DK148038B - PROCEDURE FOR MANUFACTURING LOW-FOAMING DETERGENTS - Google Patents
PROCEDURE FOR MANUFACTURING LOW-FOAMING DETERGENTS Download PDFInfo
- Publication number
- DK148038B DK148038B DK330376AA DK330376A DK148038B DK 148038 B DK148038 B DK 148038B DK 330376A A DK330376A A DK 330376AA DK 330376 A DK330376 A DK 330376A DK 148038 B DK148038 B DK 148038B
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- DK
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- Prior art keywords
- mono
- moles
- ethylene oxide
- detergent
- compound
- Prior art date
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- 239000003599 detergent Substances 0.000 title claims description 26
- 238000000034 method Methods 0.000 title claims description 25
- 238000005187 foaming Methods 0.000 title description 13
- 238000004519 manufacturing process Methods 0.000 title description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 34
- 150000001875 compounds Chemical class 0.000 claims description 22
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 19
- 239000012418 sodium perborate tetrahydrate Substances 0.000 claims description 16
- IBDSNZLUHYKHQP-UHFFFAOYSA-N sodium;3-oxidodioxaborirane;tetrahydrate Chemical compound O.O.O.O.[Na+].[O-]B1OO1 IBDSNZLUHYKHQP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 13
- 239000002518 antifoaming agent Substances 0.000 claims description 12
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 230000003254 anti-foaming effect Effects 0.000 claims description 9
- 150000002148 esters Chemical class 0.000 claims description 9
- 238000001694 spray drying Methods 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 8
- 150000005690 diesters Chemical class 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 5
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 229940055577 oleyl alcohol Drugs 0.000 claims description 3
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims 1
- 239000000843 powder Substances 0.000 description 22
- 238000005406 washing Methods 0.000 description 21
- 150000002191 fatty alcohols Chemical class 0.000 description 19
- 239000003760 tallow Substances 0.000 description 14
- -1 alkylbenzene sulfonates Chemical class 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- FRXGWNKDEMTFPL-UHFFFAOYSA-N dioctadecyl hydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCCCOP(O)(=O)OCCCCCCCCCCCCCCCCCC FRXGWNKDEMTFPL-UHFFFAOYSA-N 0.000 description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 7
- 238000000889 atomisation Methods 0.000 description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 description 7
- 235000011152 sodium sulphate Nutrition 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000002002 slurry Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 4
- 239000007900 aqueous suspension Substances 0.000 description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 4
- 239000000344 soap Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 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 3
- RFIAZLDIPGGNCH-UHFFFAOYSA-I [O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[Na+].CCCCC.[Na+].[Na+].[Na+].[Na+] Chemical compound [O-]P([O-])(=O)OP(=O)([O-])OP(=O)([O-])[O-].[Na+].CCCCC.[Na+].[Na+].[Na+].[Na+] RFIAZLDIPGGNCH-UHFFFAOYSA-I 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 239000007859 condensation product Substances 0.000 description 3
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 3
- 239000000391 magnesium silicate Substances 0.000 description 3
- 229910052919 magnesium silicate Inorganic materials 0.000 description 3
- 235000019792 magnesium silicate Nutrition 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 150000003871 sulfonates Chemical class 0.000 description 3
- FKKAGFLIPSSCHT-UHFFFAOYSA-N 1-dodecoxydodecane;sulfuric acid Chemical compound OS(O)(=O)=O.CCCCCCCCCCCCOCCCCCCCCCCCC FKKAGFLIPSSCHT-UHFFFAOYSA-N 0.000 description 2
- KEZYHIPQRGTUDU-UHFFFAOYSA-N 2-[dithiocarboxy(methyl)amino]acetic acid Chemical compound SC(=S)N(C)CC(O)=O KEZYHIPQRGTUDU-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 239000001177 diphosphate Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 2
- LIFHMKCDDVTICL-UHFFFAOYSA-N 6-(chloromethyl)phenanthridine Chemical compound C1=CC=C2C(CCl)=NC3=CC=CC=C3C2=C1 LIFHMKCDDVTICL-UHFFFAOYSA-N 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 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 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 102000035195 Peptidases Human genes 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- ZUBJEHHGZYTRPH-KTKRTIGZSA-N [(z)-octadec-9-enyl] hydrogen sulfate Chemical compound CCCCCCCC\C=C/CCCCCCCCOS(O)(=O)=O ZUBJEHHGZYTRPH-KTKRTIGZSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 125000002947 alkylene group Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical class OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- JTXUVYOABGUBMX-UHFFFAOYSA-N didodecyl hydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(=O)OCCCCCCCCCCCC JTXUVYOABGUBMX-UHFFFAOYSA-N 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- GYQBBRRVRKFJRG-UHFFFAOYSA-L disodium pyrophosphate Chemical compound [Na+].[Na+].OP([O-])(=O)OP(O)([O-])=O GYQBBRRVRKFJRG-UHFFFAOYSA-L 0.000 description 1
- CSVGEMRSDNSWRF-UHFFFAOYSA-L disodium;dihydrogen phosphate Chemical compound [Na+].[Na+].OP(O)([O-])=O.OP(O)([O-])=O CSVGEMRSDNSWRF-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010616 electrical installation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- YNBADRVTZLEFNH-UHFFFAOYSA-N methyl nicotinate Chemical compound COC(=O)C1=CC=CN=C1 YNBADRVTZLEFNH-UHFFFAOYSA-N 0.000 description 1
- 239000006199 nebulizer Substances 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 229940024999 proteolytic enzymes for treatment of wounds and ulcers Drugs 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 210000002374 sebum Anatomy 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229960001922 sodium perborate Drugs 0.000 description 1
- KEAYESYHFKHZAL-OUBTZVSYSA-N sodium-24 Chemical group [24Na] KEAYESYHFKHZAL-OUBTZVSYSA-N 0.000 description 1
- CVYDEWKUJFCYJO-UHFFFAOYSA-M sodium;docosanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCCCCC([O-])=O CVYDEWKUJFCYJO-UHFFFAOYSA-M 0.000 description 1
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 description 1
- 239000008234 soft water Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- FKHIFSZMMVMEQY-UHFFFAOYSA-N talc Chemical compound [Mg+2].[O-][Si]([O-])=O FKHIFSZMMVMEQY-UHFFFAOYSA-N 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 239000004711 α-olefin Substances 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
- C11D11/02—Preparation in the form of powder by spray drying
-
- 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
- C11D1/02—Anionic compounds
- C11D1/34—Derivatives of acids of phosphorus
- C11D1/345—Phosphates or phosphites
-
- 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
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0026—Low foaming or foam regulating compositions
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)
- Detergent Compositions (AREA)
Description
148038148038
Den foreliggende opfindelse angår en fremgangsmåde til fremstilling af lavtskummende vaskemidler under anvendelse af partielle phosphorsyreestere som skumdæmpende forbindelse.The present invention relates to a process for the preparation of low-foaming detergents using partial phosphoric acid esters as antifoaming agents.
Vaskemidler, der skal anvendes i husholdningsvaskemaskiner, skal have en formindsket eller reguleret skummeevne, for at der ikke skal forekomme overskumning af vaskeflotten under vaskeprocessen, fordi der herved på den ene side sker indskrænkninger i vasketøjets frie bevægelse og på den anden side bevirkes beskadigelser på de elektriske installationer i vaskemaskinen. Af denne grund har man til de hidtil fortrinsvis anvendte, særlig overfladeaktive tensider, såsom alkylbenzensulfonater, alkansulfonater og alkylethersulfater, foruden lavtskummende ikke-ionogene tensider sat væsentlige mængder 2 148038 langkædede alkalimetalsæber og/eller langkædede partielle phosphor-syreestere for herigennem at opnå en acceptabel skumregulering.Detergents to be used in household washing machines must have a diminished or regulated foaming ability so that no washing of the washing float occurs during the washing process, because on the one hand there are restrictions on the free movement of the laundry and on the other, damage to the electrical installations in the washing machine. For this reason, in addition to the predominantly used, particularly surfactant surfactants such as alkylbenzene sulfonates, alkanesulfonates and alkyl ether sulfates, in addition to low foaming nonionic surfactants, substantial amounts of long-chain alkali metal soaps and / or long-chain partial phosphoric acid esters have been obtained for obtaining hereby acceptable .
Det har imidlertid vist sig, at der med sådanne tensidkombinationer i vaskepulvere, der er fremstillet ved varmforstøvningsfremgangsmåden, ikke altid fremkommer en tilfredsstillende skumdæmpning og indtræder overskumning i højere temperaturområder på - over 70°C og i blødt vand med en vandhårdhed på under 10° dH.However, it has been found that with such surfactant combinations in washing powders prepared by the hot spraying process, satisfactory foaming damping does not always occur and foaming occurs in higher temperature ranges of - above 70 ° C and in soft water with a water hardness of less than 10 ° dH .
Denne ulempe gælder også for de rensemidler, der er fremstillet ved fremgangsmåden ifølge tysk fremlæggelsesskrift nr. 1.617.160. Tysk fremlæggelsesskrift nr. 1.617.160 angår en fremgangsmåde til fremstilling af forstøvningstørrede rensepræpara-ter ud fra vandige opslæmninger, der indeholder overfladeaktive ethylenoxid-additionsprodukter og organiske samt uorganiske tilsætningsstoffer, hvilken fremgangsmåde består i, at man forud for, under eller efter fremstillingen af den vandige opslæmning tilsætter en eller flere phosphatestere eller alkalimetalsalte eller ammoniumsalte deraf og dernæst forstøvningstørrer den fremkomne opslæmning på kendt måde.This disadvantage also applies to the detergents produced by the process according to German Patent Specification No. 1,617,160. German Patent Specification No. 1,617,160 relates to a process for preparing spray-dried cleaning preparations from aqueous slurries containing surfactant ethylene oxide addition products and organic as well as inorganic additives, the process of which precedes, during or after the preparation of the aqueous slurry adds one or more phosphate esters or alkali metal salts or ammonium salts thereof and then atomization dries the resulting slurry in known manner.
Det har overraskende vist sig, at den grad af skumdæmpning, der kan opnås i vaskeflotter med ovenstående forbindelser, ved anvendelse af partielle phosphorsyreestere i vaskemidler afhænger af, på hvilken fase af fremstillingsfremgangsmåden for vaskemidlet den partielle phosphorsyreester indføres i vaskemiddelpræparatet.Surprisingly, it has been found that the degree of foam cushioning that can be achieved in wash floats with the above compounds, using partial phosphoric acid esters in detergents, depends on which phase of the detergent preparation process the partial phosphoric acid ester is introduced into the detergent composition.
Man har således erkendt, at der ved indarbejdning af de partielle phosphorsyreestere i den vandige opslæmning af vaskemiddelkomponenterne ifølge tysk fremlæggelsesskrift nr. 1.617.160 fremkommer et vaskemiddel, der ikke har nogen optimal skumdæmpning. Denne erkendelse er overraskende, forsåvidt som partielle phosphorsyreestere som bekendt er relativ temperatur- og hydrolysebestandige, og der ikke kan forventes en sønderdeling eller delvis nedbrydning af esterne under tilberedningen af den vandige opslæmning af vaskemiddelkomponenterne eller under varmforstøvningstørringen af opslæmningen.Thus, it has been recognized that by incorporating the partial phosphoric acid esters into the aqueous slurry of the detergent components according to German Patent Specification No. 1,617,160, a detergent having no optimal foaming is obtained. This finding is surprising, as partial phosphoric acid esters are known to be relatively temperature and hydrolysis resistant, and no decomposition or partial degradation of the esters can be expected during the preparation of the aqueous slurry of the detergent components or during the hot spray drying of the slurry.
Ulemperne ved tysk fremlæggelsesskrift nr. 1.617.160 overvindes ved hjælp af den nedenfor illustrerede opfindelse.The disadvantages of German Patent Specification No. 1,617,160 are overcome by the invention illustrated below.
Den foreliggende opfindelse angår en fremgangsmåde til fremstilling af lavtskummende vaskemidler indeholdende mindst én anionisk eller ikke-ionogen, vaskeaktiv forbindelse, vaskehjælpemidler og tilsætningsstoffer samt en skumdæmpende forbindelse i form af mindst én partiel mono- og/eller diester af ortho-, pyro- 3 148038 eller tripolyphosphorsyre, hvilken partiel mono- og/eller diesters alkoholiske komponent er defineret ved et radikal med den almene formel R -f 0C2H4 + „ hvor R betyder en mættet eller umættet, ligekædet eller forgrenet alkylgruppe med 12 - 22 carbonatomer, og n er et tal fra 0 til 6, hvilken fremgangsmåde er ejendommelig ved, at man forener den skumdæmpende forbindelse med det ud fra de øvrige vaskemiddelkomponenter eller en del af disse komponenter ved varmforstøvningstørring fremstillede forprodukt.The present invention relates to a process for the preparation of low foaming detergents containing at least one anionic or nonionic, detergent-active compound, detergent and additives, and a antifoaming compound in the form of at least one partial mono- and / or diester of ortho-, pyro- or tripolyphosphoric acid, the alcoholic component of the partial mono- and / or diester being defined by a radical of the general formula R -f OC2H4 + where R is a saturated or unsaturated, straight-chain or branched alkyl group having 12-22 carbon atoms and n is a number from 0 to 6, which is characterized by combining the antifoam compound with the precursor product obtained from the other detergent components or a portion of these components by hot spray drying.
Ved anioniske tensider skal forstås de vandopløselige salte af højere fedtsyrer eller harpikssyrer, såsom natrium- eller kaliumsæber af hærdet eller uhærdet kokospalmekerne- eller rapsolie samt af talg og tilsvarende blandinger deraf. Ved anionaktive forbindelser skal der ved den foreliggende opfindelse endvidere forstås højere alkylsubstituerede, énkernede, aromatiske sulfonater, såsom alkylbenzensulfonater med 9-14 carbonatomer i alkylgruppen, alkyl-naphthalensulfonater, alkyltoluensulfonater, alkylxylensulfonater eller alkylphenolsulfonater samt sulfaterede aliphatiske alkoholer eller alkoholethere, såsom natrium- eller kaliumlauryl- eller -hexa-decylsulfat, triethanolaminlaurylsulfat, natrium- eller kaliumoleyl-sulfat samt natrium- eller kaliumsalte af med ca. 2-6 mol ethylen-oxid ethoxyleret laurylsulfat. Yderligere, egnede, anioniske tensider er sekundære lineære alkansulfonater,samt α-olefinsulfonater med en kædelængde på fra 12 til 20 carbonatomer. Inden for rammerne af den foreliggende opfindelse skal der ved ikke-ionogene tensider forstås sådanne forbindelser, som indeholder en organisk hydrofob gruppe samt en hydrofil gruppe. Eksempler på ikke-ionogene tensider er kondensationsprodukterne af alkylphenoler med ethylenoxid eller af højere fedtalkoholer med ethylenoxid, endvidere kondensationsprodukterne af polypropylenglycol med ethylenoxid eller propylenoxid samt kondensationsprodukterne af ethylenoxid med reaktionsproduktet ud fra ethylendiamin og propylenoxid. Også langkædede, tertiære aminoxider hører til gruppen af ovenstående forbindelser.Anionic surfactants are understood to mean the water-soluble salts of higher fatty or resin acids, such as sodium or potassium soaps of cured or uncured coconut palm or rapeseed oil, and of tallow and similar mixtures thereof. Furthermore, by anion-active compounds, the present invention is understood to mean higher alkyl-substituted, single-core, aromatic sulfonates, such as alkyl benzene sulfonates having 9-14 carbon atoms in the alkyl group, alkyl naphthalenesulfonates, alkyltoluenesulfonates, alkylxylene sulfonates or alkylphenol sulfonates, or alcoholates, - or -hexa-decyl sulfate, triethanolamine lauryl sulfate, sodium or potassium oleyl sulfate and sodium or potassium salts of approx. 2-6 moles of ethylene oxide ethoxylated lauryl sulfate. Additional suitable anionic surfactants are secondary linear alkanesulfonates, as well as α-olefin sulfonates having a chain length of from 12 to 20 carbon atoms. Within the scope of the present invention, nonionic surfactants are understood to include such compounds which contain an organic hydrophobic group as well as a hydrophilic group. Examples of nonionic surfactants are the condensation products of alkyl phenols with ethylene oxide or of higher fatty alcohols with ethylene oxide, further the condensation products of polypropylene glycol with ethylene oxide or propylene oxide and the condensation products of ethylene oxide with the reaction product from ethylene diamine and propylene oxide. Also long chain tertiary amine oxides belong to the group of the above compounds.
Ved den her omhandlede fremgangsmåde anvendes f.eks. natriumdodecylbenzensulfonat, talgfedtalkoholethoxylat med 11 - 15 mol ethylenoxid pr. mol fedtalkohol, hærdet talgsæbe, palmi tinf edtaminethoxylat med 8-15 mol ethylenoxid pr. mol fedtamin 4 148038 eller laurylethersulfat med 2-6 mol ethylenoxid pr. mol lauryl-alkohol som vaskeaktive forbindelser.In the method of the present invention, e.g. sodium dodecylbenzenesulfonate, tallow fatty alcohol ethoxylate with 11-15 moles of ethylene oxide per ml. mole of fatty alcohol, cured tallow soap, palm tin edtamine ethoxylate with 8-15 moles of ethylene oxide per or lauryl ether sulfate with 2-6 moles of ethylene oxide per mole of fatamine 4 moles of lauryl alcohol as detergents.
Vaskehjælpemidler ifølge opfindelsen omfatter sådanne produkter som uorganiske eller organiske kompleksdannere, alkalimetal-eller ammoniumsalte af svovlsyre, kiselsyre, carbonsyre, borsyre, alkylen-, hydroxyalkylen- eller aminoalkylenphosphonsyre. Som vaskehjælpemidler anvendes især natriumtripolyphosphat, tetra-natriumdiphosphat, dinatriumdihydrogenphosphat, natriumsulfat, natriumcarbonat, natrium- eller magnesiummetasilicat eller natrium-perborat-tetrahydrat.Laundry aids of the invention include such products as inorganic or organic complexing agents, alkali metal or ammonium salts of sulfuric acid, silicic acid, carbonic acid, boric acid, alkylene, hydroxyalkylene or aminoalkylene phosphonic acid. Sodium tripolyphosphate, tetra-sodium diphosphate, disodium dihydrogen phosphate, sodium sulfate, sodium carbonate, sodium or magnesium metasilicate, or sodium perborate tetrahydrate are used as washing aids.
Forbindelser, der forøger vaskeflotters evne til at bære snavs, såsom carboxymethylcellulose, carboxymethylstivelse, poly-vinylalkohol eller polyvinylpyrrolidon samt stabilisatorer for peroxidforbindelser eller desinfektionsmidler og/eller proteolytiske enzymer kan ligeledes være bestanddele i de ved den her omhandlede fremgangsmåde fremstillede vaskemidler, hvorhos der som egnede stabilisatorer for peroxider skal nævnes fældet magnesiumsilicat, nitrilotrieddikesyre og ethylendiamintetraeddikesyre.Compounds which increase the ability of wash floats to carry debris, such as carboxymethyl cellulose, carboxymethyl starch, polyvinyl alcohol or polyvinylpyrrolidone, as well as stabilizers for peroxide compounds or disinfectants and / or proteolytic enzymes, may also be constituents of the process of the present invention. Stabilizers for peroxides should be mentioned precipitated magnesium silicate, nitrilotriacetic acid and ethylenediaminetetraacetic acid.
En yderligere, foretrukket variant ifølge opfindelsen består i, at der som skumdæmpende forbindelse anvendes mono- eller dilaurylethoxylat-phosphorsyreester med 4 mol ethylenoxid pr. mol laurylalkohol, mono- eller distearylphosphorsyreester, mono- eller distearylethoxylatphosphorsyreester med 2 mol ethylenoxid pr. mol stearylalkohol, mono- eller dioleylethoxylatphosphorsyreester med 4 mol ethylenoxid pr. mol oleylalkohol eller en blanding af mono-og diesteren. Indholdet af den skumdæmpende forbindelse i det færdige vaskemiddel er ca. 0,2 til 2 vægtprocent.A further preferred variant of the invention consists in the use of a mono- or dilaurylethoxylate phosphoric acid ester with 4 moles of ethylene oxide as the antifoam compound. moles of lauryl alcohol, mono- or distearylphosphoric ester, mono- or distearylethoxylate phosphoric ester with 2 moles of ethylene oxide per moles of stearyl alcohol, mono- or dioleylethoxylate phosphoric acid ester with 4 moles of ethylene oxide per mole of oleyl alcohol or a mixture of the mono and diester. The content of the antifoam in the finished detergent is approx. 0.2 to 2% by weight.
Endelig foreligger der forskellige muligheder for at forene den skumdæmpende forbindelse med det ud fra de øvrige vaskemiddelkomponenter eller en del af disse komponenter ved varmforstøvningstørring fremstillede forprodukt. Således kan man f.eks. blande forproduktet, eventuelt i blanding med natriumperborat-tetra-hydrat, mekanisk med den skumdæmpende forbindelse eller sprøjte det med den flydendegjorte skumdæmpende forbindelse under samtidig blanding af forproduktet.Finally, there are various options for combining the antifoam compound with the precursor product prepared from the other detergent components or a portion of these components by hot spray drying. Thus, e.g. mixing the precursor, optionally in admixture with sodium perborate tetrahydrate, mechanically with the antifoaming compound or spraying it with the liquefied antifoaming compound while simultaneously mixing the precursor.
Yderligere, foretrukne alternativer består i, at man blander forproduktet mekanisk med natriumtripolyphosphat, der er sprøjtet med den skumdæmpende forbindelse, eller at man sprøjter forproduktet med en flydende blanding ud fra den skumdæmpende for- 5 148038 bindeIse, den vaskeaktive forbindelse og natriumperborat under samtidig blanding af forproduktet.Further preferred alternatives include mixing the precursor mechanically with sodium tripolyphosphate sprayed with the antifoaming compound or spraying the precursor with a liquid mixture from the antifoaming precursor, washing active compound and sodium perborate. of the pre-product.
Den her omhandlede fremgangsmåde må betegnes som et teknisk fremskridt, fordi den på grund af den senere tilsætning af den skumdæmpende forbindelse til det ved varmforstøvningstørring i forvejen fremstillede vaskemiddelforprodukt muliggør en optimal udnyttelse af de partielle phosphorsyreesteres skumdæmpende virkning. Selv ved forhøjet temperatur af vaskeflotten eller ved anvendelse af et blødt vaskevand med en hårdhedsgrad på under 10° dH opnås der således en tilfredsstillende skumdæmpningseffekt allerede ved en tilsætning på ca.o,2 til 2 yægtprocent partiel phosphorsyre-ester til vaskemidlet, medens f.eks. fremgangsmådeproduktet fra tysk fremlæggelsesskrift nr. 1.617.160 ikke kan forhindre en overskumning af vaskeflotten under tilsvarende betingelser. Anvendelsen af så ringe mængder skumdæmpende forbindelse som muligt er anbefalelsesværdig allerede af økonomiske grunde, fordi fremstillingen af langkædede partielle phosphorsyreestere er kostbar.The process of the present invention must be regarded as a technical advance because, due to the later addition of the antifoam compound to the pre-fabricated detergent drying product, it enables optimal utilization of the antifoaming effect of the partial phosphoric acid esters. Thus, even at elevated temperature of the washing float or using a soft wash water with a hardness degree of less than 10 ° dH, a satisfactory antifoaming effect is already obtained by adding about 2, 2 to 2 weight percent partial phosphoric acid ester to the detergent, while f. eg. the process product from German Patent Specification No. 1,617,160 cannot prevent foaming of the wash fleet under similar conditions. The use of as small amounts of antifoam as possible is advisable already for economic reasons because the preparation of long chain partial phosphoric esters is expensive.
Fremgangsmåden ifølge opfindelsen illustreres nærmere ved nedenstående eksempler.The process according to the invention is further illustrated by the following examples.
Eksempel 1 (sammenligningseksempel) I et anlæg, der består af et apparat til suspen-sionsopberedning og et varmforstøvningstårn, der drives med varm luft ved 320°C ved modstrømsfremgangsmåden, udrøres først 3,2 dele natriumdodecylbenzensulfonat, 1,6 dele talgfedtalkoholethoxylat med 11 mol ethylenoxid pr. mol fedtalkohol, 1,6 dele hærdet talgsæbe, 6,0 dele natriumsulfat, 0,6 dele carboxymethylcellulose, 1,6 dele natriummetasilicat-pentahydrat, 1,6 dele magnesiumsilicat, 19,3 dele pentanatriumtriphosphat og 0,53 dele mono/distearyl-phosphorsyreester (blandingsforhold mellem mono- og diphosphor-syreester 1:4) i 24 dele vand ved 70°C til en homogen suspension, hvorpå der homogeniseres og forstøvningstørres ved 320°C i et varm-luftforstøvningstårn ved modstrømsfremgangsmåden. Det på denne måde fremkomne pulver har et fugtighedsindhold på 11,1%. Dernæst blandes 3 dele af dette pulver mekanisk med 1 del natriumperborat--tetrahydrat.Example 1 (Comparative Example) In a plant consisting of a suspension preparation apparatus and a hot atomization tower operated with hot air at 320 ° C by the countercurrent process, first 3.2 parts of sodium dodecylbenzenesulfonate, 1.6 parts of saturated fatty alcohol ethoxylate are first stirred. ethylene oxide per moles of fatty alcohol, 1.6 parts hardened tallow soap, 6.0 parts sodium sulfate, 0.6 parts carboxymethyl cellulose, 1.6 parts sodium metasilicate pentahydrate, 1.6 parts magnesium silicate, 19.3 parts pentane sodium triphosphate and 0.53 parts mono / distearyl phosphoric acid ester (mixing ratio of mono- and diphosphoric acid ester 1: 4) in 24 parts of water at 70 ° C to a homogeneous suspension and then homogenized and atomized at 320 ° C in a hot-air atomization tower by the countercurrent process. The powder thus obtained has a moisture content of 11.1%. Next, 3 parts of this powder is mechanically mixed with 1 part sodium perborate - tetrahydrate.
6 1480386 148038
Eksempel 2 (sammenligningseksempel)Example 2 (Comparative Example)
Der gås frem analogt med eksempel 1, idet der dog i stedet for 0,53 dele mono/distearylphosphorsyreester tilsættes 1,59 dele af denne partielle phosphorsyreester, og andelene af natriumsulfat reduceres tilsvarende. Det ved varmforstøvningstørringen fremkomne tårnpulver har en fugtighed på 10,5%. Dernæst blandes 3 dele af dette produkt mekanisk med 1 del natriumperborat-tetrahydrat.Analogous to Example 1 is proceeded with, however, instead of 0.53 parts of mono / distearyl phosphoric acid ester 1.59 parts of this partial phosphoric acid ester is added and the proportions of sodium sulfate are reduced accordingly. The tower powder produced by the heat spray drying has a humidity of 10.5%. Next, 3 parts of this product are mechanically mixed with 1 part sodium perborate tetrahydrate.
Eksempel 3 (sammenligningseksempel)Example 3 (Comparative Example)
Der gås frem analogt med eksempel 1, idet der dog i stedet for mono/distearylphosphorsyreesteren tilsættes 0,26 dele natrium-behenat, og andelene af natriumsulfat forhøjes tilsvarende. Det ved varmforstøvningstørringen fremkomne pulver har en fugtighed på 10,8%. 3 dele af dette produkt blandes dernæst mekanisk med 1 del natriumperborat-tetrahydrat.Analogous to Example 1 is proceeded with, however, instead of the mono / distearyl phosphoric acid ester 0.26 parts of sodium behenate is added and the proportions of sodium sulfate are increased accordingly. The powder produced by the hot spray drying has a humidity of 10.8%. Three parts of this product are then mechanically mixed with 1 part sodium perborate tetrahydrate.
Eksempel 4 (sammenligningseksempel)Example 4 (Comparative Example)
Der tilberedes en vandig suspension med nedenstående sammensætning: 3,2 dele natriumdodecylbenzensulfonat, 0,8 dele talgfedt-alkoholethoxylat med 15 mol ethylenoxid pr. mol fedtalkohol, 8,6 dele natriumsulfat, 0,6 dele carboxymethylcellulose, 1,6 dele natriummetasilicat-pentahydrat, 1,6 dele magnesiumsilicat, 19,3 dele pentanatriumtriphosphat og 0,26 dele ethoxyleret mono/-distearylphosphorsyreester med 2 mol ethylenoxid pr. mol stearyl-alkohol (blandingsforhold mellem mono- og diphosphorsyreester 1:5) samt 24 dele vand. Efter homogenisering af denne suspension følger varmforstøvningstørring i et forstøvningstårn med varm luft ved 320°C ved modstrømsfremgangsmåden. Det fremkomne pulver har en fugtighed på 10,6%. Dernæst blandes 71 dele af dette pulver mekanisk med 25 dele natriumperborat-tetrahydrat, og på blandingen sprøjtes yderligere 4 dele af et smeltet talgfedtalkoholethoxylat med 15 mol ethylenoxid pr. mol fedtalkohol under samtidig omrøring af blandingen.An aqueous suspension of the following composition is prepared: 3.2 parts sodium dodecylbenzenesulfonate, 0.8 parts sebum fat alcohol ethoxylate with 15 moles of ethylene oxide per ml. moles of fatty alcohol, 8.6 parts sodium sulfate, 0.6 parts carboxymethyl cellulose, 1.6 parts sodium metasilicate pentahydrate, 1.6 parts magnesium silicate, 19.3 parts pentane sodium triphosphate, and 0.26 parts ethoxylated mono / distearyl phosphoric acid ester with 2 moles ethylene oxide. mole of stearyl alcohol (mixture ratio of mono- and diphosphoric acid ester 1: 5) as well as 24 parts of water. After homogenization of this suspension, hot spray drying follows in a hot air atomization tower at 320 ° C by the countercurrent process. The resulting powder has a humidity of 10.6%. Next, 71 parts of this powder are mechanically mixed with 25 parts of sodium perborate tetrahydrate, and on the mixture a further 4 parts of a molten tallow fatty alcohol ethoxylate is sprayed with 15 moles of ethylene oxide per liter. moles of fatty alcohol while stirring the mixture simultaneously.
Eksempel 5 (sammenligningseksempel)Example 5 (Comparative Example)
Der gås frem analogt med eksempel 4, idet der dog i stedet for de 0,26 dele ethoxyleret mono/distearylphosphorsyreester an 7 148038 vendes 1,6 dele af denne partielle phosphorsyreester, og indholdet af natriumsulfat formindskes tilsvarende. Det efter varmforstøvningstørringen fremkomne pulver har en fugtighed på 10,8%. Pulveret sprøjtes dernæst med smeltet talgfedtalkoholethoxylat analogt med eksempel 4.Analogous to Example 4 is proceeded with, however, instead of the 0.26 parts of ethoxylated mono / distearyl phosphoric acid ester, 1.6 parts of this partial phosphoric acid ester are reversed, and the sodium sulfate content is reduced accordingly. The powder obtained after the hot spray drying has a humidity of 10.8%. The powder is then sprayed with molten tallow fatty alcohol ethoxylate analogous to Example 4.
Eksempel 6 (arbejdsgang ifølge opfindelsen)Example 6 (Invention Procedure)
Der gås frem analogt med eksempel 1, idet der dog ikke sættes partiel phosphorsyreester til den vandige suspension af vaskemiddelkomponenterne. Det ved varmforstøvningstørringen fremkomne pulver har et fugtighedsindhold på 10,8%. Nærmere angivet sættes nedenstående mængder partiel phosphorsyreester samt eventuelt natriumperborat-tetrahydrat til pulveret.Analogous to Example 1 is proceeded with, however, no partial phosphoric acid ester is added to the aqueous suspension of the detergent components. The powder obtained by the hot spray drying has a moisture content of 10.8%. More specifically, the following amounts of partial phosphoric acid ester as well as optionally sodium perborate tetrahydrate are added to the powder.
a) 7,5 kg af pulveret blandes med 2,4 kg natriumperborat-tetrahydrat og 0,1 kg spåneformet mono/distearylphosphorsyreester i en hvirvelblander, b) 7,5 kg af pulveret for-blandes med 2,4 kg natriumperborat--tetrahydrat i en hvirvelblander og sprøjtes dernæst under yderligere blanding med 0,1 kg ved smeltning flydendegjort ethoxyleret mono/distearylphosphorsyreester, der indholder 2 mol ethylenoxid pr. mol stearylalkohol, c) 7,5 kg af pulveret blandes i en hvirvelblander med 2,5 kg af et ved forstøvningsblanding fremstillet produkt ud fra 98 vægtprocent natriumtripolyphosphat og 2 vægtprocent ethoxyleret mono/distearylphosphorsyreester, der indeholder 6 mol ethylen-oxid pr. mol stearylalkohol, og d) 7,5 kg af pulveret for-blandes i en hvirvelblander med 2,4 kg natriumperborat-tetrahydrat og sprøjtes dernæst under yderligere blanding i en hvirvelblander med 0,1 kg mono/dioleylethoxylat-phosphorsyreester (blandingsforhold mellem mono- og diphosphor-syreester 1:5), der indeholder 4 mol ethylenoxid pr. mol oleyl-alkohol.a) 7.5 kg of the powder is mixed with 2.4 kg of sodium perborate tetrahydrate and 0.1 kg of particulate mono / distearyl phosphoric acid ester in a vortex mixer; b) 7.5 kg of the powder is premixed with 2.4 kg of sodium perborate - tetrahydrate in a vortex mixer, and then further blended with 0.1 kg of melt liquefied ethoxylated mono / distearyl phosphoric acid ester containing 2 moles of ethylene oxide per mol. c) 7.5 kg of the powder is mixed in a vortex mixer with 2.5 kg of a product prepared by atomization from 98% sodium tripolyphosphate and 2% by weight ethoxylated mono / distearylphosphoric acid ester containing 6 moles of ethylene oxide per ml. and d) 7.5 kg of the powder is premixed in a vortex mixer with 2.4 kg sodium perborate tetrahydrate and then sprayed under further mixing in a 0.1 kg mono / dioleyl ethoxylate phosphoric acid ester mixer (mono-mixture ratio and diphosphoric acid ester 1: 5) containing 4 moles of ethylene oxide per liter. mole of oleyl alcohol.
Eksempel 7 (arbejdsgang ifølge opfindelsen)Example 7 (Invention Procedure)
Ud fra de i eksempel 4 nævnte vaskemiddelkomponenter med undtagelse af den partielle phosphorsyreester fremstilles og forstøvningstørres en vandig suspension. Det fremkomne pulver har et fugtighedsindhold på 11%. Nærmere angivet sættes nedenstående 8 148038 mængder, beregnet på det færdige vaskepulver, natriumperborat--tetrahydrat, talgfedtalkoholethoxylat, der indeholder 15 mol ethylenoxid pr. mol talgfedtalkohol, og ethoxyleret mono/distearyl-phosphorsyre, der indeholder 2 mol ethylenoxid pr. mol stearyl-alkohol, til dette pulver ved forstøvningsblandingsfremgangsmådens a) 19 vægtprocent natriumperborat-tetrahydrat, 4 vægtprocent talgfedtalkoholethoxylat med 15 mol ethylenoxid pr. mol talgfedtalkohol og 2 vægtprocent ethoxyleret mono/distearylphosphorsyreester med 2 mol ethylenoxid pr. mol stearylalkohol, b) 20 vægtprocent natriumperborat-tetrahydrat, 4 vægtprocent talgfedtalkoholethoxylat med 15 mol ethylen oxid pr. mol talgfedtalkohol og 1 vægtprocent ethoxyleret mono/distearylphosphorsyreester med to mol ethylenoxid pr. mol stearylalkohol, c) 20,5 vægtprocent natriumperborat-tetrahydrat, 4 vægtprocent talgfedtalkoholethoxylat med 15 mol ethylenoxid pr. mol talgfedtalkohol og 0,5 vægtprocent ethoxyleret mono/distearylphosphorsyreester med 2 mol ethylenoxid pr. mol, d) 20,8 vægtprocent natriumperborat-tetrahydrat, 4 vægtprocent talgfedtalkoholethoxylat med 15 mol ethylenoxid pr. mol talgfedtalkohol og 0,2 vægtprocent ethoxyleret mono/distearylphosphorsyreester med 2 mol ethylenoxid pr. mol stearylalkohol.From the detergent components mentioned in Example 4, with the exception of the partial phosphoric acid ester, an aqueous suspension is prepared and atomized. The resulting powder has a moisture content of 11%. Specifically, the following 8 amounts are added, based on the final washing powder, sodium perborate tetrahydrate, sebaceous fatty alcohol ethoxylate containing 15 moles of ethylene oxide per liter. moles of sebaceous fatty alcohol, and ethoxylated mono / distearyl phosphoric acid containing 2 moles of ethylene oxide per ml. a mole of stearyl alcohol, to this powder by the atomization mixture process a) 19% by weight sodium perborate tetrahydrate, 4% by weight tallow fatty alcohol ethoxylate with 15 moles of ethylene oxide per mole of tallow fatty alcohol and 2% by weight ethoxylated mono / distearylphosphoric ester with 2 moles of ethylene oxide per b) 20% by weight sodium perborate tetrahydrate, 4% by weight tallow fatty alcohol ethoxylate with 15 moles of ethylene oxide per mole of tallow fatty alcohol and 1% by weight ethoxylated mono / distearylphosphoric ester with two moles of ethylene oxide per c) 20.5% by weight sodium perborate tetrahydrate, 4% by weight tallow fatty alcohol ethoxylate with 15 moles of ethylene oxide per ml. mole of tallow fatty alcohol and 0.5% by weight ethoxylated mono / distearylphosphoric ester with 2 moles of ethylene oxide per d) 20.8% by weight sodium perborate tetrahydrate, 4% by weight tallow fatty alcohol ethoxylate with 15 moles of ethylene oxide per ml. mole of tallow fatty alcohol and 0.2% by weight of ethoxylated mono / distearyl phosphoric acid ester with 2 moles of ethylene oxide per mole of stearyl alcohol.
Eksempel 8 (arbejdsgang ifølge opfindelsen)Example 8 (Invention Procedure)
Til fremstilling af et varmforstøvet finvaskemiddel, der anvendes i temperaturområdet op til maksimalt 40°C, tilberedes først, en vandig suspension med nedenstående sammensætning.To prepare a hot-sprayed fine washing agent used in the temperature range up to a maximum of 40 ° C, an aqueous suspension of the composition below is prepared first.
3,2 dele natriumdodecylbenzensulfonat, 0,8 dele palmitin-fedtaminethoxylat med 8 mol ethylenoxid pr. mol fedtamin, 1,6 dele laurylethersulfat med 2 mol ethylenoxid pr. mol laurylalkohol, 0,4 dele carboxymethylcellulose, 9,6 dele pentanatriumtriphosphat, 7 dele tetranatriumdiphosphat, 2,6 dele dinatriumdihydrogendiphos-phat, 10,8 dele natriumsulfat og 24 dele vand. Efter homogenisering forstøvningstørres denne suspension ved 300°C i et varmluftfor-stovningstårn ved medstrømsfremgangsmåden. Det fremkomne forstøv 9 148038 ningsprodukt har en fugtighed på 8,2%. På 99 dele af dette forstøvningsprodukt sprøjtes dernæst ved sprøjteblandingsfremgangs-måden 1 del af en ethoxyleret mono/dilaurylphosphorsyreester, der indeholder 4 mol ethylenoxid pr. mol laurylalkohol.3.2 parts sodium dodecylbenzenesulfonate, 0.8 parts palmitine-fatamine ethoxylate with 8 moles of ethylene oxide per moles of fatamine, 1.6 parts of lauryl ether sulfate with 2 moles of ethylene oxide per moles of lauryl alcohol, 0.4 parts carboxymethyl cellulose, 9.6 parts pentane sodium triphosphate, 7 parts tetrasodium diphosphate, 2.6 parts disodium dihydrogen diphosphate, 10.8 parts sodium sulfate and 24 parts water. After homogenization, this suspension is dried at 300 ° C in a hot-air spray tower by the co-flow method. The resulting nebulizer product has a humidity of 8.2%. Then, on 99 parts of this atomization product, 1 part of an ethoxylated mono / dilauryl phosphoric acid ester containing 4 moles of ethylene oxide is sprayed by spraying method. mole of lauryl alcohol.
Afprøvningen af skumdannelsen af de ifølge eksempel 1-7 fremstillede vaskepulvere i vaskeflotter gennemføres i en normal husholdningsvaskemaskine. Til dette formål anbringes 1,2 kg ikke--snavset vævet bomuldstøj i syede strimler på 40 x 80 cm i maskinen som ballast. Vaskepulverdoseringen er 100 g hver gang, idet kun kogevaskeprogrammet anvendes.The testing of the foaming of the washing powders produced in Examples 1-7 in washing floats is carried out in a normal household washing machine. For this purpose, 1.2 kg of non - soiled woven cotton clothing is placed in 40 x 80 cm stitched strips in the machine as a ballast. The washing powder dosage is 100 g each time, using only the boiling program.
Mængden af det vand, der strømmer ind, beløber sig til gennemsnitlig 20 liter. Vandhårdheden af det anvendte ledningsvand er 5° dH. Den skumudvikling, der fremkommer i løbet af kogevaske-processen, iagttages visuelt og registreres i afhængighed af temperaturen. Til dette formål afkobles vaskemaskinens reverseringsrytme i kort tid.The amount of water flowing in averages 20 liters. The water hardness of the tap water used is 5 ° dH. The foam development that occurs during the boiling process is visually observed and recorded depending on the temperature. For this purpose, the washing machine reversal rhythm is switched off for a short time.
De ved de enkelte forsøg opnåede resultater er gengivet i fig. 1-5. Det fremgår heraf, at der med vaskepulverne ifølge fremstillingseksempel 1-3 samt 4 og 5 optræder overskumning af vaskeflotten i temperaturområdet over 70°C, hvilket er vist ved bølgelinien. Med de vaskepulvere, der er fremstillet ifølge fremstillingseksemplerne 6 a) - d) og 7 a) - d) ifølge opfindelsen, iagttages der derimod ingen overskumning af vaskeflotten under den samlede vaskeproces. Med det ifølge eksempel 8 fremstillede finvaskemiddel fremkommer der ligeledes ingen overskumning i temperaturområdet op til 40°C, som skal anvendes til dette produkt, således som dette fremgår af kurveforløbet i fig. 5.The results obtained in the individual experiments are shown in FIG. 1-5. It can be seen from this that with the washing powders according to Preparation Examples 1-3 and 4 and 5, foaming of the washing float occurs in the temperature range above 70 ° C, which is shown at the wavy line. By contrast, with the washing powders prepared according to Preparative Examples 6 a) - d) and 7 a) - d) according to the invention, no foaming of the washing float is observed during the overall washing process. Also, with the fine detergent prepared according to Example 8, no foaming occurs in the temperature range up to 40 ° C which is to be used for this product, as is evident from the curve of FIG. 5th
Claims (5)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2532804 | 1975-07-23 | ||
| DE2532804A DE2532804B2 (en) | 1975-07-23 | 1975-07-23 | Process for the production of low-foaming detergents |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DK330376A DK330376A (en) | 1977-01-24 |
| DK148038B true DK148038B (en) | 1985-02-11 |
| DK148038C DK148038C (en) | 1985-07-08 |
Family
ID=5952168
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DK330376A DK148038C (en) | 1975-07-23 | 1976-07-22 | PROCEDURE FOR MANUFACTURING LOW-FOAMING DETERGENTS |
Country Status (11)
| Country | Link |
|---|---|
| AT (1) | ATA536376A (en) |
| BE (1) | BE844444A (en) |
| CH (1) | CH602914A5 (en) |
| DE (1) | DE2532804B2 (en) |
| DK (1) | DK148038C (en) |
| FR (1) | FR2318921A1 (en) |
| GB (1) | GB1506120A (en) |
| IT (1) | IT1062630B (en) |
| NL (1) | NL7608208A (en) |
| NO (1) | NO762572L (en) |
| SE (1) | SE417725B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4363740A (en) * | 1980-07-29 | 1982-12-14 | Lever Brothers Company | Process for making controlled sudsing detergent powder |
| DE3144470A1 (en) * | 1981-11-09 | 1983-05-19 | Unilever N.V., 3000 Rotterdam | FOAM CONTROLLED DETERGENTS |
| FR2564853B1 (en) * | 1984-05-28 | 1987-08-21 | Lesieur Cotelle | LIQUID COMPOSITION FOR CLEANING HARD SURFACES. |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA810158A (en) * | 1966-01-04 | 1969-04-08 | D. Hathaway Harley | Defoaming agent |
-
1975
- 1975-07-23 DE DE2532804A patent/DE2532804B2/en not_active Withdrawn
-
1976
- 1976-06-23 CH CH804076A patent/CH602914A5/xx not_active IP Right Cessation
- 1976-07-20 GB GB30165/76A patent/GB1506120A/en not_active Expired
- 1976-07-21 IT IT50523/76A patent/IT1062630B/en active
- 1976-07-21 AT AT536376A patent/ATA536376A/en not_active Application Discontinuation
- 1976-07-22 SE SE7608357A patent/SE417725B/en not_active IP Right Cessation
- 1976-07-22 NO NO762572A patent/NO762572L/no unknown
- 1976-07-22 DK DK330376A patent/DK148038C/en not_active IP Right Cessation
- 1976-07-23 NL NL7608208A patent/NL7608208A/en not_active Application Discontinuation
- 1976-07-23 FR FR7622552A patent/FR2318921A1/en active Granted
- 1976-07-23 BE BE169168A patent/BE844444A/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| NO762572L (en) | 1977-01-25 |
| CH602914A5 (en) | 1978-08-15 |
| FR2318921A1 (en) | 1977-02-18 |
| FR2318921B1 (en) | 1980-05-16 |
| DE2532804B2 (en) | 1978-10-05 |
| SE417725B (en) | 1981-04-06 |
| DK148038C (en) | 1985-07-08 |
| BE844444A (en) | 1977-01-24 |
| ATA536376A (en) | 1978-07-15 |
| NL7608208A (en) | 1977-01-25 |
| DE2532804A1 (en) | 1977-02-10 |
| DK330376A (en) | 1977-01-24 |
| GB1506120A (en) | 1978-04-05 |
| IT1062630B (en) | 1984-10-20 |
| SE7608357L (en) | 1977-01-24 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PBP | Patent lapsed |