NO782864L - PROCEDURES FOR AA IMPROVING THE PRODUCTS OF SODIUM ALUMINUM SILICATE DOUGHS AND POWDER - Google Patents
PROCEDURES FOR AA IMPROVING THE PRODUCTS OF SODIUM ALUMINUM SILICATE DOUGHS AND POWDERInfo
- Publication number
- NO782864L NO782864L NO782864A NO782864A NO782864L NO 782864 L NO782864 L NO 782864L NO 782864 A NO782864 A NO 782864A NO 782864 A NO782864 A NO 782864A NO 782864 L NO782864 L NO 782864L
- Authority
- NO
- Norway
- Prior art keywords
- dough
- aluminum silicate
- sodium
- sodium aluminum
- improving
- Prior art date
Links
- DNEHKUCSURWDGO-UHFFFAOYSA-N aluminum sodium Chemical compound [Na].[Al] DNEHKUCSURWDGO-UHFFFAOYSA-N 0.000 title claims description 16
- 238000000034 method Methods 0.000 title claims description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 41
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 25
- 235000011152 sodium sulphate Nutrition 0.000 claims description 25
- 239000007787 solid Substances 0.000 claims description 14
- 229910001868 water Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000725 suspension Substances 0.000 description 9
- 238000009826 distribution Methods 0.000 description 7
- 239000004115 Sodium Silicate Substances 0.000 description 4
- 239000003599 detergent Substances 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 229910052911 sodium silicate Inorganic materials 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000007832 Na2SO4 Substances 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- -1 aluminum silicates Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 235000012216 bentonite Nutrition 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 230000009969 flowable effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 206010067482 No adverse event Diseases 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004094 surface-active agent 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/026—After-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Detergent Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Description
Fremgangsmåte for å forbedre egenskapene- til deigerProcess for improving the properties of dough
og pulvere av natriumaluminiumsilikatand sodium aluminum silicate powders
Fremstilling av aluminiumsilikater av zeolittypen, bl.a. også av typen A, ved omsetning av en vandig alkalisilikatopp-løsning med en alkaiialuminatoppløsning har vært kjent i flere o Production of aluminum silicates of the zeolite type, i.a. also of type A, by reacting an aqueous alkali silicate solution with an alkali aluminate solution has been known for several years
ar. year.
I nyere tid er ytterligere anvendelsesområder kommet til for zeolitten A, som f.eks. bygger i vaskemidler. Denne nye anvendelse stiller ytterligere krav hva gjelder produktets egenskaper. Således ønskes foruten en god evne til å binde jord-alkalier f.eks. en høy hvithet og en lav midlere partikkeldiameter med en samtidig snever partikkelstørrelsesfordeling. Det er i den forbindelse et viktig krav at produktet, uavhengig i hvilken form det foreligger, igjen skal oppvise den opprinnelige fordel-ing når det er blitt dispergert i vann, dvs. at det ikke skal oppvise en irreversibel agglomerering. In recent times, further areas of application have come to light for the zeolite A, such as e.g. builds in detergents. This new application places further demands on the product's properties. Thus, in addition to a good ability to bind soil alkalis, e.g. a high whiteness and a low mean particle diameter with a simultaneous narrow particle size distribution. In this connection, it is an important requirement that the product, regardless of the form in which it is present, should again show the original distribution when it has been dispersed in water, i.e. that it should not show an irreversible agglomeration.
Det forventes dessuten av natriumaluminiumsilikatet at dette i form av en filterdeig som kan anvendes som sådan ved fremstillingen av vaskemidler, skal ha bestemte egenskaper som er nærmere beskrevet nedenfor. It is also expected of the sodium aluminum silicate that, in the form of a filter dough that can be used as such in the production of detergents, it should have certain properties which are described in more detail below.
Filterdeigen som fås ved fremstillingen av natriumaluminiumsilikatet efter at moderluten er blitt fraskilt og efter vasking og som vanligvis inneholder 40-50% faststoff, oppviser foruten andre rheologiske unormalheter en sterk strukturviskositet. Dette muliggjør i alminnelighet at deigen ved den videre arbeidsprosess kan transporteres ved pumping uten å fortynnes. Dessuten kan deigen på grunn av de nevnte rheologiske egenskaper i alminnelighet lagres i egnede beholdere og fra disse igjen gjøres flytende under anvendelse av forholdsvis liten energi ved røring, rysting eller pumping etc. The filter dough which is obtained during the production of the sodium aluminum silicate after the mother liquor has been separated and after washing and which usually contains 40-50% solids, exhibits, in addition to other rheological abnormalities, a strong structural viscosity. This generally enables the dough to be transported during the further work process by pumping without being diluted. In addition, due to the aforementioned rheological properties, the dough can generally be stored in suitable containers and from these again liquefied using relatively little energy by stirring, shaking or pumping etc.
Uttrykket "i alminnelighet" er ment å betegne at de beskrevne flyteegenskaper foreligger i det overveiende antall av tilfeller. For pumpbarheten av deigen efter at denne er blitt lagret, gjelder "dette spesielt for et tidsrom av opp til 48 The expression "in general" is intended to denote that the described flow properties are present in the predominant number of cases. For the pumpability of the dough after it has been stored, "this applies in particular for a period of up to 48
timers lagring. Ved lengre lagring dannes imidlertid en seigere bunnmasse gradvis som hverken kan pumpes eller omrøres. hours of storage. With longer storage, however, a tougher bottom mass is gradually formed which can neither be pumped nor stirred.
Det er derfor blitt foreslått i tysk tilgjengeliggjort patentsøknad nr. 2527388 å tilsette et dispergeringsmiddel til natriumaluminiumsilikatsuspensjonene for å forbedre suspensjonenes stabilitet og pumpbarhet, idet disse dispergeringsmidler hoved-sakelig utgjøres av organiske, overflateaktive stoffer eller svellbare leirer, som bl.a. bentonitter. Som forsøkene i den ovenfor angitte tilgjengeliggjorte tyske patentsøknad viser, kan suspensjoner som er blitt stabilisert med organiske, overflateaktive stoffer, fremdeles pumpes efter 24 timer og er vidtgående homogene. Egne forsøk har imidlertid vist at det allerede efter to dager dannes en bunnavsetning og at suspensjonen ikke lenger kan pumpes efter tre dager.. Det nevnes intet i den tilgjengeliggjorte tyske patentsøknad angående stabiliteten for suspensjoner hvortil bentonitter er blitt tilsatt. Oppbearbeidede leirer er dessuten beheftet medflen ulempe at de må befris meget omhyggelig for jern og at de forstyrrer vaskeprosessen ved at de ikke fjernes fullstendig under skyllingen, slik at det dannes avsetninger på fibrene inntil det tii slutt forekommer en skorpedannelse. It has therefore been proposed in German patent application no. 2527388 to add a dispersant to the sodium aluminum silicate suspensions in order to improve the stability and pumpability of the suspensions, these dispersants mainly consisting of organic, surface-active substances or swellable clays, which e.g. bentonites. As the experiments in the German patent application made available above show, suspensions that have been stabilized with organic surfactants can still be pumped after 24 hours and are largely homogeneous. However, my own experiments have shown that a bottom deposit already forms after two days and that the suspension can no longer be pumped after three days. Nothing is mentioned in the German patent application made available regarding the stability of suspensions to which bentonites have been added. Processed clays are also burdened with the disadvantage that they must be very carefully freed of iron and that they disrupt the washing process by not being completely removed during the rinse, so that deposits form on the fibers until eventually a crust forms.
Det har nu vist seg at når natriumsulfat er tilstede i deigen, unngås de beskrevne vanskeligheter ved den videre bearbeidelse av deigen. Tilsetningen av natriumsulfat byr ikke bare på den fordel at det derved fås en rimeligere bestanddel i natrium-aluminiumsilikatsuspensjonen og som likevel er tilstede i vaske-midlet, men denne bestanddel bevirker dessuten at når det tørkede produkt dispergeres i vann, vil natriumsilikatet igjen foreligge med sin opprinnelige kornfordeling. It has now been shown that when sodium sulphate is present in the dough, the described difficulties are avoided in the further processing of the dough. The addition of sodium sulphate not only offers the advantage that a more affordable component is obtained in the sodium aluminum silicate suspension and which is nevertheless present in the detergent, but this component also means that when the dried product is dispersed in water, the sodium silicate will again be present with its original grain distribution.
Som en gunstig utførelsesform av den videre bearbeidelseAs a favorable embodiment of the further processing
av natriumsilikatdeigen anvendes vanligvis forstøvningstørking. Ved siden av vesentlige fordeler sammenlignet med andre tørke-metoder er forstøvningstørkingen beheftet med en ulempe, dvs. at produktet fås i form av priller. Denne i og for segønskede egen-skap fører imidlertid til at den .kornfordeling som opprinnelig forelå i deigen, ikke igjen vil fås med tilstrekkelig sikkerhet ved dispergering i vann. Prillene (midlere diameter 30-80 um) of the sodium silicate dough, spray drying is usually used. In addition to significant advantages compared to other drying methods, spray drying has a disadvantage, i.e. that the product is obtained in the form of pellets. However, this intrinsically desirable property means that the grain distribution that was originally present in the dough will not be obtained again with sufficient certainty when dispersed in water. Prills (average diameter 30-80 um)
brytes hyppig ikke fullstendig ned til de opprinnelige primær-partikler med en finhet av 98 - 99% ^ 15 p svarende til 9 5% ^ 10 ja. Denne ulempe unngås ved tilsetningen av natriumsulfat. is often not completely broken down to the original primary particles with a fineness of 98 - 99% ^ 15 p corresponding to 9 5% ^ 10 ja. This disadvantage is avoided by the addition of sodium sulphate.
Det kunne ikke forventes at natriumsulfat ville gi en slik gunstig virkning for natriumsilkatsuspensjonens egenskaper. Det kan fra den tyske tilgjengeliggjorte patentsøknad nr. 2527388 ut-ledes at natriumsulfat ikke vil ha noen stabiliserende virkning på suspensjonen. Det vises riktignok til at natriumhydroxyd som fremdeles foreligger i den vaskede filterdeig, kan nøytraliseres med svovelsyre, men i tillegg måtte den nødvendige mengde av dispergeringsmidlet imidlertid tilsettes til suspensjonen for å oppnå den ønskede stabilitet. Det anbefales i den forbindelse å utføre nøytraliseringen av natronluten i det minste delvis med et dispergeringsmiddel av sur type for derved å erstatte ikke-stabiliserende syrer, som svovelsyre. It could not be expected that sodium sulphate would have such a beneficial effect on the properties of the sodium silicate suspension. It can be deduced from the German patent application no. 2527388 that sodium sulphate will not have any stabilizing effect on the suspension. It is true that sodium hydroxide which is still present in the washed filter dough can be neutralized with sulfuric acid, but in addition the required amount of dispersant had to be added to the suspension in order to achieve the desired stability. In this connection, it is recommended to carry out the neutralization of the caustic soda at least partially with an acid-type dispersant to thereby replace non-stabilizing acids, such as sulfuric acid.
Ved tilsetning av natriumsulfat beholdt filterdeigen sin fordelaktige konsistens i og eventuelt utover en samlet iakttagelses-tid av 8 uker. Det skal spesielt nevnes at ingen seig, ikke pump-bar og ikke omrøringsbar bunnmasse ble dannet. Allerede ved en tilsetning av 1% Na2S04, basert på den faststoffdeig som forelå efter tilsetningen, kunne en virkning iakttas. I praksis er en tilsetning av 2% natriumsulfat den nedre grense. Med økende Na2SO^-konsentrasjon stiger først virkningen av natriumsulfatet, slik at en tilsetning av 2-10% er gunstig for å forbedre de rheologiske egenskaper. Ved en økning av tilsetningen til over 10% og oppad til 25%, basert på den samlede faststoffmengde, kunne ingen uhel-dige virkninger for de rheologiske egenskaper fastslås. When sodium sulphate was added, the filter dough retained its advantageous consistency during and possibly beyond a total observation period of 8 weeks. It should be mentioned in particular that no tough, non-pumpable and non-stirrable bottom mass was formed. Already with the addition of 1% Na2S04, based on the solid dough that was present after the addition, an effect could be observed. In practice, an addition of 2% sodium sulphate is the lower limit. With increasing Na2SO^ concentration, the effect of the sodium sulphate first increases, so that an addition of 2-10% is beneficial for improving the rheological properties. By increasing the addition to over 10% and up to 25%, based on the total amount of solids, no adverse effects on the rheological properties could be determined.
For å forbedre det tørkede natriumaluminiumsilikats dispergerbarhet er en tilsetning av over 10%, fortrinnsvis 15-20%, basert på den samlede faststoffmengde, nødvendig. Dersom en filterdeig med Na2SO^-innhold av over 10% og opp til ca. 25%, basert på faststoffmengden, forstøvningstørkes, viser de fremstilte tørkede produkter ved bestemmelse av kornstørrelsen en vidtgående lignende kornstørrelsesfordeling som den opprinnelige efter dispergering i vann. To improve the dispersibility of the dried sodium aluminum silicate, an addition of over 10%, preferably 15-20%, based on the total solids amount, is necessary. If a filter dough with a Na2SO^ content of over 10% and up to approx. 25%, based on the amount of solids, is spray-dried, the dried products produced show, when determining the grain size, a broadly similar grain size distribution to the original after dispersion in water.
Natriumsulfatet kan tilsettes på ethvert trinn av frem-gangsmåten ved fremstillingen av natriumaluminiumsilikater, så- lenge natriumaluminiumsilikatet som sådant ikke forandres struktur-messig på grunn av tilsetningsformen. Det må dessuten selvfølgelig påses at natriumsulfatet ikke fjernes under den påfølgende vaske-prosess. Det er således likegyldig om f.eks. natriumsulfatet allerede er tilstede ved en utfelling av natriumaluminiumsilikatet, dvs. om natriumsulfatet tilsettes til alkalisilikat- og/eller alkalialuminatoppløsningen, eller om det tilføres under den på-følgende temperaturfase. Det kan også tilsettes til den vaskede filterdeig. The sodium sulfate can be added at any stage of the process in the production of sodium aluminum silicates, as long as the sodium aluminum silicate as such is not structurally altered due to the form of addition. It must of course also be ensured that the sodium sulphate is not removed during the subsequent washing process. It is thus indifferent if, for example, the sodium sulfate is already present when the sodium aluminum silicate is precipitated, i.e. if the sodium sulfate is added to the alkali silicate and/or alkali aluminate solution, or if it is added during the subsequent temperature phase. It can also be added to the washed filter dough.
Natriumsulfatet kan også innføres under vaskeprosessen som utføres for å senke pH-verdien, ved at natriumhydroxydet i vaske-vannet, som med fordel føres i motstrøm, nøytraliseres helt eller delvis med svovelsyre. Riktignok er som regel den natriumsulfat-mengde som på denne måte innføres for å forbedre egenskapene til The sodium sulphate can also be introduced during the washing process, which is carried out to lower the pH value, in that the sodium hydroxide in the washing water, which is advantageously carried in countercurrent, is completely or partially neutralized with sulfuric acid. Admittedly, as a rule, the amount of sodium sulphate introduced in this way is to improve the properties of
natriumaluminiumsilikatdeiger og -pulvere, ikke tilstrekkelig,sodium aluminum silicate pastes and powders, not sufficient,
og en ytterligere tilsetning av natriumsulfat er nødvendig. Også på grunn av den nøye dosering av natriumsulfatet er en ytterligere tilsetning som regel nødvendig. and a further addition of sodium sulphate is required. Also due to the careful dosing of the sodium sulphate, a further addition is usually necessary.
Eksempel 1Example 1
4,4 6 m 3 natriumaluminatoppløsning med molsammensetningen Na20/Al203= 6,2 og H20/Na20 = 23 ble under omrøring hurtig blandet med 0,54 m^ av en samtidig tilsatt natriumsilikatoppløsning med molsammensetningen Na2/OSi09= 0,83 og H20/Na20 = 13,4. Bland-ingen bie omrørt i 100 minutter ved 90°C, hurtig avkjølt, filtrert og vasket inntil en pH av 10,5. Filterdeigen inneholdt 40,2% faststoff. 4.4 6 m 3 sodium aluminate solution with the molar composition Na20/Al203= 6.2 and H20/Na20 = 23 was quickly mixed with 0.54 m^ of a simultaneously added sodium silicate solution with the molar composition Na2/OSi09= 0.83 and H20/ Na 2 O = 13.4. The mixture was stirred for 100 minutes at 90°C, rapidly cooled, filtered and washed until a pH of 10.5. The filter dough contained 40.2% solids.
En del av filterdeigen fikk henstå uten tilsetning i en 2001beholder (fyllingshøyde 60 cm). Efter 24 timer var deigen Part of the filter dough was left without addition in a 2001 container (filling height 60 cm). After 24 hours the dough was done
fremdeles flytbar, og dette ble fastslått ved en langsom tipping still floatable, and this was determined by a slow tipping
av beholderen med 45°. Da en stang (diameter 25 mm, flat ende) bie langsomt ført loddrett inn i deigen, kunne ingen uhomogenitet i deigens beskaffenhet fastslås. of the container by 45°. When a rod (diameter 25 mm, flat end) was slowly guided vertically into the dough, no inhomogeneity in the nature of the dough could be determined.
Efter 48 timer kunne et 1 cm høyt klart skikt iakttas over deigen. Deigen var imidlertid fremdeles flytbar. Et ca. 2 cm høyt bunnlegeme kunne fastslås ved hjelp av den loddrett innførte stav og var seigere enn den øvrige deig. After 48 hours, a 1 cm high clear layer could be observed over the dough. However, the dough was still flowable. An approx. The 2 cm high bottom body could be determined with the help of the vertically inserted rod and was tougher than the other dough.
Efter 72 timer kunne et 8 cm høyt, klart, overstående skikt over deigen og et likeledes ca. 8 cm tykt bunnskikt fastslås, og bunnskiktet var seigere enn deigen. Deigen kunne ikke lenger flyte. After 72 hours, an 8 cm high, clear, overlying layer could be placed over the dough and a similarly approx. An 8 cm thick bottom layer is determined, and the bottom layer was tougher than the dough. The dough could no longer flow.
Efter en uke var det klare, overstående skikt vokset til 28 cm. Ved å tippe beholderen 135° strømmet én øvre halvdel av deigen straks inn i et forlag, og bunnskiktmassen strømmet over . i løpet av 2 timer, med unntagelse av en ca. 1 cm tykk rest som heftet til bunnen. After a week, the upper layer was clear and had grown to 28 cm. By tipping the container 135°, one upper half of the dough immediately flowed into a press, and the bottom layer mass flowed over. within 2 hours, with the exception of an approx. 1 cm thick residue as a staple to the bottom.
Deigen som hadde et restinnhold av vann av 19,6%, ble homogenisert og igjen gjort flytbar ved rysting i 2 timer, og en prøve av deigen ble tørket i et laboratorieforstøvningstørke-apparat (utløpstemperatur 110°C) . The dough, which had a residual water content of 19.6%, was homogenized and made flowable again by shaking for 2 hours, and a sample of the dough was dried in a laboratory spray dryer (outlet temperature 110°C).
Kornstørrelsesfordelingen ble efter dispergering i vann (10 g produkt, 700 ml H20, 60 minutters omrøring ved 1000 om-dreininger pr. minutt) bestemt ifølge Andreasens metode. The grain size distribution was determined after dispersion in water (10 g of product, 700 ml of H2O, stirring for 60 minutes at 1000 revolutions per minute) according to Andreasen's method.
Resultatene er sammenfattet i den nedenstående tabell 1. The results are summarized in table 1 below.
En sammenligning mellom den dispergerte prøve efter for-støvningstørkingen og en prøve som ikke var blitt tørket, viste at det tørkede produkt hadde en utilfredsstillende dispergerbarhet, Sammenligningsprøven av deigen tilfredsstilte kravene fra vaskemiddel-industrien. A comparison between the dispersed sample after the spray drying and a sample that had not been dried showed that the dried product had an unsatisfactory dispersibility. The comparative sample of the dough satisfied the requirements of the detergent industry.
Eksempel 2Example 2
Ved en annen del av den ifølge eksempel 1 fremstilte deigWith another part of the dough prepared according to example 1
ble pr.1 kg av deigen efter vasking av denne 10 g fast Na^O^, 10 g of solid Na^O^ became per 1 kg of the dough after washing it,
svarende til 2,4% av den faststoffmengde som da var tilstede i deigen, blandet. Deigen ble likeledes fylt i en 200 1 beholder inntil en fyllingshøyde av 60 cm og iakttatt på samme måte som ifølge eksempel 1. De enkle forsøk, dvs. langsom helling av beholderen med 45° og innføring av staven,.viste at deigen fremdeles var homogen efter 7 dager. Derefter begynte gradvis de egenskaper å vise seg som inntraff for en deig uten tilsetning av Na2S04. corresponding to 2.4% of the amount of solids then present in the dough, mixed. The dough was likewise filled in a 200 1 container up to a filling height of 60 cm and observed in the same way as according to example 1. The simple tests, i.e. slowly tilting the container at 45° and introducing the rod, showed that the dough was still homogeneous after 7 days. Then, gradually, the properties that occurred for a dough without the addition of Na2SO4 began to appear.
Eksempel 3Example 3
Med en ytterligere del av deigen ifølge eksempel 1 bleWith a further part of the dough according to example 1 was
4 5 g fast natriumsulfat blandet pr. 1 kg deig, og denne natrium-sulfatmengde svarte til ca. 10% av den da. tilstedeværende faststoffmengde. Deigen ble iakttatt ved lagring i en 200 1 beholder (60 cm fyllingshøyde), som beskrevet i de ovenstående eksempler. 4 5 g of solid sodium sulphate mixed per 1 kg of dough, and this amount of sodium sulphate equaled approx. 10% of it then. amount of solids present. The dough was observed when stored in a 200 1 container (60 cm filling height), as described in the above examples.
Det ovenfor beskrevne forsøk viste at først efter ca. 4 uker begynte en avsetning ved at det ble dannet et klart, overstående skikt og en tettere bunnmasse. Denne bunnmasse fløt imidlertid også efter lagring i 8 uker ved å helle beholderen 135° praktisk talt kvantitativt straks over i forlaget sammen med hovedmassen uten at det var nødvendig med en omrøring. The experiment described above showed that only after approx. After 4 weeks, a deposit began with the formation of a clear, overlying layer and a denser bottom mass. However, this bottom mass also floated after storage for 8 weeks by pouring the container at 135° practically quantitatively immediately into the press together with the main mass without stirring being necessary.
Eksempel 4Example 4
100 g fast Na-jSO^pr. 1 kg deig ble blandet med en ytterligere del av deigen ifølge eksempel 1, og denne Na2SO^-mengde svarte til ca. 20% av den samlede faststoffmengde. Deigen ble iakttatt ved lagring i beholderen på 200 1 og med en fyllings- 100 g solid Na-jSO^pr. 1 kg of dough was mixed with a further part of the dough according to example 1, and this amount of Na2SO^ corresponded to approx. 20% of the total amount of solids. The dough was observed during storage in the container of 200 1 and with a filling
høyde av 60 cm. Hva gjelder flytbarheten viste deigen det samme forhold som ifølge eksempel 3. height of 60 cm. In terms of flowability, the dough showed the same ratio as according to example 3.
Efter en henstandstid på 4 uker ble en prøve av den homogeniserte deig tørket i et laboratorieforstøvningstørke-apparat. Kornstørrelsesfordelingen for det tørkede produkt og dessuten for deigen uten Na2S04-tilsetning ble efter dispergering i vann bestemt ifølge Andreasens metode. Det ble tatt hensyn til natriumsulfåtets innvirkning på det vandige mediums densitet og viskositet. Resultatene er gjengitt i tabell 2. After a standing time of 4 weeks, a sample of the homogenized dough was dried in a laboratory spray drying apparatus. The grain size distribution for the dried product and also for the dough without Na2SO4 addition was determined after dispersion in water according to Andreasen's method. Consideration was given to the effect of sodium sulphate on the density and viscosity of the aqueous medium. The results are reproduced in table 2.
Det fremgår av tabellen at det tørkede produkt praktisk talt igjen ble spaltet til de opprinnelige primære partikler ved dispergering i vann. It appears from the table that the dried product was practically split again into the original primary particles when dispersed in water.
Claims (5)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19772738085 DE2738085A1 (en) | 1977-08-24 | 1977-08-24 | PROCESS FOR IMPROVING THE PROPERTIES OF SODIUM ALUMINUM SILICATE POWDER AND POWDER |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| NO782864L true NO782864L (en) | 1979-02-27 |
Family
ID=6017132
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO782864A NO782864L (en) | 1977-08-24 | 1978-08-23 | PROCEDURES FOR AA IMPROVING THE PRODUCTS OF SODIUM ALUMINUM SILICATE DOUGHS AND POWDER |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP0000870A1 (en) |
| AT (1) | ATA615178A (en) |
| DE (1) | DE2738085A1 (en) |
| DK (1) | DK371378A (en) |
| IT (1) | IT1098273B (en) |
| NO (1) | NO782864L (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5738317A (en) * | 1980-08-12 | 1982-03-03 | Toyo Soda Mfg Co Ltd | Zeolite powder with high fluidity and its manufacture |
| AU558660B2 (en) * | 1982-06-21 | 1987-02-05 | Unilever Plc | Aluminosilicates |
| US4582615A (en) * | 1984-11-26 | 1986-04-15 | Colgate Palmolive Co. | Bentonite-sulfate fabric softening particulate agglomerate, processes for manufacture and use thereof, and detergent compositions containing it |
| US5236680A (en) * | 1987-01-20 | 1993-08-17 | Mizusawa Industrial Chemicals, Ltd. | Preparation of amorphous silica-alumina particles by acid-treating spherical P-type zeolite particles crystallized from a sodium aluminosilicate gel |
| DE3702764A1 (en) * | 1987-01-30 | 1988-08-11 | Degussa | DETERGENT PICTURES |
| US5174918A (en) * | 1987-06-06 | 1992-12-29 | Degussa Ag | Stable aqueous suspensions of detergent zeolites and four oxo-alcohol ethoxylates |
| CN100411983C (en) * | 2006-08-23 | 2008-08-20 | 中国铝业股份有限公司 | Method for preparing superfine alumina silicate |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2514399C2 (en) * | 1975-04-02 | 1987-01-29 | Degussa Ag, 6000 Frankfurt | Process for the production of aluminium silicates |
| DE2533614C2 (en) * | 1975-07-26 | 1985-10-31 | Degussa Ag, 6000 Frankfurt | Process for the production of zeolitic alkali aluminum silicates |
| US4102977A (en) * | 1975-11-18 | 1978-07-25 | Mizusawa Kagaku Kogyo Kabushiki Kaisha | Process for the preparation of alkali aluminosilicate detergent builder |
| AT356628B (en) * | 1976-02-06 | 1980-05-12 | Henkel Kgaa | METHOD FOR THE PRODUCTION OF AQUEOUS, FOR FURTHER PROCESSING OF WASHING AND CLEANING AGENTS SUITABLE SUSPENSIONS OF FINE-PARTICULATE WATER-UNLOCATED WATER-UNLOCKED WATER-UNLOCKED |
-
1977
- 1977-08-24 DE DE19772738085 patent/DE2738085A1/en not_active Withdrawn
-
1978
- 1978-07-25 EP EP78100496A patent/EP0000870A1/en not_active Withdrawn
- 1978-08-22 IT IT26914/78A patent/IT1098273B/en active
- 1978-08-23 AT AT615178A patent/ATA615178A/en not_active Application Discontinuation
- 1978-08-23 NO NO782864A patent/NO782864L/en unknown
- 1978-08-23 DK DK371378A patent/DK371378A/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| DK371378A (en) | 1979-02-25 |
| IT1098273B (en) | 1985-09-07 |
| ATA615178A (en) | 1980-08-15 |
| IT7826914A0 (en) | 1978-08-22 |
| DE2738085A1 (en) | 1979-03-08 |
| EP0000870A1 (en) | 1979-03-07 |
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