NO150487B - PROCEDURE FOR THE PREPARATION OF A CRYSTIC DETECTIVE DETERGENT AND CLEANING GRANULATE CONTAINING NON-IONIC TENSID - Google Patents
PROCEDURE FOR THE PREPARATION OF A CRYSTIC DETECTIVE DETERGENT AND CLEANING GRANULATE CONTAINING NON-IONIC TENSID Download PDFInfo
- Publication number
- NO150487B NO150487B NO800437A NO800437A NO150487B NO 150487 B NO150487 B NO 150487B NO 800437 A NO800437 A NO 800437A NO 800437 A NO800437 A NO 800437A NO 150487 B NO150487 B NO 150487B
- Authority
- NO
- Norway
- Prior art keywords
- detergent
- ionic surfactant
- premix
- weight
- formula
- Prior art date
Links
- 239000003599 detergent Substances 0.000 title claims description 32
- 238000000034 method Methods 0.000 title claims description 31
- 239000008187 granular material Substances 0.000 title claims description 9
- 238000004140 cleaning Methods 0.000 title description 3
- 239000002736 nonionic surfactant Substances 0.000 claims description 35
- 150000003839 salts Chemical class 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 19
- 150000001875 compounds Chemical class 0.000 claims description 16
- 239000012459 cleaning agent Substances 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- 239000004615 ingredient Substances 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical class OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 239000004482 other powder Substances 0.000 claims description 4
- 239000012418 sodium perborate tetrahydrate Substances 0.000 claims description 3
- IBDSNZLUHYKHQP-UHFFFAOYSA-N sodium;3-oxidodioxaborirane;tetrahydrate Chemical compound O.O.O.O.[Na+].[O-]B1OO1 IBDSNZLUHYKHQP-UHFFFAOYSA-N 0.000 claims description 3
- 125000003342 alkenyl group Chemical group 0.000 claims 1
- 229920001521 polyalkylene glycol ether Polymers 0.000 claims 1
- 239000000843 powder Substances 0.000 description 32
- 239000004094 surface-active agent Substances 0.000 description 19
- 239000002253 acid Substances 0.000 description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
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- -1 poly-alkylene glycol ether derivatives Chemical class 0.000 description 9
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- 238000001694 spray drying Methods 0.000 description 8
- 239000003760 tallow Substances 0.000 description 8
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- 229910019142 PO4 Inorganic materials 0.000 description 7
- 150000007513 acids Chemical class 0.000 description 7
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- 229960001922 sodium perborate Drugs 0.000 description 7
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 description 7
- 238000000889 atomisation Methods 0.000 description 6
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- 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 5
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 5
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- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 4
- 239000000391 magnesium silicate Substances 0.000 description 4
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- 238000007711 solidification Methods 0.000 description 4
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- JDSQBDGCMUXRBM-UHFFFAOYSA-N 2-[2-(2-butoxypropoxy)propoxy]propan-1-ol Chemical group CCCCOC(C)COC(C)COC(C)CO JDSQBDGCMUXRBM-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
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical class CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- 239000002585 base Substances 0.000 description 3
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- 239000007858 starting material Substances 0.000 description 3
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- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 3
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- 108090000790 Enzymes Proteins 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
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- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- DNEHKUCSURWDGO-UHFFFAOYSA-N aluminum sodium Chemical compound [Na].[Al] DNEHKUCSURWDGO-UHFFFAOYSA-N 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
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- YDSWCNNOKPMOTP-UHFFFAOYSA-N mellitic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(O)=O)=C(C(O)=O)C(C(O)=O)=C1C(O)=O YDSWCNNOKPMOTP-UHFFFAOYSA-N 0.000 description 2
- 235000011837 pasties Nutrition 0.000 description 2
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 2
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- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
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- UGFSLKRMHPGLFU-UHFFFAOYSA-N 2-[5-(1,3-benzoxazol-2-yl)thiophen-2-yl]-1,3-benzoxazole Chemical compound C1=CC=C2OC(C3=CC=C(S3)C=3OC4=CC=CC=C4N=3)=NC2=C1 UGFSLKRMHPGLFU-UHFFFAOYSA-N 0.000 description 1
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- QWZHDKGQKYEBKK-UHFFFAOYSA-N 3-aminochromen-2-one Chemical class C1=CC=C2OC(=O)C(N)=CC2=C1 QWZHDKGQKYEBKK-UHFFFAOYSA-N 0.000 description 1
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- 230000009965 odorless effect Effects 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
- 235000014366 other mixer Nutrition 0.000 description 1
- UFOIOXZLTXNHQH-UHFFFAOYSA-N oxolane-2,3,4,5-tetracarboxylic acid Chemical compound OC(=O)C1OC(C(O)=O)C(C(O)=O)C1C(O)=O UFOIOXZLTXNHQH-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920006149 polyester-amide block copolymer Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001444 polymaleic acid Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 238000005029 sieve analysis Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910021647 smectite Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 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
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 125000000565 sulfonamide group Chemical group 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 150000003628 tricarboxylic acids Chemical class 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Landscapes
- Detergent Compositions (AREA)
Description
Ved fremstilling av vaske- og rensemidler, med.et innhold av ikke-ioniske tensider går man ofte frem således at man påsprøyter, resp. tilblander disse tensider i flytende eller smeltet form.på en. pulverformet bestanddel av middelet, f.eks. tripolyfosfat, perborat eller et silikat med stor sug-bar overflate. Det således behandlede forpulver forenes deretter med de øvrige pulyerbestanddeler. Slike fremgangsmåter er eksempelvis omtalt i US-patent nr. 3 769 222 og DOS 25 35 792 og 27 17 281. Arbeidsmåten har i forhold til varmforstøv-ningstørkning av ikke-ioniske tensidholdige vaskemiddelopp-slemninger den fordel at det ikke oppstår fordampningstap av flyktige ikke-ioniske tensider og avstøvningskammer resp. av-luten forurenses ikke ved de fordampede.deler. In the production of detergents and cleaning agents, with a content of non-ionic surfactants, the procedure is often such that one sprays on, resp. mixes these surfactants in liquid or molten form.on one. powdered component of the agent, e.g. tripolyphosphate, perborate or a silicate with a large absorbent surface. The pre-powder thus treated is then combined with the other pulley components. Such methods are described, for example, in US patent no. 3 769 222 and DOS 25 35 792 and 27 17 281. Compared to hot spray drying of non-ionic surfactant-containing detergent slurries, the working method has the advantage that there is no evaporation loss of volatile -ionic surfactants and dedusting chambers resp. the de-lyte is not contaminated by the evaporated parts.
Da de vanligvis i vaskemidler anvendte ikke-ioniske tensider stivner ved temperaturer under 25-30°C, kan-det imidlertid ved blande- og granuleringsprosessen.komme til betraktelige vanskeligheter når pulveret som skal behandles har en temperatur på mindre enn 20°C, eksempelvis fra 0 til 10°C. Dette er vanligvis tilfelle i den kolde årstid, når pulveret.uttas fra en. vanligvis uoppvarmet vogn eller silo. Det ikke-ioniske tensid stivner da til faste, fettlignende agglomerater og lar seg ikke mere fordele homogent i pulveret. Da det imidlertid i. stortekniske områder er forholdsvis om-stendelig og'komplisert å oppvarme større pulvermengder jevnt, er man tvunget til å anvende slike ikke-ioniske tensider eller tensidblandinger.som ved de lave temperaturer ennu er flytende eller i det minste ennu tilstrekkelig pastøse, således at de. ennu lar seg fordele homogent, sammenlign her tysk patent. 24 18 294. Man er imidlertid da betraktelig begrenset i valg av tensider, dvs. det kan ikke mere foregå etter synspunkt av en optimal rense- og smussbæreevne. Spesielt de meget, vaskevirk-somme, godt vannoppløselige, høyere etoksylerte forbindelser er ikke mere anvendbare i disse tilfeller. Man er heller anvist til anvendelsen av laveresmeltende kokosfettalkoholetoksylater med lav etoksyleringsgrad, som imidlertid har en sterk egen-lukt, som av mange forbrukere finnes ubehagelig. Videre er det fra US-PS 21 74 161 kjent ikke-ioniske tensider som avleder seg fra alifatiske eller cykloalifatiske alkoholer, fenoler, naftoler og aminoalkoholer og fremstilles således at man til utgangsforbindelsen først tilleier propylenoksyd og deretter etylenoksyd, idet hver gang delene av propylen- resp. etylenoksyd velges således at det oppstår i vann oppløselige resp. dispergerbare produkter. Disse kan blant aneet i tekstilindustrien anvendes som ullvaskemiddel eller kalksåpedispergatorer sammen med ytterligere vanlige vaskemiddelbestanddeler. Teknisk interesse har slike alkoksylater ikke funnet hvorfor de også siden ikke igjen er benyttet. Angivelsen over hvorledes de angjeldende alkoksylater- videreforarbeides resp. på hvilken måte de eventuelt skal innfor-lives i et vaskemiddel eksisterer ikke. As the non-ionic surfactants usually used in detergents harden at temperatures below 25-30°C, considerable difficulties can arise during the mixing and granulation process when the powder to be treated has a temperature of less than 20°C, for example from 0 to 10°C. This is usually the case in the cold season, when the powder is extracted from a. usually unheated wagon or silo. The non-ionic surfactant then solidifies into solid, fat-like agglomerates and can no longer be distributed homogeneously in the powder. Since, however, in high-tech areas it is relatively time-consuming and complicated to heat large amounts of powder evenly, one is forced to use such non-ionic surfactants or surfactant mixtures, which at the low temperatures are still liquid or at least still sufficiently pasty , so that they. can still be distributed homogeneously, compare German patent here. 24 18 294. However, one is then considerably limited in the choice of surfactants, i.e. it can no longer proceed from the point of view of an optimal cleaning and dirt carrying capacity. In particular, the highly detergent-active, highly water-soluble, higher ethoxylated compounds are no longer applicable in these cases. Rather, one is directed to the use of lower-melting coconut fat alcohol ethoxylates with a low degree of ethoxylation, which, however, have a strong odor, which many consumers find unpleasant. Furthermore, non-ionic surfactants are known from US-PS 21 74 161 which are derived from aliphatic or cycloaliphatic alcohols, phenols, naphthols and amino alcohols and are produced in such a way that one first adds propylene oxide and then ethylene oxide to the starting compound, each time the parts of propylene respectively ethylene oxide is selected so that water-soluble resp. dispersible products. These can, among other things, be used in the textile industry as wool detergent or lime soap dispersants together with further common detergent ingredients. Technical interest has not been found in such alkoxylates, which is why they have not been used since. The indication of how the relevant alkoxylates are further processed resp. in which way they should possibly be incorporated into a detergent does not exist.
Det lar seg forøvrig vise at stivnepunktet av de fra Cj 2-Cig-alkoholer avledede propylerioksyd- étylenoksydaddukter ikke adskiller seg vesentlig fra stivnepunktet av analoge étylenoksydaddukter med samme alkoksyleringsgrad. Det var derfor heller ikke å vente at produktene ville forholde seg vesentlig annerledes ved vanlige blande- og granulerings-prosesser enn de generelt vanlige relativt høytsmeltende fett-alkoholetoksylater. Problemet besto mere i å utvikle en fremgangsmåte som muliggjør å blande ikke-ioniske tensider jevnt på pulverformede vaskemiddelbestanddeler som f.eks. natriumperborat idet også da det ville oppnås en homogen fordeling av det ikke-ioniske tensid når de pulverformede komponenters temperatur ligger vesentlig under stivnetemperaturen av det tensid som skal påblandes. Dette problem løses ved foreliggende op<p>finnelse. Incidentally, it can be shown that the solidification point of the propyleryoxide-ethylene oxide adducts derived from Cj 2-Cig alcohols does not differ significantly from the solidification point of analogous ethylene oxide adducts with the same degree of alkylation. It was therefore also not to be expected that the products would behave significantly differently in normal mixing and granulation processes than the generally common relatively high-melting fat-alcohol ethoxylates. The problem consisted more in developing a method which makes it possible to mix non-ionic surfactants evenly on powdered detergent ingredients such as e.g. sodium perborate also since a homogeneous distribution of the non-ionic surfactant would be achieved when the temperature of the powdered components is significantly below the solidification temperature of the surfactant to be mixed. This problem is solved by the present invention.
Det er nu funnet en fremgangsmåte som unngår de om-talte ulemper. Oppfinnelsens gjenstand er en fremgangsmåte til fremstilling av et risledyktig, ikke-ionisk vaske- og rensemiddelgranulat som inneholder et tensid fra klassen poly-alkylenglykoleterderivater ved'tilblanding av det ikke-ioniske tensid til en pulverformet til kornet bestanddel av vaske- og rensemiddelet og etterfølgende blanding av den således dannede forblanding med de øvrige bestanddeler av vaske-og rensemiddelet, idet fremgangsmåten er karakterisert ved at det som ikke-ionisk tensid anvendes en i og for seg kjent forbindelse med den generelle formel I A method has now been found which avoids the aforementioned disadvantages. The object of the invention is a method for the production of a free-flowing, non-ionic detergent and cleaning agent granule which contains a surfactant from the class of poly-alkylene glycol ether derivatives by mixing the non-ionic surfactant into a powdery to granular component of the detergent and subsequent mixing of the thus formed premix with the other components of the detergent, the method being characterized in that a known compound with the general formula I is used as a non-ionic surfactant
hvori R betyr en alifatisk hydrokarbonrest med 8 til 20 karbonatomer, m betyr et tall fra 0,5 til 8 og n et tall fra 2 til 20, med den forholdsregel at n er lik eller større enn m, i en mengde av 5-20 vekt-% av forblandingen. wherein R means an aliphatic hydrocarbon residue having 8 to 20 carbon atoms, m means a number from 0.5 to 8 and n a number from 2 to 20, with the precaution that n is equal to or greater than m, in an amount of 5-20 % by weight of the premix.
Fortrinnsvis anvendes forbindelser med formel I,, hvori R betyr en primær alkyl- eller alkylenrest med 12 til 18 karbonatomer og hvor m betyr et tall fra 1 til 5 og n betyr et tall fra 3 til 15 med den forholdsregel at n utgjør 2 ganger til 10 ganger m. Preferably, compounds of formula I are used, in which R means a primary alkyl or alkylene residue with 12 to 18 carbon atoms and where m means a number from 1 to 5 and n means a number from 3 to 15 with the precaution that n amounts to 2 times 10 times m.
Ikke-ioniske tensider med formel I er kjent og fås eksempelvis ifølge US patent 2 174 761 ved omsetning av alkoholer med propylenoksydet og deretter med etylenoksyd. Non-ionic surfactants with formula I are known and are obtained, for example, according to US patent 2,174,761 by reacting alcohols with propylene oxide and then with ethylene oxide.
Man kan gjennomføre fremgangsmåten således at man blander en blanding av ønskelig pulverformede vaskemiddelbestanddeler, eventuelt etter foregående granulering eller forstøvningstørkning, med de ikke-ioniske tensider med formel I og deretter granulerer, idet en jevn blanding lettes ved påsprøytning av tensidet i form av en fin forstøvningståke. Fortrinnsvis behandles imidlertid en bestemt pulverbestand-del av vaskemiddelet med fremgangsmåten ifølge oppfinnelsen, bg denne tensidholdige forblanding forenes deretter med de øvrige pulverbestanddeler. For dette formål egner det seg spesielt de såkalte.byggersalter, hvortil det hører de kon-denserte fosfater, alkalisilikater, alkalikarbonater, alkali-borater og alkalisulfater. Egnet er videre vannuoppløselige byggersalter, spesielt ioneutvekslende natriumaluminiumsili-kater med formel The method can be carried out in such a way that a mixture of desirable powdered detergent ingredients is mixed, possibly after prior granulation or spray drying, with the non-ionic surfactants of formula I and then granulated, a uniform mixture being facilitated by spraying the surfactant in the form of a fine atomizing mist . Preferably, however, a specific powder constituent part of the detergent is treated with the method according to the invention, because this surfactant-containing premix is then combined with the other powder constituents. The so-called building salts are particularly suitable for this purpose, which include condensed phosphates, alkali silicates, alkali carbonates, alkali borates and alkali sulphates. Water-insoluble building salts are also suitable, especially ion-exchanged sodium aluminum silicates with the formula
hvor X betyr 0,9 - 13, Y betyr 1,3 - 4 og z betyr \ - 6. where X means 0.9 - 13, Y means 1.3 - 4 and z means \ - 6.
Egnet er videre kieselsyreholdige midler resp. kolloidal leire, som overflateaktive kieselsyre ("Aerosil")/ magnesiumsilikat, bentoniter og smektit-leire. Riktignok er slike stoffer mindre interessante fra et vasketeknisk synspunkt da de i motsetning til byggersaltene bare virker som adsorpsjons-middel og ikke bidrar til vaske- og rensevirkningen. Av de nevnte byggersalter gjelder derfor fosfater, spesielt pentanatriumtrifosfat, samt de ioneutvekslende natriumaluminium-silikater som foretrukkede utgangsstoffer. Også blandinger av forskjellige pulverformede eller kornede materialer kan anvendes for det nevnte formål. Also suitable are agents containing silicic acid or colloidal clay, such as surfactant silicic acid ("Aerosil")/magnesium silicate, bentonites and smectite clays. Admittedly, such substances are less interesting from a washing technical point of view as, in contrast to building salts, they only act as adsorption agents and do not contribute to the washing and cleaning effect. Of the building salts mentioned, phosphates, especially pentasodium triphosphate, as well as the ion-exchanged sodium aluminum silicates are therefore preferred starting materials. Mixtures of different powdered or granular materials can also be used for the aforementioned purpose.
Som spesielt hensiktsmessige har det vist seg anvendelsen av pulverformet resp. kornet natriumperborattetra-hydrat som utgangsmaterial for forblandingen. Man sparer på denne måte en ekstra blandeprosess, da perboratet på grunn av sin termiske følsomhet vanligvis ikke forstøvningstørkes sammen med de øvrige vaskemiddelbestanddeler, men først til-blandes til forstøvningsproduktet etterpå. Den spesielle egen-skap av natriumperborat er overraskende da vanlig teknisk perborat vanligvis ikke er krystallinske og ikke porøse og derfor bare har en forholdsvis liten opptaksevne for flytende resp. pastøse stoffer. The use of powdered resp. granular sodium perborate tetrahydrate as starting material for the premix. In this way, an additional mixing process is saved, as the perborate, due to its thermal sensitivity, is usually not spray-dried together with the other detergent ingredients, but is first mixed into the spray product afterwards. The special property of sodium perborate is surprising as common technical perborates are usually not crystalline and not porous and therefore only have a relatively small absorption capacity for liquid or pasty substances.
Ved blande- resp. granuleringsprosessen dannes stabile agglomerater av de ikke-ioniske tensider og byggersaltene resp. perboratpartiklene idet tensidet dannet et mer eller mindre lukket overtrekk på partiklene. Mengden av ikke-ionisk middel skal, referert yil tensidholdig perborat-forblanding, utgjøre 5 til 20 vekt-%, fortrinnsvis 7 til 15 vekt-%. Anvendes byggersalter som grunnpulver, kan- mengden av det ikke-ioniske tensid som skal tilføres ligge innen de samme grenser. Hvis byggersaltene foreligger i voluminøs resp. forstøvnings-tørket form, f.eks. ved anvendelse av natriumaluminiumsili-kater eller voluminøse tripolyfosfater som grunnpulver, kan mengden av ikke-ionisk tensid økes inntil 35 vekt-%, fortrinnsvis anvendes inntil 20 vekt-%, referert til tensidholdig forblanding. Mengden av det ikke-ioniske tensid med formel I og mengden av den dermed fremstilte forblanding innstilles fortrinnsvis således at innholdet av det ikke-ioniske tensid i det ferdige vaske- og rensemiddel utgjør 1 til 10 vekt-%. When mixing or the granulation process, stable agglomerates are formed of the non-ionic surfactants and the building salts resp. the perborate particles as the surfactant formed a more or less closed coating on the particles. The amount of nonionic agent, referred to the surfactant-containing perborate premix, should amount to 5 to 20% by weight, preferably 7 to 15% by weight. If building salts are used as a foundation powder, the amount of non-ionic surfactant to be added can be within the same limits. If the building salts are available in voluminous or spray-dried form, e.g. when using sodium aluminum silicates or voluminous tripolyphosphates as base powder, the amount of non-ionic surfactant can be increased up to 35% by weight, preferably up to 20% by weight, referred to surfactant-containing premix. The amount of the non-ionic surfactant with formula I and the amount of the thus produced premix are preferably adjusted so that the content of the non-ionic surfactant in the finished detergent and cleaning agent amounts to 1 to 10% by weight.
Fremstillingen av agglomeratene resp. overtrekkene The production of the agglomerates or the covers
kan foregå således at det smeltede, til temperaturer over 30°C, fortrinnsvis 50° til 70°C oppvarmede ikke-ioniske tensid blandes godt med det pulverformede til kornede byggersalt eller natriumperborat. Grunnpulveret som anvendes kan ha en temperatur på 0° til 30°C. En ekstra oppvarmning av pulveret under blandeprosessen er ikke nødvendig. Det er også ved anvendelse av et relativt koldt pulver sikret en homogen fordeling uten støvdannelse. can take place in such a way that the melted non-ionic surfactant heated to temperatures above 30°C, preferably 50° to 70°C, is mixed well with the powdered to granular building salt or sodium perborate. The base powder used can have a temperature of 0° to 30°C. Additional heating of the powder during the mixing process is not necessary. A homogeneous distribution without dust formation is also ensured by using a relatively cold powder.
Sammenblandingen kan foretas kontinuerlig eller por-sjonsvis under anvendelse av vanlige blande-, granulerings-eller forstøvningsinnretninger. Egnet er f.eks. trommel-, kaskade-, plogskovel- eller andre blandere som arbeider etter tvangsblandefremgangsmåten, samt anordninger, hvor den flytende smelte kontinuerlig påsprøytes et frittfallende eller på The mixing can be carried out continuously or in portions using conventional mixing, granulating or atomizing devices. Suitable is e.g. drum, cascade, plow vane or other mixers that work according to the forced mixing method, as well as devices, where the liquid melt is continuously sprayed onto a free-falling or on
et transportbånd i tynnsjikt utbredt pulver. Etter påsprøyt-ningen kan det slutte seg eventuelt en ettergranulering. a conveyor belt in thin layer spread powder. After the spraying, post-granulation may be added.
Kornstørrelse og litervekt av det anvendte byggersalt resp. natriumperborat kan svinge innen vide grenser. Grain size and liter weight of the building salt used resp. sodium perborate can fluctuate within wide limits.
Mest hensiktsmessig skal imidlertid mengden grovkornede partikler med en kornstørrelse på mer enn 2 mm utgjøre mindre enn 10 vekt-% og fortrinnsvis mindre enn 2 vekt-%. Mengden av partikler med en kornstørrelse under 0,1 mm utgjør fortrinnsvis mindre enn 25 vekt-% og spesielt mindre enn 10 vekt-%. Most appropriately, however, the amount of coarse-grained particles with a grain size of more than 2 mm should amount to less than 10% by weight and preferably less than 2% by weight. The amount of particles with a grain size below 0.1 mm preferably amounts to less than 25% by weight and in particular less than 10% by weight.
Den midlere kornstørrelse er mest hensiktsmessig fra 0,1 til 0,8 mm. The average grain size is most suitable from 0.1 to 0.8 mm.
Ved behandlingen med det flytende tensid inntrer vanligvis en kornøkning, idet i første rekke partikler med en kornstørrelse på mindre enn 0,2 mm sterkt.eller fullstendig sammenkittes til større partikler. Partikler med en korn-størrelse fra 1 til 3 mm øker bare lite. Eventuelt kan partikler utsiktes, knuses og deretter videreanvendes. Den midlere kornstørrelse av det med ikke-ionisk tensid behandlede perborat resp. byggersalt utgjør 0,4 til 1,0 mm og ligger dermed i størrelsesorden av et ved hjelp av forstøvningstørkning eller granulering dannet vaske- og rensemiddelpulver. Heri sees en spesiell fordel, da herved motvirkes uønskede sepa-reringsprosesser under transport eller lagring av vaskemiddelet. During the treatment with the liquid surfactant, a grain increase usually occurs, as primarily particles with a grain size of less than 0.2 mm are strongly or completely aggregated into larger particles. Particles with a grain size of 1 to 3 mm increase only slightly. If necessary, particles can be screened, crushed and then reused. The average grain size of the non-ionic surfactant-treated perborate resp. building salt amounts to 0.4 to 1.0 mm and is thus in the order of magnitude of a washing and cleaning agent powder formed by means of spray drying or granulation. This is seen as a particular advantage, as unwanted separation processes are counteracted during transport or storage of the detergent.
Forblandingen fremstilt ifølge oppfinnelsen kan, spesielt, når det blir fremstilt under anvendelse av byggersalter som tripolyfosfat eller natriumaluminiumsilikat, innblåses umiddelbart i forstøvningstårnet som tjener til forstøvnings-tørkning av vaskemiddeloppslemmingen. Tilførselen foregår da mest hensiktsmessig innenfor resp. under området av forstøv-ningsdysene av oppslemningene. De forstøvede vaskemiddel-dråper og de innstøvede forblandepartikler forbinder resp. sammenkitter seg derved til et løst, homogent pulver som ikke separerer. For denne i og for seg kjente samtidige tørke- og blandefremgangsmåte hvor det spares et ekstra blandetrinn og en del av fordampningsenergien, er fremgangsmåteproduktene spesielt godt egnet da tensidene med formel I overraskende viser en spesielt liten tendens til såkalt "pluming". Med "pluming" betegner man den uønskede dannelse av røkskyer i avluften av forstøvningstørkeanlegg, frembragt ved hjelp av vanndampflyktige ikke-ioniske tensider. Det fører til tap av vaskeaktivt stoff og til forurensning av avluften samt til dannelse av uønskede fettagglomerater i avstøvningsanlegg. The premix produced according to the invention can, in particular, when it is produced using building salts such as tripolyphosphate or sodium aluminum silicate, be blown immediately into the atomization tower which serves for atomization drying of the detergent slurry. The supply then takes place most appropriately within resp. below the area of the atomizing nozzles of the slurries. The nebulized detergent droplets and the entrained premix particles connect resp. thereby clumping together into a loose, homogeneous powder that does not separate. For this per se known simultaneous drying and mixing method where an extra mixing step and part of the evaporation energy is saved, the process products are particularly well suited as the surfactants with formula I surprisingly show a particularly small tendency to so-called "pluming". "Pluming" refers to the unwanted formation of smoke clouds in the exhaust air of spray drying facilities, produced with the help of water vapor-volatile non-ionic surfactants. This leads to a loss of detergent active substance and to pollution of the exhaust air as well as to the formation of unwanted fat agglomerates in dust removal systems.
Eventuelt kan det sammen med den ikke-ioniske forbindelse dessuten påføres ytterligere tilsetningsstoffer som farvestoffer, pigmenter eller luktstoffer på natriumperbo-ratet resp. byggersaltet. Ved anvendelsen av farvede tilsetningsstoffer lar det seg oppnå en optisk tiltalende og til karakterisering tjenende farvenyanse av pulverblandingen. Optionally, together with the non-ionic compound, further additives such as dyes, pigments or odorants can also be applied to the sodium perborate or the building salt. By using colored additives, it is possible to achieve an optically appealing and characterizing shade of the powder mixture.
Natriumperborathaldige forpulver blandes med de øvrige pulverbestanddeler mest hensiktsmessig etter deres forstøvningstørkning. Også forpulver inneholdende byggersalter kan på denne måte videreforarbeides, idet det kan anvendes vanlige blandeinnretninger. Prepowders containing sodium perborate are mixed with the other powder components most appropriately after their spray drying. Pre-powders containing building salts can also be further processed in this way, as ordinary mixing devices can be used.
Vektforholdet mellom forpulveret som inneholder tensidet med formel I, og de ved forstøvningstørkning eller også granulering fremstilte pulverformede vaske- og rensemiddel-blandinger utgjør 1:10 til 1:3, idet innholdet av tensidet med formel I i det sammensatte vaske- og rensemiddel kan ligge mellom 1 og 10 vekt-%. I tilfelle av tekstilvaskemiddel, inneholder dette komponenter av minst et anionisk, ikke-ionisk eller zwitterionisk tensid, samt for det meste et byggerstoff som virker kompleksdannende resp. binder vannets kalkhårdhet, samt eventuelt ytterligere vaskehjelpestoffer. The weight ratio between the pre-powder containing the surfactant with formula I, and the powdered detergent and cleaning agent mixtures produced by spray drying or granulation amounts to 1:10 to 1:3, as the content of the surfactant with formula I in the combined detergent and cleaning agent can be between 1 and 10% by weight. In the case of textile detergent, this contains components of at least one anionic, non-ionic or zwitterionic surfactant, as well as mostly a building material that acts as a complexing agent or binds the water's limescale hardness, as well as any additional washing aids.
Egnede anioniske tensider er slike av sulfonat- eller sulfattypen, spesielt alkylbenzensulfonater, olefinsulfonater, alkylsulfonater bg a-sulfofettsyreestere, primære alkylsul-fater samt sulfatene av etoksylerte, 2 til 3 glykoletergruppe-holdige høyeremolekylære alkoholer. Aktuelle er videre alkali-såper av fettsyrer av naturlig eller syntetisk opprinnelse, f.eks. natriumsåpen av kokos-, palmekjerne- eller talgfett-syrer, og hvis en skumdempning er ønskelig, også slike av hydrerte raps- eller fiskeoljefettsyrer. Som zwitterioniske tensider kommer det på tale alkylbetainer og spesielt alkyl-sulfobetainer. De anioniske tensider foreligger fortrinnsvis i form av natriumsalter. Hvis de nevnte anioniske og zwitterioniske forbindelser har en alifatisk hydrokarbonrest, skal denne fortrinnsvis være rettlinjet og ha 8 til 22, fortrinnsvis 12 til 18 karbonatomer. I forbindelsene med en aralifatisk hydrokarbonrest inneholder de fortrinnsvis uforgrenede alkyl-kjeder 6 til 16, spesielt 10 til 14 karbonatomer. Suitable anionic surfactants are those of the sulfonate or sulfate type, especially alkylbenzenesulfonates, olefinsulfonates, alkylsulfonates such as α-sulfofatty acid esters, primary alkyl sulfates and the sulfates of ethoxylated, 2 to 3 glycol ether group-containing higher molecular weight alcohols. Also relevant are alkali soaps of fatty acids of natural or synthetic origin, e.g. the sodium soap of coconut, palm kernel or tallow fatty acids, and if a foam suppression is desired, also those of hydrogenated rapeseed or fish oil fatty acids. Zwitterionic surfactants include alkyl betaines and especially alkyl sulfobetaines. The anionic surfactants are preferably in the form of sodium salts. If the anionic and zwitterionic compounds mentioned have an aliphatic hydrocarbon residue, this should preferably be linear and have 8 to 22, preferably 12 to 18 carbon atoms. In the compounds with an araliphatic hydrocarbon residue, they preferably contain unbranched alkyl chains of 6 to 16, especially 10 to 14 carbon atoms.
I en foretrukket utførelsesform inneholder de for-støvningstørkede vaskemidler for det meste et ikke-ionisk tensid,.som adskiller seg fra forbindelsen ifølge formel I. Dette er de etoksylerte alkoholer, vicinale dioler og alkyl-fenoler av den angitte formel med gjennomsnittlig 3 til 20, fortrinnsvis 5 til 15 glykoletergrupper. Spesielt egnet er blandinger av etoksylerte, primære Cj ^j-C^-alkoholer, sora talgfettalkohol eller oleylalkohol, hvorav en del av disse har 10 til 16 glykoletergrupper og en annen del 3 til 7 glykoletergrupper. Mengdeforholdet mellom de to deler kan fortrinnsvis utgjøre 4:1 til 1:4. In a preferred embodiment, the spray-dried detergents mostly contain a nonionic surfactant, which differs from the compound according to formula I. These are the ethoxylated alcohols, vicinal diols and alkylphenols of the indicated formula with an average of 3 to 20 , preferably 5 to 15 glycol ether groups. Particularly suitable are mixtures of ethoxylated, primary C 1 -C 2 alcohols, such as tallow fatty alcohol or oleyl alcohol, part of which has 10 to 16 glycol ether groups and another part 3 to 7 glycol ether groups. The quantity ratio between the two parts can preferably amount to 4:1 to 1:4.
Når det på perboratet resp. byggersaltet påførte tensid med formel I med et innhold fra 1 til 4 propylenglykol-grupper ikke har mer enn 6-8 etylenglykoletergrupper, anvendes i forstøvningspulveret fortrinnsvis vannoppløselige høyere etoksylerte C, I 4 .-C.\ o«-alkoholer med 10 til 16 etylenglykoletergrupper. Vektforholdet mellom de på perboratet resp. byggersaltet påførte, lave etoksylerte tensider med formel I og de i forstøvningspulveret inneholdte høyere etoksylerte tensider, utgjør i disse tilfeller hensiktsmessig 3:1 til 1:4, fortrinnsvis 1:1 til 1:3. When the perborate or the building salt applied surfactant with formula I with a content of from 1 to 4 propylene glycol groups does not have more than 6-8 ethylene glycol ether groups, preferably water-soluble higher ethoxylated C, I 4 .-C.\ o«-alcohols with 10 to 16 ethylene glycol ether groups are used in the atomizing powder . The weight ratio between those on the perborate or low ethoxylated surfactants of formula I applied to the builder's salt and the higher ethoxylated surfactants contained in the atomizing powder, in these cases suitably amount to 3:1 to 1:4, preferably 1:1 to 1:3.
Ytterligere egnede ikke-ioniske tensider er slike som avledes fra de ovennevnte forbindelser og såvel har etylen-glykol- som også propylenglykoletergrupper, eksempelvis alkoholer med 10 til 30 etylenglykoletergrupper og 3 til 30 propylenglykoletergrupper; videre etoksyléringsprodukter av itier-kaptaner, fettsyreamider og fettsyrer. Anvendbare er også de vannoppløselige, 20 til 250 etylenglykoletergrupper'og 10 til 100 propylenglykbletergruppeholdige polyetylenoksyaddukter til polypropylenglykol, etylendiaminpolypropylenglykol og alkylpolypropyleriglykol og alkylpolypropylenglykol med 1 til 10 karbonatomer i alkylkjeden. Dé nevnte forbindelser inneholder vanligvis pr. propylenglykolenhet 1 til 5 etylenglykol-enheter. Også ikke-ioniske forbindelser av typen aminoksyder og sulfoksyder, som eventuelt også kan være etoksylert er anvendbare . Further suitable non-ionic surfactants are those which are derived from the above-mentioned compounds and have both ethylene glycol and propylene glycol ether groups, for example alcohols with 10 to 30 ethylene glycol ether groups and 3 to 30 propylene glycol ether groups; further ethoxylation products of itier-captans, fatty acid amides and fatty acids. The water-soluble polyethylene oxide adducts containing 20 to 250 ethylene glycol ether groups and 10 to 100 propylene glycol ether groups to polypropylene glycol, ethylene diamine polypropylene glycol and alkyl polypropylene glycol and alkyl polypropylene glycol with 1 to 10 carbon atoms in the alkyl chain are also applicable. The aforementioned compounds usually contain per propylene glycol unit 1 to 5 ethylene glycol units. Also non-ionic compounds of the type amine oxides and sulphoxides, which can optionally also be ethoxylated, can be used.
Egnede byggerstoffer er polymerfosfater, karbonater og silikater av kalium og spesielt av natrium, idet sistnevnte har et forhold Si02 til Na20 fra 1:1 til 3,5:1. Som polymer-fosf at kommer det spesielt på tale pentanatriumtrifosfat, som kan foreligge i blanding med dets hydrolyseprodukter, mono-og difosfater, samt høyerekondenserte fosfater, f.eks. tetra-fosfatene. Suitable building materials are polymer phosphates, carbonates and silicates of potassium and especially of sodium, the latter having a ratio of SiO 2 to Na 2 O from 1:1 to 3.5:1. As polymer-phosphate, pentasodium triphosphate is particularly mentioned, which can be present in a mixture with its hydrolysis products, mono- and diphosphates, as well as higher condensed phosphates, e.g. the tetra-phosphates.
Polymerfosfåtene kan også helt eller delvis være er-stattet med organiske, kompleksdannende virkende aminopolykarboksylsyrer. Hertil hører spesielt alkalisalter av nitri-lotrieddiksyre og etylendiaminotetraeddiksyre. Egnet er'videre saltene av dietylentriaminopentaeddiksyre samt de høyere' homologe av de nevnte aminopolykarboksylsyrer. Disse homologer The polymer phosphates can also be completely or partially replaced with organic, complex-forming aminopolycarboxylic acids. This includes, in particular, alkali salts of nitrilotriacetic acid and ethylenediaminotetraacetic acid. Also suitable are the salts of diethylenetriaminopentaacetic acid as well as the higher homologues of the aforementioned aminopolycarboxylic acids. These homologues
kan eksempelvis fremstilles ved polymerisasjon av en ester, can, for example, be produced by polymerization of an ester,
et amid eller nitril av N-eddiksyreaziridin og etterfølgende forsåpning til karboksylsyresalter eller ved omsetning av polyetylenimin med kloreddiksyre eller bromeddiksure salter i alkalisk miljø. Ytterligere egnede aminopolykarboksylsyrer er poly-(N-ravsyre)-etylenimin, poly-(N-trikarballylsyre)-etyl-enimin og poly-(N-butan-2,3,4-trikarboksylsyre)-etylenimin, som er oppnåelig analogt N-eddiksyrederivatene. an amide or nitrile of N-acetic acid aziridine and subsequent saponification to carboxylic acid salts or by reacting polyethyleneimine with chloroacetic acid or bromoacetic acid salts in an alkaline environment. Further suitable aminopolycarboxylic acids are poly-(N-succinic acid)-ethyleneimine, poly-(N-tricarballylic acid)-ethylenimine and poly-(N-butane-2,3,4-tricarboxylic acid)-ethyleneimine, which are obtainable analogously to N- the acetic acid derivatives.
Videre kan det være tilstede polyfosfonsure salter som virker kompleksdannende, f.eks. alkalisaltene av aminopolyfos-fonsyrer, spesielt aminotri-(metylenfosfonsyre, 1-hydroksy-etan-1,1-difosfonsyre, metylendifosfonsyre, etylendifosfonsyre samt salter av de høyere homologe av nevnte polyfosfonsyre. Også blandinger av de ovennevnte kompleksdannende midler er anvendbare. Furthermore, polyphosphonic acid salts may be present which have a complex-forming effect, e.g. the alkali salts of aminopolyphosphonic acids, in particular aminotri-(methylenephosphonic acid, 1-hydroxy-ethane-1,1-diphosphonic acid, methylenediphosphonic acid, ethylenediphosphonic acid and salts of the higher homologues of said polyphosphonic acid. Also mixtures of the above-mentioned complexing agents can be used.
Av spesiell betydning er de nitrogen- og fosforfrie, med kalsiumioner komplekssaltdannende polykarboksylsyrer, hvortil det også hører karboksylgruppeholdige polymerisater. Egnet er sitronsyre, vinsyre, benzenheksakarboksylsyre og tetrahydrofurantetrakarboksylsyre. Også polykarboksylsyrer inneholdende karboksymetyletergrupper er brukbare som 2,2'-oksydiravsyre, samt med glykolsyre delvis eller fullstendig foretrede flerverdige alkoholer eller hydroksykarboksylsyrer, eksempelvis triskarboksymetylglycerol, biskarboksymetyl-glycerolsyre og karboksymetylerte resp. oksyderte polysacca-rider. Videre egner det seg de polymere karboksylsyrer med en molekylvekt på minst 350 i form av vannoppløselige natrium-eller kaliumsalter, som polyakrylsyre, polymetakrylsyre, poly-a-hydroksyakrylsyre, polymaleinsyre, polyitakonsyre, polymesa-konsyre, polybutentrikarboksylsyre samt kopolymerisatene av de tilsvarende monomere karboksylsyrer med hverandre eller med etylenisk umettede forbindelser som etylen, propylen, iso-butylen, vinylmetyleter eller furan. Of particular importance are the nitrogen- and phosphorus-free polycarboxylic acids that form complex salts with calcium ions, which also include polymers containing carboxyl groups. Suitable are citric acid, tartaric acid, benzenehexacarboxylic acid and tetrahydrofurantetracarboxylic acid. Polycarboxylic acids containing carboxymethyl ether groups are also usable as 2,2'-oxysuccinic acid, as well as partially or completely etherified polyhydric alcohols or hydroxycarboxylic acids with glycolic acid, for example tricarboxymethylglycerol, biscarboxymethylglycerol acid and carboxymethylated resp. oxidized polysacca rides. Also suitable are the polymeric carboxylic acids with a molecular weight of at least 350 in the form of water-soluble sodium or potassium salts, such as polyacrylic acid, polymethacrylic acid, poly-α-hydroxyacrylic acid, polymaleic acid, polyitaconic acid, polymesaconic acid, polybutene tricarboxylic acid as well as the copolymers of the corresponding monomeric carboxylic acids with each other or with ethylenically unsaturated compounds such as ethylene, propylene, iso-butylene, vinyl methyl ether or furan.
Også i vann uoppløselige kompleksdannende forbindelser kan anvendes. Hertil hører fosforylert cellulose og podnings-polymere av akrylsyre eller metakrylsyre på cellulose, som kan foreligge som vevnad, fiberflor eller som pulver. Videre er det egnet romlige nettdannere og derved vannuoppløselige kopolymere av akryl-, métakryl-, kroton- og maleinsyre samt andre polymeriserbare polykarboksylsyrer, eventuelt med ytterligere etylenisk umettede forbindelser i form av natrium-eller kaliumsaltene som sequestreringsmiddel. Disse uoppløse-lige kopolymere kan foreligge som flor, svamp eller også i form av finmalt, spesifikt lette skum med åpencellet struktur. Anvendbare er videre uorganiske vannuoppløselige kationut-vekslere, f.eks. zeolitter og spesielt vannhoIdige aluminium-silikater av formel (Na_0) - A1_G0 . (SiO„) . (H_0) med x Water-insoluble complexing compounds can also be used. This includes phosphorylated cellulose and graft polymers of acrylic acid or methacrylic acid on cellulose, which can be available as woven fabric, fiber pile or as powder. Furthermore, there are suitable spatial network formers and thereby water-insoluble copolymers of acrylic, methacrylic, crotonic and maleic acids as well as other polymerizable polycarboxylic acids, possibly with further ethylenically unsaturated compounds in the form of the sodium or potassium salts as a sequestering agent. These insoluble copolymers can be available as fluff, sponge or also in the form of finely ground, specifically light foam with an open-cell structure. Also usable are inorganic water-insoluble cation exchangers, e.g. zeolites and especially hydrous aluminum silicates of formula (Na_0) - A1_G0. (SiO 2 ) . (H_0) with x
z x 2 3 2. y 2z z x 2 3 2. y 2z
= 0,9 - 13, y = 1,3 - 4,0 og z = 1 til 6. = 0.9 - 13, y = 1.3 - 4.0 and z = 1 to 6.
Som ytterligere bestanddeler kommer det i betraktning nøytralsalter, spesielt natriumsulfat, samt magnesiumsilikat, virkende som stabilisator for perforbindelser. <y>tterligere vaskehjelpemidler som kan være tilstede som forstøvnings-tørkede pulverkomponenter, er grådannelsesinhibitorer og optiske lysgjørere og tilsetninger som forbedrer pulverstrukturen, f.eks. alkalisalter av toluen-, kumol- eller xylensulfonsyrer. As additional components, neutral salts, especially sodium sulfate, as well as magnesium silicate, acting as a stabilizer for per compounds, come into consideration. Additional washing aids that may be present as spray-dried powder components are graying inhibitors and optical brighteners and additives that improve powder structure, e.g. alkali salts of toluene, cumolic or xylene sulfonic acids.
Som grådannelsesinhibitorer egner det seg spesielt karboksymetylcellulose, metylcellulose, videre vannoppløselige polyestere og polyamider av flerverdige karboksylsyrer og glykoler resp. diaminer, som har frie, til saltdannelse egnede karboksylgrupper, betaingrupper eller sulfobetaingrupper samt kolloidalt i vann oppløselige polymere resp. kopolymere av vinylalkohol, vinylpyrrolidon, akrylamid og akrylnitril. As graying inhibitors, carboxymethylcellulose, methylcellulose, further water-soluble polyesters and polyamides of polyvalent carboxylic acids and glycols are particularly suitable. diamines, which have free carboxyl groups suitable for salt formation, betaine groups or sulfobetaine groups as well as colloidally water-soluble polymers or copolymers of vinyl alcohol, vinyl pyrrolidone, acrylamide and acrylonitrile.
Egnede optiske lysgjørere er alkalisaltene av 4,4-bis-(2"-anilino-4"-morfolino-1,3,5-triazinyl-6"-amino)-stilben-2,2<1->disulfonsyre eller likeartet oppbygget forbindelse, som istedenfor morfolinogruppen har-en dietanolamingruppe, en metylaminogruppe eller en 3-metoksyetylaminogruppe. Videre kommer det som lysgjører for polyamidfibre på tale slike av typen diarylpyrazoliner, eksempelvis 1-(-p-sulfonamidoferiyl)-3-(p-klorfenyl)-A<2> -pyrazolin, samt likeartede oppbyggede forbindelser, som istedenfor sulfonamidgruppen har en karboksy-metyl- eller acetylaminogruppe. Brukbar er videre substituerte aminocumariner, f.eks. 4-metyl-7-dimetylamino- eller 4-metyl-7-dietylaminocumarin. Videre er det som polyamidlysgjørere anvendbare forbindelsene 1-{2-benzimidazolyl)-2-(1-hydroksy-etyl-2-benzimidazolyl)-etylen og 1-etyl-3-fenyl-7-dietylamino-karbostyryl. Som lysgjører for polyester- og polyamidfibre er det egnet forbindelsene 2,5-di-(2-benzoksazolyl)-tiofen, 2-(2-benzoksazolyl)-nafto-/2,3-b/-tiofen og 1,2-di-(5-metyl-2-benzoksazolyl)-etylen. Videre kan det være tilstede lysgjører av typen av de substituerte difenylstyriler. Også blandinger av de ovennevnte lysgjørere kan anvendes. Suitable optical brighteners are the alkali salts of 4,4-bis-(2"-anilino-4"-morpholino-1,3,5-triazinyl-6"-amino)-stilbene-2,2<1->disulfonic acid or similarly structured compound, which instead of the morpholino group has a diethanolamine group, a methylamino group or a 3-methoxyethylamino group. Furthermore, brighteners for polyamide fibers include those of the diarylpyrazoline type, for example 1-(-p-sulfonamidoferriyl)-3-(p-chlorophenyl)- A<2>-pyrazoline, as well as similarly structured compounds, which instead of the sulfonamide group have a carboxy-methyl or acetylamino group. Substituted aminocoumarins can also be used, e.g. 4-methyl-7-dimethylamino- or 4-methyl-7-diethylaminocoumarin Furthermore, the compounds 1-{2-benzimidazolyl)-2-(1-hydroxy-ethyl-2-benzimidazolyl)-ethylene and 1-ethyl-3-phenyl-7-diethylamino-carbostyryl are useful as polyamide brighteners. As brighteners for polyester - and polyamide fibers, the compounds 2,5-di-(2-benzoxazolyl)-thiophene, 2-(2-benzoxazolyl)-naphtho-/2,3-b/-thiophene are suitable one and 1,2-di-(5-methyl-2-benzoxazolyl)-ethylene. Brighteners of the substituted diphenylstyryl type may also be present. Mixtures of the above brighteners can also be used.
Foruten de to pulverkomponentene kan det også være tilstede ytterligere pulverbestanddeler, som ikke egner seg for en felles forarbeidelse med perborat og ikke for en varm-forstøvningstørkning. Hertil hører blekeaktivatorer, spesielt tetraacetylglykoluril eller tetraacetyletylendiamin. De av blekeaktivator bestående pulverpartikler kan være overtrukket med belegningsmaterialer, spesielt blandinger av vannoppløse-lige <p>olymere og fettsyrer eller fettalkoholer, for å unngå In addition to the two powder components, further powder components may also be present, which are not suitable for joint processing with perborate and not for hot spray drying. This includes bleaching activators, especially tetraacetyl glycoluril or tetraacetylethylenediamine. The powder particles consisting of bleach activator can be coated with coating materials, in particular mixtures of water-soluble polymers and fatty acids or fatty alcohols, to avoid
en vekselvirkning mellom perforbindelsen.og aktivatoren under lagring. Ytterligere tilsetninger som tilsettes adskilt til . pulveret er enzymer fra klassen proteaser, lipaser og amylaser, resp. deres blandinger. Spesielt egnet er enzymatisk virksomme stoffer fremstilt fra bakteriestammer eller sopp som bacillus subtilis, bacillus licheniformis og streptomyces griseus. Enzymene kan være innleiret i belegningsmaterialer eller på-granulert etterpå på de forstøvningstørkede pulverkomponenter. Også luktstoffer og bestemte fettaktige skumdempningsmidler, som trialkylmelaminer eller parafinhydrokarboner, påsprøytes fortrinnsvis etterpå på det forstøvningstørkede pulver. an interaction between the per-compound and the activator during storage. Additional additives that are added separately to . the powder is enzymes from the class of proteases, lipases and amylases, resp. their mixtures. Particularly suitable are enzymatically active substances produced from bacterial strains or fungi such as bacillus subtilis, bacillus licheniformis and streptomyces griseus. The enzymes can be embedded in coating materials or subsequently granulated onto the spray-dried powder components. Odors and certain fatty defoamers, such as trialkylmelamines or paraffin hydrocarbons, are also preferably sprayed afterwards onto the spray-dried powder.
Det er å anse som spesielt fordelaktig ved fremgangsmåten ifølge oppfinnelsen, at det med forholdsvis lite energi-og tidsforbruk oppnås et godt blanderesultat. De ve fremgangsmåten ifølge oppfinnelsen fremstilte granulater er fri for støvdeler og klumper, homogene og godt risledyktige, idet disse fordelaktige egenskaper også oppnås når det anvendte grunn<p>ulver på grunn av tilsvarende lagringsbetingelser har tem<p>eraturer på mindre enn 10°C. I motsetning til slike granulater, som fremstilles under anvendelse av lavere smeltende kokosfettalkoholetoksylater av liten etoksyleringsgrad, utmerker de foreliggende granulater seg i vesentlig grad av luktfrihet, hvilket forbrukeren setter pris på. Dessuten har de ikke-toksiske tensider som anvendes ifølge oppfinnelsen sammenlignet med lavetoksylerte kokosfettalkoholer betraktelig mindre tendens til dannelse av uønsket skum, hvorfor fremgangsmåteproduktet med fordel kan anvendes i automatiske vaske- og oppvaskmaskiner. Ved anvendelsen utmerker de seg ved en høy rense- og fettoppløsningsevne. It is considered particularly advantageous with the method according to the invention that a good mixing result is achieved with relatively little energy and time consumption. The granulates produced by the method according to the invention are free of dust particles and lumps, homogeneous and well-flowable, as these advantageous properties are also achieved when the base material used, due to corresponding storage conditions, has temperatures of less than 10°C . In contrast to such granules, which are produced using lower-melting coconut fat alcohol ethoxylates of a low degree of ethoxylation, the present granules are distinguished to a significant degree by being odorless, which the consumer appreciates. In addition, the non-toxic surfactants used according to the invention, compared to low-toxylated coconut fatty alcohols, have considerably less tendency to form unwanted foam, which is why the process product can be advantageously used in automatic washing and dishwashing machines. When used, they are distinguished by a high cleaning and fat-dissolving ability.
Eksemp_el_1_ Example_el_1_
Siktanalyse av natriumperborattetrahydratet som skal behandles skal ha følgende fordeling: Sieve analysis of the sodium perborate tetrahydrate to be treated must have the following distribution:
90 kg av perboratet ble fylt i en trommeIblander med hurtigomløpende blandeorgan (såkalt LODIGE-blandinger). Temperaturen i det fra en silo uttatte perborat utgjorde 10°C. I den sirkulerende blanding ble det fylt 10 kg av et i første rekke med 1,2 mol propylenoksyd og deretter med 6,3 mol etylenoksyd omsatt talgfettalkohol. Temperaturen av det smeltede ikke-ioniske tensid utgjorde 60°C. Etter 2,5 minutter var blandeprosessen avsluttet og det dannede granulat ble undersøkt på homogenitet, støvfrihet og risleevne. På samme måte ble det for sammenligning fremstilt blandinger under anvendelse av andre vanlige ikke-ioniske tensider. Resultatene befinner seg i tabell I. Forkortelsene EO og PrO betyr etylenoksyd og propylenoksyd, S betyr sammenligningsforsøk, Sp betyr stivnepunkt. 90 kg of the perborate was filled into a drum mixer with a fast-circulating mixing device (so-called LODIGE mixtures). The temperature in the perborate removed from a silo was 10°C. In the circulating mixture, 10 kg of a tallow fatty alcohol reacted firstly with 1.2 mol of propylene oxide and then with 6.3 mol of ethylene oxide were filled. The temperature of the molten nonionic surfactant was 60°C. After 2.5 minutes, the mixing process was finished and the formed granules were examined for homogeneity, freedom from dust and flowability. Similarly, for comparison, mixtures were prepared using other common nonionic surfactants. The results are in Table I. The abbreviations EO and PrO mean ethylene oxide and propylene oxide, S means comparative test, Sp means solidification point.
Undersøkelse på støvdannelse ble gjennomført som følger. På en ren skumgummimatte (dimensjoner 50 x 50 cm, tykkelse ca. 1 cm) utbres en rund polyetylenfolie (diameter 45 cm). I midten av folien stilles et sylindrisk oppfangningskar av 18 cm diameter og 10 cm høyde. Derover settes en på den ene side lukket blikksylinder av 40 cm diameter og 70 cm høyde, således med åpningen nedad at avstanden mellom sylin-derveggen og oppfangningskarets kant overalt er lik. Denne sylinder har i midten av den lukkede side et rundt hull av ca. 3,5 cm diameter, hvori det innføres en trakt med et 19 cm langt rør av 2,5 cm indre vidde. Over en rysterenne lar man 100 g produkt som skal undersøkes risle i trakten resp. sylinderen. Derved faller produktet i det oppfangningskar som står ved bunnen på folien. Støvdelen av produktet løser seg imidlertid ved det frie fall fra produktstrømmen og opphvirv-les i luften innen den store sylinder. Etter at 100 g produkt er blitt innført venter man i 1 minutt. I løpet av denne tid avsetter støvet seg på folien ved bunnen. Man fjerner da for-siktig sylinderen og oppfangningskaret og folder folien om-hyggelig sammen og bestemmer mengden av det støv som er av-leiret ved meining. Etter denne metode finnes det sideveis avleirede, dvs. den ikke i produktet gjenblivende støvdel. Det tilsvarer således omtrent støvtapet. Examination of dust formation was carried out as follows. A round polyethylene foil (diameter 45 cm) is spread on a clean foam rubber mat (dimensions 50 x 50 cm, thickness approx. 1 cm). A cylindrical collection vessel of 18 cm diameter and 10 cm height is placed in the middle of the foil. Above that, a tin cylinder of 40 cm diameter and 70 cm height, closed on one side, is placed, with the opening downwards, so that the distance between the cylinder wall and the edge of the collection vessel is the same everywhere. This cylinder has a round hole of approx. 3.5 cm diameter, into which a funnel with a 19 cm long tube of 2.5 cm internal width is inserted. Over a shaking trough, 100 g of the product to be examined is allowed to trickle into the funnel or the cylinder. As a result, the product falls into the catch basin at the bottom of the foil. However, the dust part of the product dissolves during the free fall from the product stream and is stirred up in the air within the large cylinder. After 100 g of product has been introduced, wait for 1 minute. During this time, the dust settles on the foil at the bottom. You then carefully remove the cylinder and the collection vessel and carefully fold the foil together and determine the amount of the dust that has been deposited by measuring. According to this method, there is laterally deposited, i.e. the dust part that does not remain in the product. It thus roughly corresponds to the dust loss.
Videré ble det ved enkelte fremgangsmåteprodukter gjennomført siktanalyser. Resultatene gjengis i tabell II. In addition, sieve analyzes were carried out for some process products. The results are reproduced in table II.
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Resultatene viser at produktene fremstilt ifølge oppfinnelsen har et snevert og dermed gunstig kornspektrum og er fri for grov-,og findeler samt støvformede partikler. The results show that the products manufactured according to the invention have a narrow and thus favorable grain spectrum and are free of coarse and fine parts as well as dust-shaped particles.
Granulatet ble i en frittfall-blander forenet med et ved varmforstøvningstørkning fremstilt hulkulepulver til vaskemidler av følgende sammensetning (angivelser i vekt-%): The granulate was combined in a free-fall mixer with a hollow ball powder produced by hot spray drying for detergents of the following composition (indications in % by weight):
8,5 Na-n-dodecylbenzensulfonat 8.5 Na-n-dodecylbenzenesulfonate
3,5 talgfettalkohol + 14 EO 3.5 tallow fatty alcohol + 14 EO
3,5 Såpe (Na-talgsåpe/Na-behenat 1:1) 3.5 Soap (Na-tallow soap/Na-behenate 1:1)
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40,0 Pentanatriumtripolyfosfat 5,0 Natriumsilikat (Na20 : Si02 = 1:3) 40.0 Pentasodium tripolyphosphate 5.0 Sodium silicate (Na20 : SiO2 = 1:3)
3,0 Magnesiumsilikat 3.0 Magnesium silicate
0,2 Na-etylendiamintetraacetat 1,5 Na-karb6ksynetylcellulose 0,5 optisk lysgjører 0.2 Na-ethylenediaminetetraacetate 1.5 Na-carboxyethyl cellulose 0.5 optical brightener
0,1 Luktstoffer 0.1 Odors
6,5 Natriumsulfat 6.5 Sodium sulfate
7,7 Vann 7.7 Water
20,0 Blanding ifølge eksempel 1 20.0 Mixture according to example 1
Vaskemiddelprøver ble fylt i flatesker som tar 200 g og i 2 timer underkastet en rysteprøve. En separering av vaskemiddel- og perboratkorn opptrådde derved ikke. Detergent samples were filled in flat boxes that hold 200 g and for 2 hours subjected to a shaking test. A separation of detergent and perborate grains thereby did not occur.
Eksemp_el_2 Example_el_2
Som angitt i eksempel 1 ble 450 kg natriumtripolyfos-fat blandet i LODIGE-blander med 50 kg av et ikke-ionisk tensid, fremstilt ved omsetning av en kokos-talgfettalkoholblan-ding (kjedelengde c-\ 2~ C-\ 8' m;i-dlere kjedelengde 5) med 1,5 mol propylenoksyd og 5 mol etylenoksyd. Blandeprosessen var avsluttet etter 2,5 minutter. Forblandingen ble ved hjelp av en luftstrøm innblåst i et forstøvningstårn. Tilførsels-stussene for den innblåste forblanding førte fra forstøvnings-tårnets topp til i høyde av de ringformet anordnede oppslem-nings-forstøvningsdyser. Den i motstrøm førte tørrluft har en inngangstemperatur på 2 70°C og en uttredelsestemperatur på 92°C. Under forstøvningsprosessen opptrådte ingen røkdannelse resp. intet tap av ikke-ionisk vaskeaktivt stoff. As indicated in example 1, 450 kg of sodium tripolyphos was mixed in LODIGE mixers with 50 kg of a non-ionic surfactant, prepared by reaction of a coconut-tallow fatty alcohol mixture (chain length c-\ 2~ C-\ 8' m; longer chain length 5) with 1.5 mol propylene oxide and 5 mol ethylene oxide. The mixing process was finished after 2.5 minutes. The premix was blown into an atomization tower by means of an air stream. The supply nozzles for the blown-in premix led from the top of the atomization tower to the height of the annularly arranged slurry atomization nozzles. The countercurrent dry air has an inlet temperature of 270°C and an outlet temperature of 92°C. During the atomization process, no smoke formation or no loss of non-ionic detergent.
Produksjonen hver gang ble styrt således at det for-støvningstørkede produkt har følgende sammensetning ( i vekt-<%>) The production each time was controlled so that the spray-dried product has the following composition (in weight <%>)
2,5% Fettalkoholblanding +1,5 PrO + 5 EO 22,5% Na-tripolyfosfat fra forblanding 7,5% Na-tripolyfosfat fra oppslemming 2,7% Talgfettalkohol + 14 EO 2.5% Fatty alcohol mixture +1.5 PrO + 5 EO 22.5% Na-tripolyphosphate from premix 7.5% Na-tripolyphosphate from slurry 2.7% Tallow fatty alcohol + 14 EO
7,8% Na-alkylbenzensulfonat 4,0% Na-såpe (talgfettsyre-behensyre 3:1) 1,8% Na-karboksymetylcellulose 22,0% Natriumaluminiumsilikat 2,5% Magnesiumsilikat 7.8% Na-alkylbenzenesulfonate 4.0% Na-soap (tallow fatty acid-behenic acid 3:1) 1.8% Na-carboxymethyl cellulose 22.0% Sodium aluminum silicate 2.5% Magnesium silicate
4,0% Na-silikat (Na20 : Si02 = 1:3,3) 4.0% Na silicate (Na20 : SiO2 = 1:3.3)
0,2% EDTA 0.2% EDTA
0,3% Optisk lysgjører 0.3% Optical brightener
13,5% Natriumsulfat 13.5% Sodium sulfate
Resten Vann The rest Water
Det forstøvningstørkede produkt var homogent og har en litervekt på 450 g. Sikttallene er: The spray-dried product was homogeneous and has a liter weight of 450 g. The sieve figures are:
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Pulveret var godt risledyktig og fri for ubehagelig lukt. Etter sammenblanding av 75 vektdeler av forstøvnings-pulveret med 2 4,8 vekt<*->% natriumperborat og 0,2 vektdeler luktstoff var pulveret anvendbart som svaktskummende, maskin-egnet vaskemiddel for 60° vasking, resp. kokevasking. The powder was well flowable and free of unpleasant odours. After mixing 75 parts by weight of the atomizing powder with 2 4.8 weight<*->% sodium perborate and 0.2 parts by weight of fragrance, the powder was usable as a low-foaming, machine-suitable detergent for 60° washing, resp. kitchen washing.
Claims (5)
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NO800437A NO150487C (en) | 1980-02-18 | 1980-02-18 | PROCEDURE FOR THE PREPARATION OF A CRYSTIC DETECTIVE DETERGENT AND CLEANING GRANULATE CONTAINING NON-IONIC TENSID |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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NO800437A NO150487C (en) | 1980-02-18 | 1980-02-18 | PROCEDURE FOR THE PREPARATION OF A CRYSTIC DETECTIVE DETERGENT AND CLEANING GRANULATE CONTAINING NON-IONIC TENSID |
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Publication Number | Publication Date |
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NO800437L NO800437L (en) | 1981-08-19 |
NO150487B true NO150487B (en) | 1984-07-16 |
NO150487C NO150487C (en) | 1984-10-31 |
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NO800437A NO150487C (en) | 1980-02-18 | 1980-02-18 | PROCEDURE FOR THE PREPARATION OF A CRYSTIC DETECTIVE DETERGENT AND CLEANING GRANULATE CONTAINING NON-IONIC TENSID |
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1980
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NO800437L (en) | 1981-08-19 |
NO150487C (en) | 1984-10-31 |
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