CN1233275A - Free-flowing agglomerated nonionic surfactant detergent composition and process for making same - Google Patents
Free-flowing agglomerated nonionic surfactant detergent composition and process for making same Download PDFInfo
- Publication number
- CN1233275A CN1233275A CN97194403.2A CN97194403A CN1233275A CN 1233275 A CN1233275 A CN 1233275A CN 97194403 A CN97194403 A CN 97194403A CN 1233275 A CN1233275 A CN 1233275A
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- CN
- China
- Prior art keywords
- carboxylic acid
- detergent
- acid
- nonionogenic tenside
- water
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 121
- 239000003599 detergent Substances 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000008569 process Effects 0.000 title abstract description 5
- 239000002736 nonionic surfactant Substances 0.000 title description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 68
- -1 alkali metal salt Chemical class 0.000 claims abstract description 56
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 32
- 239000004094 surface-active agent Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 24
- 150000001735 carboxylic acids Chemical class 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 98
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 65
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 49
- 235000017550 sodium carbonate Nutrition 0.000 claims description 49
- 239000013543 active substance Substances 0.000 claims description 36
- 239000002253 acid Substances 0.000 claims description 18
- 241000282326 Felis catus Species 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 229910000288 alkali metal carbonate Inorganic materials 0.000 abstract description 3
- 150000008041 alkali metal carbonates Chemical class 0.000 abstract description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 abstract 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 abstract 1
- 239000001630 malic acid Substances 0.000 abstract 1
- 235000011090 malic acid Nutrition 0.000 abstract 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 44
- 229910052799 carbon Inorganic materials 0.000 description 37
- 239000000047 product Substances 0.000 description 37
- 238000005054 agglomeration Methods 0.000 description 34
- 230000002776 aggregation Effects 0.000 description 34
- 150000001721 carbon Chemical group 0.000 description 32
- 239000002245 particle Substances 0.000 description 27
- 239000000377 silicon dioxide Substances 0.000 description 22
- 125000000217 alkyl group Chemical group 0.000 description 21
- 239000003795 chemical substances by application Substances 0.000 description 17
- 238000001035 drying Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 14
- 238000005406 washing Methods 0.000 description 14
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 13
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- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 13
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 13
- 238000002156 mixing Methods 0.000 description 12
- 239000011734 sodium Substances 0.000 description 12
- 229910052708 sodium Inorganic materials 0.000 description 12
- 238000011068 loading method Methods 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 10
- 125000001931 aliphatic group Chemical group 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
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- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical group [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 7
- 229940038773 trisodium citrate Drugs 0.000 description 7
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 6
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 6
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- 230000008859 change Effects 0.000 description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 6
- 229910052700 potassium Inorganic materials 0.000 description 6
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- 235000013162 Cocos nucifera Nutrition 0.000 description 4
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
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- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 4
- 238000007046 ethoxylation reaction Methods 0.000 description 4
- 150000002191 fatty alcohols Chemical class 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 150000003138 primary alcohols Chemical class 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000344 soap Substances 0.000 description 4
- REZQBEBOWJAQKS-UHFFFAOYSA-N triacontan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCO REZQBEBOWJAQKS-UHFFFAOYSA-N 0.000 description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 3
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 229910000323 aluminium silicate Inorganic materials 0.000 description 3
- 235000019504 cigarettes Nutrition 0.000 description 3
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- 230000005494 condensation Effects 0.000 description 3
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- 238000005342 ion exchange Methods 0.000 description 3
- 150000008040 ionic compounds Chemical class 0.000 description 3
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
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- 235000011152 sodium sulphate Nutrition 0.000 description 3
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- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
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- 125000002252 acyl group Chemical group 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- JHUXOSATQXGREM-UHFFFAOYSA-N dodecanediperoxoic acid Chemical compound OOC(=O)CCCCCCCCCCC(=O)OO JHUXOSATQXGREM-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
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- 150000002830 nitrogen compounds Chemical group 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 235000020030 perry Nutrition 0.000 description 1
- ZAPVCRYHKNILPH-UHFFFAOYSA-N phenyl nonanoate;sodium Chemical compound [Na].CCCCCCCCC(=O)OC1=CC=CC=C1 ZAPVCRYHKNILPH-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001444 polymaleic acid Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-O triethanolammonium Chemical compound OCC[NH+](CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-O 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
-
- 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
- C11D3/10—Carbonates ; Bicarbonates
-
- 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
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
-
- 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
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
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)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A free-flowing agglomerated powder detergent process and the resulting composition includes from about 5 % to about 80 % of an alkali metal carbonate; from about 5 % to about 50 % of a detergent surfactant, and up to about 25 % of an alkali metal salt of a carboxylic acid, wherein the carboxylic acid is selected from the group of carboxylic acids that, below a first temperature, have a greater water solubility than the water solubility of its corresponding alkali-metal salt. The alkali-metal salt is preferably provided solely by the reaction of (a) a premix comprising the alkali-metal carbonate coated with the surfactant, (b) a carboxylic acid selected from the group consisting of citric acid, malic acid, and mixtures thereof, and (c) water.
Description
Background of invention
Invention field
The present invention relates to free-pouring agglomerant powder detergent that contains the high-content nonionogenic tenside and preparation method thereof.
The discussion of correlation technique
People are making great efforts to have the powder detergent for washing clothes that increases the detergent surfactant amount so that provide.The benefit of highly enriched washing composition comprises expense and the cost of saving in the packing.Unfortunately, provide the amount of detergent surfactant of required flowability, solvability, cleaning and brightening property restricted to being included in the powder detergent simultaneously to the human consumer.
Most of granulated detergent is produced by spraying drying.Thereby this method comprise with detergent component for example tensio-active agent and washing assistant mix with water and form slurries, thereby in the high temperature air stream of then these slurries being sprayed into so that evaporate the particle that excessive water forms the hollow of pearl type.Although the spray-dried detergent slurries form the granulated detergent with fabulous deliquescent hollow, remove the heat energy that the big water gaging that is present in the slurries needs huge amount.Another shortcoming of spray drying process is: owing to need large-scale production equipment, need big initial investment.In addition, because the particle that obtains by spraying drying has low bulk density, so the particulate packaging volume is big, this has increased cost and paper refuse.In addition, may be very poor by particulate flowability and outward appearance that spraying drying obtains, because at the particle surface irregular.
Except these distinctive processing and product problem relevant with spray drying process, when adding man-hour with this method, volatile matter for example nonionogenic tenside can be put in the air.This volatilization problem, it is proved by dense " indigo plant " cigarette of discharging from spray tower, is referred to as " plumage cigarette " (pluming).Air pollution standard has limited the darkness of this plumage cigarette.The result need limit the spraying output of column, or under extreme case, can not continuous production.
Aspect the trial of this problem of avoiding being caused by spraying drying, sizable development work is added on nonionogenic tenside on the product after concentrating on the spraying drying operation again.Unfortunately, this spraying drying base-material is reinforced after with the tensio-active agent that is enough to provide satisfactory detergency energy causes obtaining poorly soluble product usually.Therefore, the amount of the tensio-active agent that can use in detergent formulation is subjected to strict restriction.Because need there be a large amount of nonionogenic tensides in heavy dirty detergent for washing clothes, so inorganic silicate is joined in these detergent formulation so that absorption nonionic liquid.
For example, people's such as Yurko US3769222 discloses liquid nonionic surfactants has been mixed with yellow soda ash up to the part solidification takes place, and then adds a large amount of silica (silicon-dioxide) thereby the free-pouring detergent composition that formation is done., the shortcoming of this technology is: because silica does not have significant cleaning active, only work to increase product cost in the detergent formulation so it is included in large quantities.In addition, in washing composition, use silica to increase total suspended solid (TSS) content of laundrywastes, disagree with the regulation of a lot of areas and national water Pollution norms.Therefore, encourage to keep the low silica amount that joins in the detergent composition.
The US4473485 of Greene has reported that free-pouring granulated detergent can prepare like this: by poly carboxylic acid structural agent solution is mixed with the carbonate of micronization, then add the mixture of nonionogenic tenside and water, then remove excessive water.The carbonate of preferred micronization is lime carbonate or yellow soda ash.Yet the shortcoming of this method is that carbonate and the general carbonate facics of Greene this micron change of being used to strengthen the Betengent product flowability is than quite expensive.Do not use the carbonate of this micron change, the product of Greene does not just have good like this flowability.In addition, when the carbonate of this micron change was lime carbonate, the ability of washing that helps of this washing composition reduced.
Therefore, exist the needs that specifically overcome free-flowing property problem in the high loading nonionic detergent.
Summary of the invention
The present invention relates to free-pouring agglomerant detergent powder that contains by high-content nonionic detergent tensio-active agent and preparation method thereof.More in a broad sense, the method that the present invention relates to contain the free-pouring agglomerant detergent powder of high-content nonionic detergent tensio-active agent and prepare this free-pouring detergent powder.The invention still further relates to free-pouring agglomerant detergent powder, particularly contain the preparation method of the detergent powder of high-content nonionic detergent tensio-active agent.This method comprises these steps: load on alkaline carbonate so that form the alkaline carbonate premixture that evenly applies with the tensio-active agent that is selected from negatively charged ion, nonionic, both sexes, positively charged ion, zwitter-ion and composition thereof; Carboxylic acid is mixed in this premixture; Water is joined on this mixture; Thereby finish agglomeration with this mixture of stirring.Preferably, this mixture feeding is advanced in the agglomeration machine of rotation, the rotation along with the agglomeration machine in this agglomeration machine is advanced a spot of water spray in this mixture.Preferred dry this agglomerate promptly is not the water as the hydrate bonding so that remove excessive water, thereby forms the free-pouring detergent composition of the present invention.
Randomly, a spot of other known detergent component may reside in the premixture.For example, can before loading, a spot of silica and carboxymethyl cellulose be mixed with alkaline carbonate with tensio-active agent.
Preferably, thus present method comprise and form the alkaline carbonate premixture of uniform surfactant-coated load yellow soda ash with tensio-active agent.This tensio-active agent is selected from negatively charged ion, nonionic, zwitter-ion, both sexes, cats product and composition thereof.This tensio-active agent is nonionogenic tenside preferably.Thereby will be from having the carboxylic acid of selecting the carboxylic-acid than the bigger water solubility of water solubility of its corresponding an alkali metal salt and mix with this premixture and form mixture being lower than first temperature.As discussed below, first temperature is about 15-40 ℃.This carboxylic acid is preferably selected from citric acid, oxysuccinic acid and composition thereof.Stirring this mixture joins a spot of water (being less than about 7%) sodium salt that makes this carboxylic acid dissolving and this carboxylic acid of neutralization formation in this mixture simultaneously and makes this mixture agglomeration.Dry this agglomerant mixture is so that thereby the water of removing at least about 50% adding forms free-pouring powder detergent composition.
The agglomerant washing composition that obtains like this contains: alkaline carbonate, its amount are about 5-80% of the finished product weight; The preferred nonionic detergent tensio-active agent of detergent surfactant, its amount are about 5-50% of the finished product weight; With an alkali metal salt that is up to about 25% carboxylic acid, wherein this carboxylic acid is selected from those carboxylic acids that have than the bigger water solubility of water solubility of its corresponding an alkali metal salt below first temperature.As discussed below, this first temperature is about 15-40 ℃.
Preferably, agglomerant detergent powder of the present invention contains the yellow soda ash of the 5-80% that has an appointment, the nonionogenic tenside of about 5-50%, wherein this nonionogenic tenside is Trisodium Citrate, sodium malate of the detergent surfactant of unique existence and about 4-18% and composition thereof.
More preferably, agglomerant detergent powder of the present invention contains the yellow soda ash of the 20-70% that has an appointment, the nonionogenic tenside of about 20-40%, wherein this nonionogenic tenside is the detergent surfactant of unique existence, complete basically neutral carboxylic acid with about 5-13%, this carboxylic acid is selected from Trisodium Citrate, sodium malate and composition thereof, wherein this Trisodium Citrate and sodium malate be by when adding entry, containing (a) nonionogenic tenside and yellow soda ash premixture and (b) reaction between blended citric acid, oxysuccinic acid or its mixture form.
The term that uses in this specification sheets and claims " coating " refers to tensio-active agent and is present on the surface of carbonate and is present in (for example by absorption) in the carbonate (with other particle).
Preferably, present method comprise mixture of sodium carbonate (with, randomly, other detergent component) and nonionogenic tenside so that form the yellow soda ash premixture that uniform nonionic applies, wherein this nonionogenic tenside is unique tensio-active agent that is present in this premixture, and the carboxylic acid that is selected from citric acid, oxysuccinic acid and composition thereof is mixed so that form mixture with this premixture.Stirring this mixture joins water the sodium salt that makes this carboxylic acid dissolving and this carboxylic acid of neutralization formation in this mixture simultaneously and makes this mixture agglomeration.Thereby dry this agglomerant mixture forms free-pouring powder detergent composition.
The term that uses in specification sheets below and claims " free-water " refers to and is not water such as the hydration or the water of crystallization on inorganic materials of bonding securely.
Unless otherwise indicated, all percentage number averages that use in specification sheets and claims below are by the weight of the finished product.
Detailed Description Of The Invention and preferred embodiment
The invention provides and contain the particularly free-pouring agglomerant detergent powder of nonionogenic tenside of high level of surfactant.The present invention also provides and has contained the particularly preparation method of the free-pouring agglomerant detergent powder of nonionogenic tenside of high level of surfactant.This method comprises: load on alkaline carbonate (with other optional detergent component) so that form the premixture of the uniform mixture that contains surfactant-coated carbonate with tensio-active agent.Thereby carboxylic acid is mixed the formation mixture with this premixture.This carboxylic acid is preferably selected from being lower than first temperature has those carboxylic acids than the bigger water solubility of water solubility of its corresponding an alkali metal salt.This mixture is incorporated in the preferred rotary drum agglomeration of the mixing machine machine, makes the dissolving of this carboxylic acid in this mixture and form an alkali metal salt of this carboxylic acid under first temperature and make this mixture agglomerate into particle being lower than with the alkaline carbonate reaction thereby there water is incorporated into.Drying and this particle of screening.
This detergent composition comprises three basal components: alkaline carbonate.Nonionogenic tenside and complete basically neutral carboxylic acid.
Because cost and efficient, alkaline carbonate is yellow soda ash preferably.In the preferred yellow soda ash that uses among the embodiment below is the mixture of the mixture of light density (LT) soda ash (Solvay method), light density (LT) and middle density soda ash (sesquicarbonate method), special high voidage " in light " soda ash (sesquicarbonate method) and light density and " in gently " soda ash.The mean density of these sodium carbonate particles is about 0.5-0.7, and average order number is in the scope (numerical value of USS sieve) of about 20-200.With the carbonate facics ratio of more multi-processing, carbonate for example can obtain from FMC Corp.and General Chemical those be relatively cheap because they do not need further processing for example to grind.
By the weight of the finished product, yellow soda ash can be present in the amount of about 5-80% in the free-pouring detergent composition.The amount that joins the yellow soda ash in the finished product is with the amount of the nonionogenic tenside that loads on yellow soda ash and with this blended carboxylic acid neutral amount phase equilibrium.By the weight of the finished product, the preferable range of this yellow soda ash is about 20-70%, more preferably from about 30-65%.What should propose is: in this preferred range, high level (as being normally used in the North America) under the condition that low production concentration is used needs often, then uses under the higher product concentration condition of (as often appearing at Europe) on the contrary.
If desired, about 10% the detergent component that can be before joining nonionogenic tenside wherein alkaline carbonate and other be no more than on a small quantity the finished product mixes.In addition, can be after the alkaline carbonate that they and nonionogenic tenside are applied mixes nonionogenic tenside be joined about 10% the detergent component that other is no more than the finished product on a small quantity.In one embodiment, be used in the method mixed carbonate of fully describing among US5458769 and the US5496486, optional detergent component and tensio-active agent, the whole disclosure of these two pieces of documents is incorporated by reference in this article.
In another embodiment, before loading with nonionogenic tenside, be up on a small quantity about 5% silica for example Silicon dioxide, hydrate mix with alkaline carbonate.For joining in the detergent composition, various silicon-containing materials all are acceptable, although the silica of the height of precipitation or gas phase legal system absorption is preferred.The oil absorption numerical value of this preferred silicon-containing compound is 150-about 350 or higher, preferred about 250 or higher.As the example of practical silica, following material is representational: Sipermat 50, Syloid 266, CabosilM-5, Hisil 7-600.Preferably, before loading,, the silica of about 0.5-4% is mixed with alkaline carbonate by the weight of the finished product with nonionogenic tenside.More preferably, by the weight of the finished product, the silica of about 3-4% is mixed with alkaline carbonate.
Also can be before loading with nonionogenic tenside the carboxymethyl cellulose (for example about 0.1-is up to 5%) of low levels mixed with alkaline carbonate in case the dirt deposition that helps to prevent in washings, to suspend at fabric for example on the cotton goods.Preferably, will about 1-3% before loading with nonionogenic tenside, more preferably from about the carboxymethyl cellulose of 2-3% mixes with alkaline carbonate.In a preferred embodiment, before loading, silica and carboxymethyl cellulose are mixed with yellow soda ash with nonionogenic tenside.
Second basal component is detergent surfactant, and it is selected from negatively charged ion, nonionic, zwitter-ion, both sexes, cats product and composition thereof.The detergent surfactant of Shi Yonging can be such any conventional substances in the present invention, they be know and be described in fully in the document, for example by Schwartz, Perry ﹠amp; In " the Surface Active Agents and Detergents " I of Berch and the II volume, in " the Nonionic Surfactants " of M.J.Schick and at " the Emulsifiers ﹠amp of McCutcheon; Detergents " in, every piece of document is all incorporated by reference in this article.The amount that this tensio-active agent exists is about 1-90%.Ideally, the amount that this tensio-active agent exists is about 10-50%, and preferably, the amount that this tensio-active agent comprises is also 20-40%.
Useful anion surfactant comprises that the water-soluble salt of higher fatty acid is a soap.It comprises that alkali metal soap for example contains sodium, potassium, ammonium and the alkylammonium salt of the higher fatty acid of 8-24 the carbon atom of having an appointment.Can prepare soap by the direct saponification of fat and oil or the neutralization by free fatty acids.Useful especially is sodium and sylvite from Oleum Cocois and tallow derived fatty acid, i.e. sodium or potassium tallow and coconut soap.
Useful anion surfactant also comprises the water-soluble salt of organic sulfuric acid reaction product, preferred as alkali, ammonium and alkanol ammonium salts, and it has alkyl and sulfonic acid or the sulfate group that contains about 8-20 carbon atom in molecular structure.Be included in the term " alkyl " is the moieties of acyl group.The example of this class synthetic surfactant is sodium alkyl sulfate and potassium, particularly by sulfation higher primary or secondary alcohol (C
8-C
18Carbon atom) those that obtain, this alcohol are those alcohol of producing by the glyceryl ester of reduction tallow or Oleum Cocois; With sodium alkyl benzene sulfonate and potassium, wherein this alkyl contains 10-16 the carbon atom of having an appointment, for the straight or branched configuration, for example see US2220099 and alkylbenzene sulfonate, wherein the mean number of carbon atom is about 11-14 in this alkyl, is abbreviated as C
11-14LAS.
Useful in the present invention anion surfactant also can comprise sodium, potassium, calcium, magnesium, ammonium or low-level chain triacontanol ammonium (for example triethanol ammonium, monoethanolamine ammonium or diisopropanol ammonium) alkane or alkene sulfonate, and wherein this alkyl contains 10-20 the carbon atom of having an appointment.The low-level chain triacontanol of above-mentioned alkanol ammonium generally has 2-4 carbon atom and ethanol preferably.This alkyl can be a straight or branched, and in addition, this sulfonate preferably is connected on the secondary carbon(atom), and promptly this sulfonate is not that end group connects.
Can be that other useful anion surfactant comprises the secondary alkyl sulfate with following general formula in the present invention:
Wherein M is potassium, sodium, calcium or magnesium, R
1Expression has the alkyl of about 3-18 carbon atom, R
2Expression has the alkyl of about 1-6 carbon atom.Preferably, M is a sodium, R
1Be alkyl with about 10-16 carbon atom, R
2It is alkyl with about 1-2 carbon atom.
Other useful in this article anion surfactant is the alkyl glycerylether sodium sulfonate, especially from the sodium sulfonate of those ethers of tallow and Oleum Cocois deutero-higher alcohols; Coco-nut oil fatty acid direactive glyceride sulfonic acid and sodium sulfate; Alkylphenol oxyethane ether sodium sulfate or sylvite, its per molecule contain the unitary oxyethane of the 1-10 that has an appointment and wherein this alkyl contain 10-20 the carbon atom of having an appointment.
Useful in the present invention ether sulfate is to have formula RO (C
2H
4O)
xSO
3Those of M, wherein R is alkyl or the alkenyl with about 10-20 carbon atom, and x is 1-30, and M is the preferred sodium of water-soluble cationic.Preferably, R has 10-16 carbon atom.This alcohol can be from natural fat for example Oleum Cocois or tallow deutero-, perhaps can be synthetic.Such alcohol and 1-30, the particularly reacting ethylene oxide of 1-12 mol ratio and with the mixture sulfation and the neutralization of the molecular substance that obtains.
Other useful herein anion surfactant comprises the water-soluble salt of α-sulfonated fatty acid ester, and it contains in fatty acid group has an appointment 6-20 carbon atom and contain 1-10 the carbon atom of having an appointment in ester group; The water-soluble salt of 2-acyl group oxidation of alkanes-1-sulfonic acid, it contains in acyl group has an appointment 2-9 carbon atom and contains 9-23 the carbon atom of having an appointment at paraffin section; Contain the have an appointment alkene of 12-20 carbon atom and the water-soluble salt of alkane sulfonic acid; And β-alkoxy alkane sulfonate, it contains in alkyl has an appointment 1-3 carbon atom and contain 8-20 the carbon atom of having an appointment in paraffin section.
Another example of anion surfactant that can be useful is those compounds that contain two anionic functional groups in this article.They are referred to as two anion surfactants.Two suitable anion surfactants are stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate, dithionate or its mixture, and they can be represented with following formula:
R(SO
3)
2M
2,R(SO
4)
2M
2,R(SO
3)(SO
4)M
2
Wherein R is the acyclic aliphatic hydrocarbyl with 15-20 carbon atom, and M is a water solubilising positively charged ion, for example, and C
15-C
20Dipotassium-1,2-alkyl stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate or vitriol, 1,9-hexadecyl two sulfuric acid disodiums, C
15-C
20Disodium-1,2-alkyl stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate or vitriol, 1,9-stearyl two sulfuric acid disodiums and 6,10-octadecyl two sulfuric acid disodiums.
The nonionic detergent tensio-active agent can be this class material of any routine, and it is that people are known and fully be described in the following document: by Schwartz, and Perry ﹠amp; In " the Surface Active Agents and Detergents " I of Berch and the II volume, in " the Nonionic Surfactants " of M.J.Schick and at " the Emulsifiers ﹠amp of McCutcheon; Detergents " in, every piece of document is all incorporated by reference in this article.For example, this nonionogenic tenside material can comprise the compound of producing by alkylene oxide group (hydrophilic) and organic hydrophobic compound (it can be aliphatic series or alkyl aromatic in nature) condensation.Can easily regulate and the length of the polyalkylene oxide groups of any specific hydrophobic grouping condensation so that obtain have required hydrophilic and hydrophobic between the water-soluble cpds of balanced degree.
Other useful ionic surfactant pack is drawn together the polyoxyethylene or the polyoxypropylene condenses of straight or branched, unsaturated or saturated aliphatic carboxylic acid, and it contains about 50 oxyethane of the 5-that had an appointment in 8-18 carbon atom and the addition or propylene oxide units in aliphatic chain.Suitable carboxylic acid comprises: contain average about 12 carbon atoms " coconut " lipid acid (obtaining) from Oleum Cocois, contain " tallow " lipid acid (obtaining), palmitinic acid, tetradecanoic acid, stearic acid and the lauric acid of average about 18 carbon atoms from tallow class fat.
This nonionogenic tenside also can comprise straight or branched, unsaturated or polyoxyethylene or polyoxypropylene condenses that radical of saturated aliphatic is pure, and it contains about 50 oxyethane of the 5-that had an appointment in 8-24 carbon atom and the addition or propylene oxide units.Suitable alcohol comprises: " coconut " Fatty Alcohol(C12-C14 and C12-C18), " tallow " Fatty Alcohol(C12-C14 and C12-C18), lauryl alcohol, tetradecanoic acid and oleyl alcohol.
The alkyl saccharides also can be used for the present composition.Usually, this alkyl saccharides is to have to contain about 8-20 carbon atom, the hydrophobic group of preferred about 10-16 carbon atom and contain those materials of individual saccharides unit, about 1 (list)-10 (gathering) (for example galactoside, glucoside, fructoside, glucosyl group, fructosyl, galactosyl) glycan hydrophilic group.In this alkyl saccharides tensio-active agent, can use the mixture of saccharides part.Preferably, this alkyl saccharides is the alkyl glucoside with following formula:
R
1O(C
nH
2nO)
t(Z)
x
Wherein Z is from glucose deutero-, R
1Be the hydrophobic grouping that is selected from alkyl, alkyl phenyl, hydroxyalkyl, hydroxyalkyl phenyl and composition thereof, wherein this alkyl contains 10-18 the carbon atom of having an appointment, and n is 2 or 3, and t is that 0-is about 10, and x is 1-about 8.The example of such alkyl saccharides is described among US4565647 (25 row-Di, 3 hurdles, the 2nd hurdle, 57 row) and the US4732704 (the 2nd hurdle 15-25 is capable), and the relative section of every piece of document is incorporated by reference in this article.
Semi-polar nonionic surfactants comprises: contain 1 about 10-18 carbon atom alkyl part and 2 and be selected from alkyl or the hydroxyalkyl water-soluble amine oxides partly that contains 1-3 the carbon atom of having an appointment; Contain 1 about 10-18 carbon atom alkyl part and 2 and be selected from alkyl or the hydroxyalkyl water soluble oxidized phosphine partly that contains 1-3 the carbon atom of having an appointment; With contain 1 about 10-18 carbon atom alkyl part and 1 and be selected from alkyl or the hydroxyalkyl water-soluble sulfoxide partly that contains 1-3 the carbon atom of having an appointment.
Amphoterics comprises the aliphatic series of the heterocycle second month in a season or tertiary amine or the derivative of aliphatic derivatives, wherein this aliphatic group can be a straight or branched, and wherein 1 aliphatic substituting group contains at least about 8-18 carbon atom and at least one aliphatic substituting group and contains the anionic water solubilizing group.
Zwitterionics comprises the derivative of aliphatic quaternary ammonium, Phosphonium and sulfonium compound, and wherein 1 aliphatic substituting group contains 8-18 the carbon atom of having an appointment.
Cats product also can comprise in the present invention.Cats product comprises being characterized as to have one or more organic hydrophobic groupings and have all cpds with the associating quaternary nitrogen atoms of acid groups usually in positively charged ion.The quinquevalent nitrogen cyclic cpds also is considered to the quaternary nitrogen compound.Halogenide, Methylsulfate and oxyhydroxide are suitable.Be lower than at about 8.5 o'clock in washing soln pH value, tertiary amine can have the characteristic that is similar to cats product.Openly can in the US4228044 of the Cambre of on October 14th, 1980 promulgation, finding more completely of the cats product that these and other is useful in this article.
Can use and have C
8-C
16Alkyl, preferred C
8-C
9The alkylphenol of the unitary ethoxylation of the about 4-12EO of alkyl and per molecule, or the fatty acid amide of ethoxylation.Other nonionic detergent tensio-active agent that can be used for the object of the invention is apparent to those skilled in the art.Should understand that using the maximum benefit of non-ionic compound is fluid cpds, it more is difficult to be incorporated in the detergent composition with other method, although also can use lotion or solid nonionic detergent compounds.In the latter case, by the temperature that use to raise can so that this non-ionic compound be adsorbed on the lime carbonate.
Preferably, this nonionogenic tenside is the polyoxyethylene or the polyoxypropylene condenses of straight or branched, unsaturated or saturated Fatty Alcohol(C12-C14 and C12-C18), and it contains had an appointment 8-24 carbon atom and addition about 5-50 oxyethane or propylene oxide units.Industrial most important and the easiest this nonionic detergent compounds that obtains comprises the synthetic or natural fatty alcohol of ethoxylation, preferably has C
8-C
18, preferred C
10-C
16The about 3-80 of alkyl and per molecule, preferred unitary uncle of 5-20 oxyethane (EO) or secondary monohydroxy-alcohol.
The example of preferred nonionic compound is to have formula R in such
1(OC
2H
4)
nThe nonionogenic tenside of OH, wherein R
1Be C
8-C
16Alkyl or C
8-C
12Alkyl phenyl, n are 3-about 80.Particularly preferred nonionogenic tenside is C
8-C
16The condensation product of the about 5-20 moles of ethylene oxide of pure and every mol of alcohol is for example with the C of the about 5-9 moles of ethylene oxide of every mol of alcohol condensation
12-C
16Alcohol.Such ionic surfactant pack is drawn together NEODOL
TMProduct, for example Neodol 23-6.5, Neodol 25-7 and Neodol 25-9, they are respectively the C with 6.5 moles of ethylene oxide
12-13Straight chain primary alcohol ethoxylate, C with 7 moles of ethylene oxide
12-15Straight chain primary alcohol ethoxylate and C with 9 moles of ethylene oxide
12-15The straight chain primary alcohol ethoxylate.
The amount that tensio-active agent particularly can be adsorbed on the liquid nonionic surfactants that obtains the unrestricted flow product on the alkaline carbonate normally is up to about 50% of resultant product weight.Although can use more high-load nonionic detergent tensio-active agent if necessary, this tends to not reach purpose of the present invention, because resulting product is lotion or the powder with mobile difference.On the other hand, very being lower than such as about 5% nonionic detergent composition of low levels then obviously only can realize very little benefit.
Alkaline carbonate is about 2 with the ratio of nonionogenic tenside: 1-3.5: the 1st, and ideal.In this proportional range, it is believed that the free-pouring powder that to produce effective cleaning.Preferably, this ratio is about 2.2: 1-3.3: 1, more preferably from about 2.3: 1-2.8: 1.In the most preferred embodiment, alkaline carbonate is about 2.4: 1 with the ratio of nonionogenic tenside.
Preferably, this glass or plastic containers, its amount with about 5-50% of the finished product weight adds.Certainly, must solve the washing composition benefit of high nonionic surfactant concentration and the contradiction of cost-performance.Therefore, the preferable range of nonionogenic tenside is about 20-40% of the finished product weight, more preferably from about 20-30%.Most preferably, the amount of nonionogenic tenside existence is about 25%.Should be noted that: in above-mentioned scope, under the condition of using higher product concentration (as using in Europe usually), often need lower content, on the contrary, under the condition of using than low production concentration (as often occurring in North America and Asia) then use higher content.
By with enough stirrings so that thereby the simple mixing that non-ionic compound fully is distributed on the alkaline carbonate premixture that forms the uniform mixture that contains the alkaline carbonate that nonionic applies can realize that nonionogenic tenside loads and is adsorbed on (with entering in its vesicular structure) on the alkaline carbonate.Can for example finish loading with any known mixing machine with ribbon or ploughshare mixing machine.Preferably, nonionogenic tenside is sprayed on alkaline carbonate and other optional components (if the change that exists), stirs them simultaneously.During premixture of the present invention, importantly apply alkaline carbonate fully in preparation, cause that water can not contact uncoated carbonate and hydrated carbonate immediately when adding entry afterwards with nonionogenic tenside.It is believed that the excessive hydration of carbonate has reduced the amount of dissolving carboxylic acid (this needs other water) used water, thereby reached needed agglomeration particle diameter.
Simultaneously, if there is excessive nonionogenic tenside in premixture, this excessive nonionogenic tenside may apply back blended carboxylic acid so.As a result, dissolving and with alkaline carbonate in and the amount of available carboxylic acid will reduce, this itself can reduce agglomeration efficient and the other carboxylic acid of needs again so that reach needed particle diameter.
In the preferred embodiment of the invention, the yellow soda ash of about 5-80% is mixed with the nonionogenic tenside of about 5-50%, thereby wherein this nonionogenic tenside is the premixture that the tensio-active agent of unique existence forms the uniform mixture contain the alkaline carbonate that nonionic applies.More preferably, this premixture is to form like this: yellow soda ash that will about 20-70% be up to about 5%, the yellow soda ash of preferred about 2-4% silica and the less important detergent components (comprising carboxymethyl cellulose) of about 1-3% are mixed, with the nonionogenic tenside loading of this yellow soda ash, silica and carboxymethyl cellulose being used about 20-40%, wherein this nonionogenic tenside is the only table surface-active agent that is present in this premixture.In a more preferred embodiment, this premixture is to form like this: yellow soda ash that will about 30-65%, the silica of about 0.5-4%, the carboxymethyl cellulose of about 2-3% and a spot of other optionally washing agent component mixing; The nonionogenic tenside of about 20-30% is sprayed on this blended carbonate, silica, carboxymethyl cellulose and the optional component, and wherein this nonionogenic tenside is the detergent surfactant of unique existence.
As mentioned above, add particularly nonionogenic tenside of tensio-active agent, so that it is measured with respect to yellow soda ash in specific ratio with such amount.In this proportional range, this tensio-active agent applies this yellow soda ash fully, and the obvious excessive tensio-active agent that applies carboxylic acid is not provided undesirablely.In addition, it is believed that adding order is important for the needed agglomeration of realization.Realized that by loading alkaline carbonate with tensio-active agent at carboxylic acid and before adding the mixing of entry needed particle diameter also produces free-pouring powder simultaneously.
The 3rd basal component in the free-pouring agglomerant powder detergent composition of the present invention is an alkali metal salt of carboxylic acid, and wherein this carboxylic acid is selected from those carboxylic acids that have the water solubility higher than the water solubility of its corresponding alkali metal salt under first temperature being lower than.Preferably, only the reaction by corresponding carboxylic acid and alkaline carbonate provides this alkali metal carboxylate.Preferred alkali metal carboxylate is selected from alkali metal citrate, basic metal malate and its mixture.Alkali metal citrate is most preferred, because citric acid is relatively cheap and can obtains easily.Alkaline carbonate is in the embodiment preferred of yellow soda ash therein, and this alkali metal carboxylate is selected from Trisodium Citrate, sodium malate and its mixture.
In detergent composition the amount of alkali metal carboxylate be up to about 25%, preferably about 4-18%, and provide by the reaction of corresponding carboxylic acid and alkaline carbonate.The amount when alkali metal carboxylate of it is believed that will preferably realize the agglomeration of the alkaline carbonate that needed nonionogenic tenside loads and form needed particle diameter in this scope the time.More preferably, the amount that this alkali metal carboxylate exists is about 5-13%, and the amount that exists in the most preferred embodiment is about 9-11%.
Ideally, as following further discussion, by in the course of processing with the reaction of alkaline carbonate, this carboxylic acid should be neutralized into its corresponding alkali metal salt basically fully.For example, oxysuccinic acid should be neutralized into the basic metal malate basically fully.Because the restriction of the reaction and the course of processing is not neutralized fully so it is believed that this carboxylic acid.Therefore, it is desirable to,, more preferably be neutralized into its alkali metal carboxylate at least about 99% carboxylate salt preferably at least about 95% at least about 90%.Preferably, this complete basically neutral carboxylic acid is selected from an alkali metal salt of citric acid, oxysuccinic acid and composition thereof.This alkaline carbonate is in the embodiment preferred of yellow soda ash therein, and this complete basically neutral carboxylic acid is selected from Trisodium Citrate, sodium malate and its mixture.
From the finished product required basically fully the amount of the alkaline carbonate of the amount of neutral carboxylic acid and existence can determine to want the amount of blended carboxylic acid.It is desirable to use the carboxylic acid that needs to realize gratifying agglomeration minimum.Yet, this amount must with the amount phase equilibrium that is enough to using the film forming alkaline carbonate of control hard water under those situations of hard water is provided in the finished product.Too high acid content by the neutralization of alkaline carbonate, can cause lower alkalescence, and this may influence the washing composition performance nocuously.On the other hand, acid reduction sour water very little closes and catches the ability that adds moisture and hinder agglomeration.Therefore, the amount that carboxylic acid adds is such, and it makes ratio between alkaline carbonate and the carboxylic acid about 6.5: 1-12: 1 scope, and preferably about 6.5: 1-8: 1 scope, more preferably from about 7: 1.
The premixture that carboxylic acid and its amount is up to the finished product weight about 18% mixes.By the weight of the finished product, the preferable range of mixing acid is about 3-13%, more preferably from about 4-10%, most preferably from about 7-9%.This carboxylic acid only mixes with this premixture a little so that use nonionogenic tenside to apply the ability minimum of carboxylic acid before adding entry afterwards.
With after this premixture mixes a little, add less water at this carboxylic acid so that finish the particulate agglomeration.Water can be used as mist, water vapour or adds with other suitable form.Ideally, the used water yield is as much as possible little so that make subsequent drying time, energy and cost minimum.Therefore the amount that adds entry is about 7% for about 0.1-is not more than, and preferably is not more than about 5%.In a more preferred embodiment, the water of adding is in the scope of about 4-5%.
Use any suitable mixing device that water is joined in the mixture so that realize the agglomeration of this mixture.Preferably, use rotary drum agglomeration machine.Thereby this agglomeration machine rotation makes mixture distribute along this rotary drum length direction, and water is sprayed so that form the agglomerant particle of fine control to the sheet that this mixture falls down simultaneously.
Do not wish to be bound by any particular theory, it is believed that this carboxylic acid is dissolved by alkaline carbonate and neutralizes, and makes this alkaline carbonate hydration simultaneously.This carboxylic acid should be neutralized into its corresponding alkali metal salt basically fully, this an alkali metal salt water-soluble lower than sour form below first temperature.During the neutralization of this carboxylic acid, thereby the alkaline carbonate particle that alkali metal carboxylate adhesive surface promoting agent applies is with their agglomeration and form needed particle diameter.Along with the rotation and the particulate agglomeration of rotary drum, macrobead moves to exit end from the entrance end of agglomeration machine, and they come out and are transported in the drying machine so that remove free-water from agglomerant particle there.This agglomeration machine preferably tilts to cause along with particle agglomeration to outlet from import, and big agglomerant particle moves from the entrance end to the exit end, and they are dried there.
Especially, although do not wish to be constrained in specific theory, thereby it is believed that this carboxylic acid reacts the neutralization fully that becomes basically with water dissolution and with alkaline carbonate.Be lower than under first temperature, this carboxylic acid for example salt of citric acid and oxysuccinic acid has the water solubility lower than its sour form, thereby so this salt from solution, come out bonding and this particle of agglomeration thus.As mentioned above, will produce the hydration of crossing of this yellow soda ash with tensio-active agent insufficient coating on the alkaline carbonate surface.As a result, needing can not obtain the water of this carboxylic acid of dissolving also to need other water and process period so that form needed agglomerant particle size.In addition, the hydration of yellow soda ash be heat release and the crossing hydration and will produce unwanted heat and the temperature of said composition is elevated to more than first temperature of yellow soda ash.Simultaneously, the excessive tensio-active agent that exists in premixture can cause that the coating of carboxylic acid causes the reduction of agglomeration efficient.In addition, need other carboxylic acid and water so that reach needed agglomerant particle size.Therefore, it is believed that the order of adding and temperature are to realizing that needed agglomeration and particle size are important.
It is believed that by after forming premixture, adding carboxylic acid, realizing that the ideal of this carboxylic acid dissolves basically with before the alkaline carbonate reaction.If before adding tensio-active agent, citric acid is mixed with alkaline carbonate, it is believed that so the product that obtains can not reach needed free-flowing property and solvability.
As mentioned above, preferred carboxylic acid has the water solubility higher than its corresponding alkali metal carbonate being lower than under first temperature.Therefore, compare with salt form, temperature is elevated to the relative solubility that will influence this carboxylic acid acid form more than first temperature nocuously, this itself influences agglomeration efficient again nocuously.As a result, the formation of controlling an alkali metal salt of this carboxylic acid is elevated to more than first temperature so that prevent the temperature of this mixture.
Usually, first temperature can be at about 15-40 ℃, preferably about 32-35 ℃.First temperature is higher than about 42 ℃ and appears to influence nocuously product performance, is unfavorable therefore.
Those skilled in the art should understand: can change Several Factors so that control the residence time (promptly the weight of this mixture of handle on bed is divided by combined feed total feed speed) and agglomerant size, these factors are the input speed of for example rotary drum, the angle of rotary drum, the speed of rotation of rotary drum, the amount and the position of water spray.The result who controls these factors controls the particle diameter and the density of agglomerate ideally.
The agglomerant particle of dry wet is so that remove free-water.By any known method for example by roller dryer or on transfer roller dry air can finish this drying.As is known to the person skilled in the art, can regulate the time, temperature and air flow quantity be so that provide gratifying rate of drying.The high envrionment temperature of use can shorten the residence time in drying machine in drying machine, and lower temperature may prolong the residence time inadequately., the Duan residence time may increase the risk of the stable or incomplete dry agglomerates that influences agglomerate nocuously.
It is desirable to as much as possible to remove and anhydrate because there is water, even when water in conjunction with the time, may with the back adding for example deleterious reaction takes place in SYNTHETIC OPTICAL WHITNER and enzyme to the detergent component of moisture-sensitive.In addition, exist water to cross long-time or under general condition of storage, can cause the product caking.Therefore, in preferred embodiments, add less water, remove the entry that adds by drying in addition at least about 50% so that finish agglomeration.More preferably, remove the entry that adds by drying at least about 60%.Therefore, the composition that obtains contains and is less than about 3% combination water, the combination water more preferably less than about 2.
This dry granules has the average grain granularity that is up to about No. 20 USS screen sizes.Preferably, this grain graininess is such, and it makes about 90% the particle scope at about 20-100 USS screen size.The bulk density that obtains powder is 0.7g/cc at least, preferably about 0.8-0.9g/cc, more preferably from about 0.85-0.9g/cc.
Can finish the mixing step for preparing in the detergent composition method of the present invention with various mixing machines known in the art.For example, simple paddle or the hydration of ribbon formula mixing machine are quite effective, and structure also can be used other mixing machine for example rotary drum agglomeration machine, fluidized-bed, disc type agglomeration machine and high shear mixer.
The preferred embodiment of agglomerant detergent composition of the present invention comprises the yellow soda ash of about 20-70%, the tensio-active agent of about 20-40% is nonionogenic tenside especially, the carboxylic acid sodium that is selected from Trisodium Citrate, sodium malate and composition thereof with about 3-13%, wherein this carboxylic acid sodium is to provide by the reaction of following material is unique under the temperature that is lower than first temperature: the premixture that (a) contains tensio-active agent and yellow soda ash, (b) be selected from carboxylic acid of citric acid, oxysuccinic acid and composition thereof and (c) water.
Preferably, the agglomerant detergent composition that obtains from the inventive method comprises the also yellow soda ash of 20-70%, the nonionic detergent tensio-active agent of about 20-40%, wherein this nonionogenic tenside is the detergent surfactant of unique existence, the Trisodium Citrate that is selected from about 4-18%, the carboxylic acid sodium salt of sodium malate and composition thereof, wherein the sodium salt of this carboxylic acid is that the reaction by following material forms under the temperature that is lower than first temperature: the premixture that (a) contains nonionogenic tenside and yellow soda ash, (b) be selected from citric acid, the carboxylic acid of oxysuccinic acid and its mixture and (c) water.
Except above-mentioned basal component, in detergent composition of the present invention, can also comprise the detergent additives that other is conventional.The example of such optional additives is: the foam secondary accelerator for example alkanolamide particularly from palm kernel fatty acid and coconut fatty acid deutero-single ethanol amide, froth suppressor is alkyl phosphate and silicone oil for example, anti redeposition agent is Xylo-Mucine for example, the SYNTHETIC OPTICAL WHITNER of release oxygen is Sodium peroxoborate and SPC-D for example, the peracid bleach precursor, the SYNTHETIC OPTICAL WHITNER that discharges chlorine is an alkali metal salt of trichlorine isocyanic acid and trichlorine isocyanic acid for example, fabric softener, inorganic salt are sodium sulfate for example, anti-dark and gloomy and corrosion inhibitor, soil-suspending agent, dirt release agent and fluorescence (brightening) agent to exist very on a small quantity usually, spices, enzyme, enzyme stabilizers and sterilant.When at one's leisure between dry epoch at detergent composition of the present invention or after, can add these optional additives after preferred.Such component is described among the US3936537, and the document is incorporated by reference in this article.
The silicate that low levels for example is up to about 5% (weight) is favourable aspect the corrosion of metal parts in reducing washing machine usually.Can use for example alkalimetal silicate of useful silicate, particularly neutral, alkaline, inclined to one side-or sodium metasilicate.
In detergent composition of the present invention, water-soluble organic washing-assisting detergent also can be found its purposes.The salt that for example, can comprise ethylenediamine tetraacetic acid (EDTA), triglycollamic acid, oxygen di-succsinic acid, mellitic acid, benzene poly carboxylic acid, polyacrylic acid and polymaleic acid.
Aluminosilicate ion exchange material can be used for detergent composition of the present invention and can comprise the silico-aluminate or the synthetic deutero-silico-aluminate of natural appearance.The method for preparing aluminosilicate ion exchange material has been discussed in US3985669, and the document is incorporated by reference in this article.Such synthetic crystallization aluminosilicate ion exchange material can title zeolite A, zeolite B and X zeolite obtain.In addition, stratiform or structurized silicate for example sell with title SKS-6 by Hoechst-Celanese those also can be used for detergent composition of the present invention.
The SYNTHETIC OPTICAL WHITNER and the activator that can be used for detergent composition of the present invention are described among US4412934 and the US4483781, and these two pieces of documents are incorporated by reference in this article.Suitable bleaching compounds comprises Sodium peroxoborate, SPC-D etc. and composition thereof.This bleaching compounds also can for example tetra acetyl ethylene diamine (TAED), nonanoyl Oxybenzene sodium sulfonate (SNOBS), diperoxy dodecanedioic acid (DPDDA) etc. and composition thereof be used in combination with activator.Sequestrant is described in 54 row-Di, 18 hurdles, the 17th hurdle, 68 row of US4663071, and the document is incorporated by reference in this article.The foaming conditioning agent also be optional components and be described in US3933672 and US4136045 in, these two pieces of documents are incorporated by reference in this article.
Smectic clays goes for herein and is described in 3 row-Di, 7 hurdles, the 6th hurdle, 24 row of US476645, and the document is incorporated by reference in this article.Can be used for the 13rd hurdle 54 row-Di, 16 hurdles, 16 row and the US4663071 that herein other suitable additive is recited in US3936537, these two pieces of documents are incorporated by reference in this article.
In addition, the whitening agent particle can be joined in the above-mentioned exsiccant powder detergent.This whitening agent particle comprises white dyes and this whitening agent that adequately protects is avoided the anion surfactant of the degraded that caused by the nonionogenic tenside that exists.Preferred whitening agent particulate composition and its preparation method are described in respectively in Application No. 08/616570 and the Application No. 08/616208 more fully, and these two pieces of documents are incorporated by reference in this article.
Laundry detergent composition of the present invention can be mixed with pH that about 7-11.5 can the be provided concentration determination of (in 20 ℃ of water with 1% (weight)).For best cleaning performance, the pH scope of about 9.5-11.5 is preferred.
In order to improve solubleness, this detergent composition also can contain the souring agent that the back adds, and as more specifically being described in the Application No. 08/617941, whole disclosures of the document are incorporated by reference in this article.
Following embodiment be used for illustrating the object of the invention and can not think limitation of the present invention.
Embodiment 1
To in table 1, listed component agglomerate into gratifying free-pouring powder detergent with following method.With yellow soda ash, whitening agent, silica and carboxymethyl cellulose mix about 1 minute so that obtain uniform mixture in ribbon mixer.With Neodol 25-7 (with the C of 7 moles of ethylene oxide ethoxylations
12-C
15Pure) be poured on this mixture and mix simultaneously so that apply this yellow soda ash and other component equably.With the yellow soda ash (with other component) of this loading transfer to laboratory scale agglomeration machine (O ' Brien Industrial Equip.Co., 3 ft diams, 1 foot is long) in, will under about 9rpm, rotate about 2 minutes after water spray is on this mixture so that cause the particulate agglomeration.Afterwards, this mixture is dried to about 2.15 moisture content.The bulk density of the composition of gained be 0.85 and flow index (Flodex) value be 12, be at Model No.211, test in the Hansen Research Corp.Flodex testing apparatus.Table 1
Embodiment 2-4
| Material | Amount (weight %) |
| The component (spices, enzyme, brightening agent) that adds behind the fumaric acid that adds behind sodium carbonate (FMC Grade 90) brightening agent (Tinopal SWN) silica (Sipernat 50) carboxymethyl cellulose Neodol 25-7 citric acid waters (adding) water (after dry) | ????55.88 ????0.02 ????3.0 ????2.0 ????22.0 ????7.5 ????4.0 ????1.5 ????5.0 ????3.1 |
With with component below the same procedure agglomeration described in the foregoing description 1, the result also is shown in Table 2.Table 2
| Embodiment | ????2??????3??????4 |
| Material sodium carbonate silica carboxymethyl cellulose brightening agent citric acid water (agglomeration adds) water (after dry) density flow index | Amount (formulation weight) 55.88 55.88 53.18 3.0 3.0 3.0 2.0--2.0 0.02 0.02 0.02 7.5 7.5 7.5 4.0 4.0 4.0 2.2 1.2 1.2 0.85 0.87 0.84 12 9 10 |
Embodiment 5-6
Table 2 has been listed the general quantity of the component that is used to prepare the free-pouring nonionic surfactant detergent of the present invention.Can mixture of sodium carbonate, silica and carboxymethyl cellulose at blended simultaneously, can be sprayed to nonionogenic tenside on this mixture so that apply this mixture.Can mix citric acid then, at blended simultaneously, can with water spray to this mixture so that cause the particulate agglomeration.Can dry this agglomerant particle.Afterwards, the optional components that can add the adding of any back resembles enzyme, and spices etc. and souring agent be fumaric acid for example.
Table 3
| Embodiment | ????5??????6 |
| The fumaric acid that adds behind the accessory constituent that material sodium carbonate silica carboxymethyl cellulose Pareth 25-7 citric acid water (after dry) is chosen wantonly | Amount (% by weight) 59.6 53.2 3.0 3.0 2.2 2.0 24.7 22.0 8.4 7.5 2.1 1.5--5.8--5.0 |
Should understand change and the adjustment that to carry out various wide regions to above-mentioned embodiment.Therefore foregoing description be intended that explanation the present invention rather than restriction the present invention, below claims (comprising all equivalents) be limitation of the invention.
Claims (11)
1. free-pouring agglomerant powder detergent composition, it contains:
A. the alkaline carbonate of about 5-80%;
B. the detergent surfactant of about 5-50%, wherein this detergent surfactant is made up of nonionogenic tenside; With
C. be up to an alkali metal salt of about 25% carboxylic acid, this carboxylic acid is selected from such carboxylic acid, and it has the water solubility higher than the water solubility of its corresponding alkali metal salt being lower than under first temperature.
2. the detergent composition of claim 1, wherein an alkali metal salt of this carboxylic acid is a yellow soda ash.
3. the detergent composition of claim 2, wherein this nonionogenic tenside has formula R
1(OC
2H
4)
nOH, wherein R
1Be C
8-C
16Alkyl or C
8-C
12Alkyl phenyl, n are 3-about 80.
4. the detergent composition of claim 3, wherein yellow soda ash and the ratio of nonionogenic tenside are about 2: 1-3.5: 1 scope.
5. the detergent composition of claim 1, wherein an alkali metal salt of this carboxylic acid is by only providing following substance reaction:
A. the premixture that contains the yellow soda ash of useful nonionogenic tenside coating;
B. be selected from the carboxylic acid of citric acid, oxysuccinic acid and composition thereof; With
C. water.
6. method for preparing free-pouring agglomerant powder detergent composition comprises following step:
A. prepare the alkaline carbonate premixture of uniform surfactant-coated, this premixture contains:
ⅰ. the alkaline carbonate of about 5-80%;
ⅱ. the detergent surfactant of about 5-50%, wherein this detergent surfactant is selected from negatively charged ion, nonionic, zwitter-ion, both sexes, cats product, and composition thereof;
B. then mix and be up to about 15% carboxylic acid so that a mixture is provided, wherein be lower than first temperature, this temperature is lower than about 42 ℃, and this carboxylic acid has the water solubility bigger than its corresponding alkali metal salt; With
C. then water is joined in this mixture, thus this carboxylic acid dissolving and being lower than under first temperature and this alkaline carbonate reaction.
7. the method for claim 6, wherein this alkaline carbonate is a yellow soda ash.
8. the method for claim 6, wherein this tensio-active agent is made up of nonionogenic tenside.
9. the method for claim 8, wherein this yellow soda ash and the ratio of nonionogenic tenside are about 2: 1-3.5: 1 scope.
10. the method for claim 6, wherein carboxylic acid is selected from citric acid, oxysuccinic acid and composition thereof.
11. the method for claim 6, wherein the amount of this carboxylic acid is such, and it makes that the yellow soda ash and the ratio of carboxylic acid are about 6.5: 1-12: 1.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US61644396A | 1996-03-15 | 1996-03-15 | |
| US61656896A | 1996-03-15 | 1996-03-15 | |
| US08/616,443 | 1996-03-15 | ||
| US08/616,568 | 1996-03-15 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1233275A true CN1233275A (en) | 1999-10-27 |
Family
ID=27087752
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97194403.2A Pending CN1233275A (en) | 1996-03-15 | 1997-03-10 | Free-flowing agglomerated nonionic surfactant detergent composition and process for making same |
Country Status (10)
| Country | Link |
|---|---|
| EP (1) | EP0888425B1 (en) |
| JP (1) | JP2002511107A (en) |
| CN (1) | CN1233275A (en) |
| AR (1) | AR006251A1 (en) |
| AT (1) | ATE223472T1 (en) |
| AU (1) | AU715795B2 (en) |
| CA (1) | CA2248994C (en) |
| DE (1) | DE69715170T2 (en) |
| HK (1) | HK1017707A1 (en) |
| WO (1) | WO1997033959A1 (en) |
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| CN111212896A (en) * | 2017-10-13 | 2020-05-29 | 荷兰联合利华有限公司 | Detergent composition comprising hydrate forming salt particles coated with betaine |
| CN111819274A (en) * | 2018-03-08 | 2020-10-23 | 埃科莱布美国股份有限公司 | Solid enzymatic detergent compositions and methods for their use and manufacture |
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| GB2315763A (en) * | 1996-07-31 | 1998-02-11 | Procter & Gamble | Preparation of an agglomerated detergent composition comprising a surfactant a an acid source |
| GB9807477D0 (en) * | 1998-04-07 | 1998-06-10 | Unilever Plc | Coloured granular composition for use in particulate detergent compositions |
| GB9826105D0 (en) † | 1998-11-27 | 1999-01-20 | Unilever Plc | Detergent compositions |
| CA2456095C (en) | 2001-08-31 | 2010-05-11 | Morepen Laboratories Ltd. | An improved process for the preparation of amorphous atorvastatin calcium salt (2:1) |
| US7955616B2 (en) | 2003-09-23 | 2011-06-07 | Orthocon, Inc. | Absorbable implants and methods for their use in hemostasis and in the treatment of osseous defects |
| NZ545521A (en) * | 2003-09-23 | 2010-02-26 | Orthocon Inc | Absorbable implants and methods for their use in hemostasis and in the treatment of osseous defects |
| US7759300B2 (en) * | 2007-07-02 | 2010-07-20 | Ecolab Inc. | Solidification matrix including a salt of a straight chain saturated mono-, di-, or tri- carboxylic acid |
| DE102008028229A1 (en) * | 2008-06-16 | 2009-12-17 | Fit Gmbh | Composition, useful for preparing detergents or in tablet mixture for preparing detergent-molded body for dishwasher, comprises particles comprising alkali metal salt of citric acid and surfactant on their surface layer |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1398263A (en) * | 1971-08-17 | 1975-06-18 | Unilever Ltd | Detergent compositions |
| US3920586A (en) * | 1972-10-16 | 1975-11-18 | Procter & Gamble | Detergent compositions |
| US4666740A (en) * | 1976-12-02 | 1987-05-19 | The Colgate-Palmolive Co. | Phosphate-free concentrated particulate heavy duty laundry detergent |
| US4473485A (en) * | 1982-11-05 | 1984-09-25 | Lever Brothers Company | Free-flowing detergent powders |
| GB9120657D0 (en) * | 1991-09-27 | 1991-11-06 | Unilever Plc | Detergent powders and process for preparing them |
| US5259994A (en) * | 1992-08-03 | 1993-11-09 | The Procter & Gamble Company | Particulate laundry detergent compositions with polyvinyl pyrollidone |
| DE4435743C2 (en) * | 1994-02-17 | 1998-11-26 | Chemolux Sarl | Process for the production of a multi-component granulate |
| US5496486A (en) * | 1994-06-30 | 1996-03-05 | Amway Corporation | Process for increasing liquid surfactant loading in free flowing powder detergents |
-
1997
- 1997-03-10 JP JP53274497A patent/JP2002511107A/en active Pending
- 1997-03-10 AT AT97908065T patent/ATE223472T1/en not_active IP Right Cessation
- 1997-03-10 CA CA002248994A patent/CA2248994C/en not_active Expired - Fee Related
- 1997-03-10 EP EP97908065A patent/EP0888425B1/en not_active Expired - Lifetime
- 1997-03-10 WO PCT/US1997/003741 patent/WO1997033959A1/en active IP Right Grant
- 1997-03-10 AU AU19906/97A patent/AU715795B2/en not_active Ceased
- 1997-03-10 CN CN97194403.2A patent/CN1233275A/en active Pending
- 1997-03-10 DE DE69715170T patent/DE69715170T2/en not_active Expired - Fee Related
- 1997-03-14 AR ARP970101047A patent/AR006251A1/en unknown
-
1999
- 1999-07-06 HK HK99102858A patent/HK1017707A1/en not_active IP Right Cessation
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111212896A (en) * | 2017-10-13 | 2020-05-29 | 荷兰联合利华有限公司 | Detergent composition comprising hydrate forming salt particles coated with betaine |
| CN111212896B (en) * | 2017-10-13 | 2021-07-09 | 荷兰联合利华有限公司 | Detergent composition comprising hydrate forming salt particles coated with betaine |
| CN111819274A (en) * | 2018-03-08 | 2020-10-23 | 埃科莱布美国股份有限公司 | Solid enzymatic detergent compositions and methods for their use and manufacture |
| CN111819274B (en) * | 2018-03-08 | 2022-06-21 | 埃科莱布美国股份有限公司 | Solid enzymatic detergent compositions and methods for their use and manufacture |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0888425A4 (en) | 2000-08-23 |
| EP0888425B1 (en) | 2002-09-04 |
| CA2248994A1 (en) | 1997-09-18 |
| HK1017707A1 (en) | 1999-11-26 |
| AU715795B2 (en) | 2000-02-10 |
| DE69715170D1 (en) | 2002-10-10 |
| WO1997033959A1 (en) | 1997-09-18 |
| AU1990697A (en) | 1997-10-01 |
| ATE223472T1 (en) | 2002-09-15 |
| DE69715170T2 (en) | 2003-05-28 |
| CA2248994C (en) | 2001-05-15 |
| JP2002511107A (en) | 2002-04-09 |
| EP0888425A1 (en) | 1999-01-07 |
| AR006251A1 (en) | 1999-08-11 |
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