached thereto, a wind classifier / centrifugal classifier, and the like. After performing at least one-stage classification operation on the base detergent particles, the weight frequency of each of the classified particles on the sieve and the classified particles below the sieve is measured with respect to the input amount of the base detergent particles. It can be obtained by blending the classified particle groups so that the above formula (1) is satisfied and the weight frequency of the classified particle groups of less than 125 m is 0.10 or less.
• the classified particles not used in the above steps 1 and 2 are subjected to a granulation operation based on the dissolution rate Vi, for example, granules having a Vi of 90% or more, and a Vi of less than 90%.
• the coarse particles are preferably subjected to a crushing operation or the like to be reused as a base detergent particle group.
• a fine granulation operation and a coarse particle disintegration operation will be exemplified.
• coarse particle crushing process Excess coarse particles can be reused as a base detergent particle group by reducing the particle size, for example, by crushing.
• coarse particle crushers include impact crushers such as a hammer crusher, impact crushers such as an atomizer and a pin mill, and shear crushers such as a flash mill. These may be a single-stage operation or a multi-stage operation of the same or different types of pulverizers. It is preferable to add fine powder as an in-machine adhesion inhibitor or a pulverized surface modifying agent.
• the fine powder is preferably an inorganic powder such as triboriphosphate, aluminosilicate, silicon dioxide, bentonite, talc, clay amorphous silica derivative, and more preferably a crystalline or amorphous aluminosilicate. Fine powders of inorganic salts such as soda ash and sodium sulfate are also used.
• inorganic powder such as triboriphosphate, aluminosilicate, silicon dioxide, bentonite, talc, clay amorphous silica derivative, and more preferably a crystalline or amorphous aluminosilicate.
• Fine powders of inorganic salts such as soda ash and sodium sulfate are also used.
• a detergent composition By the combination of the fine granulation operation and the coarse particle disintegration operation, a detergent composition can be economically obtained in a high yield from the surplus classified particles in the step 2.
• enzymes, pigments, fragrances, and the like can be blended after the classification and particle size adjustment steps.
• a washing net (model number: AXW22A-5RU0, mesh size: 300 x 640 zm) was attached to the side of the irrigation tank of the washing machine manufactured by Matsushita Electric Industrial Co., Ltd. “Aizumago NA-F70VP1J. 3 kg (50% by weight of cotton underwear, 50% by weight of polyester Z cotton blended Y-shirt), 44.0 g of the detergent composition of the example was evenly sprayed and poured, and tap water at 5 ° C was poured. After washing (excluding the rinsing step), the amount of the detergent composition remaining in the washing net was visually judged according to the following evaluation criteria. A water temperature of 5 ° C is a disadvantageous condition for the solubility of the particles in a washing time of 3 minutes, and the evaluation criteria A, B and C indicate that the detergent composition has excellent solubility. And
• A Residual detergent particles are almost zero (standard of remaining detergent particles: 0 to 5).
• B No residual detergent particles (approximately 6 to 15 residual detergent particles).
• C Detergent particles hardly remain (approximately 16 to 30 residual detergent particles).
• D A small amount of detergent particles remains (30 to 100 particles of remaining detergent particles).
• the stirring power in this evaluation is extremely weaker than the standard, and the evaluation criteria I and II indicate that the detergent composition has excellent dispersibility.
• the “aggregate” described below refers to a lump having a diameter of 3 mm or more in which the detergent particles are aggregated.
• ⁇ ⁇ A small amount of aggregate remains (lumps with a diameter of about 6 mm are found, and less than 10 lumps with a diameter of 3 to 1 Omm are found). IV: A large amount of aggregate remains (many lumps exceeding 6 mm in diameter are observed)
• the hand wash solubility was measured according to the measurement method described in the above “[6] Hand wash solubility of detergent composition”.
• the washbasin was a KW-30 type washing tub manufactured by YAZAK I, and the panel was implemented by 10 people.
• Linear alkyl (10 to 13 carbon atoms) 56 parts by weight of a 25% by weight aqueous solution of potassium benzenesulfonate, —sulfo fatty acid (14 to 16 carbon atoms) sodium methyl ester 8 parts, same nonionic surface activity as in Production Example 1 1 part, 7 parts of the same stone as in Production Example 1, 20 parts of sodium tripolyphosphate, 1 part of No.
• the volatile content (105 ° C., loss for 2 hours) was 5% by weight.
• the above particles 50 kg / H, sodium carbonate (heavy ash) 4 kgZH, the same crystalline silicate powder 1 kgZH as in Production Example 1, and the same nonionic surfactant 3 kg ZH as in Production Example 1 It was continuously added to Ni-da-1 (made by Kurimoto Iron Works).
• a twin-screw extruder (“Pellet Double”: made by Fuji Baudal) was installed to obtain a cylindrical pellet with a diameter of about 3 mm.
• the classification operation was performed on each of the base detergent particle groups in Production Examples 1 to 3 using the above-described classification device. Specifically, 100 times of the sample was put from the top of the 2000 m sieve at the top of the classifier, and the lid was put on it.
• a tapping machine made by HE IKO SE I SAKUSHO, tapping: 156 times Z Min., Rolling: 290 times), and after shaking for 10 min., Recover the sample remaining on each sieve and saucer for each sieve, and the required amount of more than 1410 tm to 2000 m Less than 1, 000 m to less than 1400 m, less than 700 tzm to less than 100 m, less than 500 m / m to less than 700 m, more than 350 m to 350 m 0 m or less, 250 cm or more to less than 355 m, 180 tzm or more to less than 250 am, 125 zm or more to less than 180 m / m, dish to 125 zm (less than 125 cm) A sample of each classified particle group was obtained.
• the particle size was adjusted according to the following method, whereby the high bulk density detergent compositions of Examples 1 to 9 were obtained.
• Table 2 shows the average particle size, bulk density, fluidity, and ⁇ (Wi ⁇ Vi) of the obtained detergent composition. Crying degree adjustment operation 1
• Each classified particle group was weighed so that each sample weighed 200 g according to the weight frequency of the particle size distribution shown in Table 2, and various particle sizes were adjusted by mixing with a rocking mixer (manufactured by Aichi Electric) for 2 minutes. A detergent composition was obtained.
• the base detergent particles obtained in Production Example 3 (1) 100 parts were classified with a gyro shifter (manufactured by Tokuju Kosakusho) equipped with a screen of 500 zm, and the particles on the sieve were classified. By removing, 55.1 parts of the detergent composition of Example 10 were obtained. Particle size adjustment operation 3
• Example 10 Detergent composition 55.1 As a group of base detergent particles, put into a gyro shifter equipped with a screen having an opening of 125 m to remove fine particles of less than 125 um.Example 1 51.1 parts of the detergent composition of 1 were obtained. Particle size adjustment operation 4
• the first stage had a diameter of 2 mm, and the second stage had a diameter of l mm.
• the average particle size of the two-stage disintegrated particles was 376 um, and 23.2 parts of particles of 500 or more in 46.7 parts of the two-stage disintegrated particles were contained.
• the two-stage crushed particles are thrown into the gyro shifter on a 500-m screen. And classified into on-sieving particle group B and under-sieving particle group B. This underscreen particle group B25.0 parts and the underscreen particle group A55.5 parts were blended to obtain 80.5 parts of the detergent composition of Example 12.
• Example 12 Detergent composition of Example 13 80.5 parts are introduced into the above gyrosif equipped with a screen of 1 2 5 zm with a screen of 1 2 5 zm and fine particles less than 1 2 5 m are removed, Composition 76.2 2 parts were obtained. Particle size adjustment operation 6
• the undersize particle group C was granulated by the following operation. To the high-speed mixer, 5.4 parts of the undersize particle group C1 were added, and 0.77 parts of the nonionic surfactant was spray-added over 1.3 minutes, followed by stirring and granulating for 10 minutes. Next, 0.92 parts of zeolite (average particle size of about 3 ⁇ m) was added, and the surface coating treatment was performed for 1 minute to obtain a base detergent particle group (2) (average particle size: 662 fim).
• Table 4 shows the results obtained by measuring the solubility of the particles and the solubility of the hand washing of the eight detergent compositions.
• the results in Table 4 show that these commercially available detergents have a low level of particle solubility and are also poor in hand wash solubility.
• a to H which has the highest particle solubility and hand wash solubility, had extremely poor fluidity.
• the detergent composition of the present invention dissolves quickly after being poured into water even in cold water, has excellent solubility when used for hand washing, and has excellent dispersibility due to aggregation between particles. It has excellent detergency and solubility even under low mechanical washing conditions like a machine.

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• 2000
  • 2000-06-12 WO PCT/JP2000/003792 patent/WO2000077157A1/ja not_active Application Discontinuation
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