SI9012000A - Method for preparation of sodium silicates - Google Patents
Method for preparation of sodium silicates Download PDFInfo
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- SI9012000A SI9012000A SI9012000A SI9012000A SI9012000A SI 9012000 A SI9012000 A SI 9012000A SI 9012000 A SI9012000 A SI 9012000A SI 9012000 A SI9012000 A SI 9012000A SI 9012000 A SI9012000 A SI 9012000A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
- C01B33/325—After-treatment, e.g. purification or stabilisation of solutions, granulation; Dissolution; Obtaining solid silicate, e.g. from a solution by spray-drying, flashing off water or adding a coagulant
Abstract
Description
HOECHST AKTIENGESELLSCHAFTHOECHST AKTIENGESELLSCHAFT
Postopek za pripravo natrijevih silikatovProcess for the preparation of sodium silicates
Pričujoči izum se nanaša na postopek za pripravo amorfnih natrijevih silikatov z vsebnostjo vode 0,3 do 6 mas.%, prednostno 0,5 do 2 mas.%, in molskim razmerjem med SiO2 in Na2O (1,9 do 2,8) : 1 iz raztopine topnega stekla z najmanj 20 mas.% trdne snovi.The present invention relates to a process for the preparation of amorphous sodium silicates having a water content of 0.3 to 6% by weight, preferably 0.5 to 2% by weight, and a molar ratio of SiO 2 to Na 2 O (1.9 to 2, 8): 1 from a solution of soluble glass with at least 20% by weight of solid.
Iz US P 3 471 253 je znano, da se da dobiti raztopino topnega stekla tako, da dajo 42 mas.%-ni natrijev lug in pesek (silicijev dioksid) v masnem razmerju okoli 2:1 v mešalni avtoklav in puste v njem 3 ure pri 210°C in 16 bar. Vroča raztopina natrijevega silikata, ki jo odvzamejo po ohlajenju vsebine avtoklava na 85°C, vsebuje po odfiltriranju prebitnega peska in drugih nečistot 57,5 % trdne snovi in kaže razmerje SiO2: Na2O 1,64:1.It is known from US P 3 471 253 that a solution of soluble glass can be obtained by placing 42% by weight of sodium alkali and sand (silica) about 2: 1 in a mixing autoclave and leaving in it for 3 hours at 210 ° C and 16 bar. The hot sodium silicate solution, which is removed after cooling the autoclave content to 85 ° C, contains 57.5% solids after filtration of excess sand and other impurities and shows a SiO 2 : Na 2 O ratio of 1.64: 1.
Kristalinične natrijeve silikate s slojevito strukturo in molskim razmerjem med SiO2 in Na2O (1,9 do 3,5) : 1 pripravijo po postopku po DE-OS 37 18 350 tako, da obdelajo raztopine topnega stekla z vsebnostjo trdne snovi od 20 do 65 mas.% v razpršilno sušilni coni ob tvorbi amorfnega natrijevega silikata, ki vsebuje vodo,- pri čemer ima odpadni plin, ki odteka iz razpršilno sušilne cone, temperaturo najmanj 140°C. Amorfni natrijev silikat, ki vsebuje vodo, temprajo v žarilni coni pri 500 do 800 °C 1 do 60 minut v prisotnosti najmanj 10 mas.% povratnega materiala, ki so ga dobili z mehanskim drobljenjem kristaliničnega natrijevega silikata, ki so ga pred tem iznesli iz žarilne cone.Crystalline sodium silicates with a layered structure and a molar ratio of SiO 2 to Na 2 O (1.9 to 3.5): 1 are prepared by the process of DE-OS 37 18 350 by treating soluble glass solutions with a solids content of 20 up to 65% by weight in the spray drying zone on formation of amorphous sodium silicate containing water - the waste gas leaving the spray drying zone has a temperature of at least 140 ° C. Amorphous sodium silicate containing water is tempered in the annealing zone at 500 to 800 ° C for 1 to 60 minutes in the presence of at least 10% by weight of the return material obtained by mechanical crushing of crystalline sodium silicate previously extracted from annealing zones.
Pri pravkar navedenem postopku je neugodno, da zahteva material, ki nastane pri razpršilnem sušenju, zaradi svoje majhne nasipne gostote 100 do 250 g/1 velik volumen in da se močno praši. Nadalje pogojuje uporaba povratnega materiala med tempranjem precej več stroškov za aparate in zahteva zaradi večjega pretoka materiala večje dimenzionirano vrtljivo cev.In the process just mentioned, it is disadvantageous to require a large bulk density of 100 to 250 g / l and to be highly dusty due to its low bulk density. Furthermore, the use of return material during tempering is significantly more costly for appliances and requires a larger dimensioned rotary tube due to the greater material flow.
V smislu izuma premagamo navedene pomanjkljivosti pri pripravi amorfnih natrijevih silikatov iz raztopine topnega stekla z najmanj 20 mas.% trdne snovi tako, daAccording to the invention, the disadvantages in the preparation of amorphous sodium silicates from a solution of soluble glass with at least 20% by weight of a solid are overcome, such that
a) pridobimo raztopino topnega stekla s presnovo kremenčevega peska z natrijevim lugom v molskem razmerju SiO2 : Na2O (2,0 do 2,8) : 1 pri temperaturah od 180 do 240°C in tlakih od 10 do 30 bar;a) obtain a solution of soluble glass by the digestion of silica sand with sodium hydroxide in a molar ratio of SiO 2 : Na 2 O (2.0 to 2.8): 1 at temperatures from 180 to 240 ° C and pressures from 10 to 30 bar;
b) obdelamo raztopino topnega stekla v razpršilno sušilni coni z vročim zrakom z 200 do 300°C pri zadrževalnem času 10 do 25 s in temperaturi odpadnega plina, ki zapušča razpršilno sušilno cono, 90 do 130°C, ob tvorbi prahastega amorfnega natrijevega silikata z vsebnostjo vode (določeno kot izguba pri žarjenju pri 700°C) 15 do 23 mas.% in nasipno maso več kot 300 g/1;b) treat the soluble glass solution in the hot air spray drying zone from 200 to 300 ° C at a holding time of 10 to 25 s and the waste gas leaving the spray drying zone 90 to 130 ° C to form a powdery amorphous sodium silicate with a water content (determined as annealing loss at 700 ° C) of 15 to 23% by weight and a bulk density exceeding 300 g / l;
c) spravimo prahasti natrijev silikat po b) v poševno nameščeno, s pripravami za premikanje trdne snovi opremljeno vrtljivo cevno peč in ga v njej protitočno obdelujemo z dimnim plinom pri temperaturah od 250 do 500°C 1 do 60 minut, pri čemer je vrtljiva cevna peč izolirana tako, da znaša temperatura njene zunanje stene manj kot 60°C;c) Put the powdered sodium silicate according to b) in a slanted, rotary tube furnace equipped with a solids moving device and counter-flow it in a flue gas at temperatures from 250 to 500 ° C for 1 to 60 minutes, with the rotary tube furnace insulated so that the temperature of its outer wall is less than 60 ° C;
d) amorfni natrijev silikat, ki izstopa iz vrtljive cevne peči, zdrobimo s pomočjo mehanskega drobilnika na zrnavost od 0,1 do 12 mm.d) the amorphous sodium silicate exiting the rotary tube furnace is crushed by means of a mechanical shredder to a grain size of 0.1 to 12 mm.
Postopek po izumu je lahko nadalje po izbiri izoblikovan še tako, da aa) zdrobljeni natrijev silikat zmeljemo s pomočjo mlina na zrnavosti od 2 do 400 gm;The process of the invention may further be optionally further formed by aa) grinding the crushed sodium silicate using a mill on a grain size of 2 to 400 gm;
bb) uporabimo mehanski mlin, ki obratuje pri obodni hitrosti 0,5 do 60 m/s; cc) uporabimo mlin na zračni curek;bb) use a mechanical mill operating at a circumferential speed of 0.5 to 60 m / s; cc) use an air jet mill;
dd) uporabimo krogelni mlin s keramično oblogo;dd) use a ball mill with a ceramic coating;
ee) uporabimo nihajni mlin s keramično oblogo;ee) use a swing mill with a ceramic coating;
ff) odsesamo odpadni plin iz vrtljive cevne peči v njenem srednjem področju in v področju njenega konca, ki rabi za vnašanje prahastega amorfnega natrijevega silikata z vsebnostjo vode od 15 do 23 mas.%, in ga očistimo s pomočjo filtra za suho odpraševanje, pri čemer kvazikontinuirno primešavamo natrijev silikat, ki smo ga odvzeli iz filtra za suho odpraševanje, prahastemu, amorfnemu natrijevemu silikatu, ki je določen za vnašanje v vrtljivo cevno peč;ff) aspirate the waste gas from a rotary tube furnace in its middle region and in the region of its end, which requires the introduction of powdered amorphous sodium silicate with a water content of 15 to 23% by weight, and purify it using a dry dust filter, whereby quasi-continually stirring the sodium silicate, which was removed from the dry dust filter, to powdered, amorphous sodium silicate, which is intended to be introduced into a rotary tube furnace;
gg) zmleti natrijev silikat dovajamo v valjčno kompaktirno pripravo, s katero ga pri pritisnem tlaku valja 20 do 40 kN/cm širine valja stisnemo v kompaktne dele;gg) the ground sodium silicate is fed into a roller compacting device, which, at a cylinder pressure of 20 to 40 kN / cm, compresses it into compact parts;
hh) predelamo kompaktne dele po predhodnem drobljenju s tem, da jih pretlačimo skozi sita v granulat z nasipno maso od 700 do 1000 g/1.hh) process the compact parts after preliminary crushing by compressing them through sieves into a granulate with a bulk weight of 700 to 1000 g / l.
Natrijeve silikate lahko uporabimo kot sredstva za mehčanje vode.Sodium silicates can be used as water softeners.
Pri postopku po izumu dobimo zaradi nizke temperature in kratkega zadrževalnega časa pri razprševanju raztopine topnega stekla natrijev silikat z veliko nasipno maso, s katerim se da dobro ravnati.In the process according to the invention, due to the low temperature and short retention time of the solution of the soluble glass solution, sodium silicate with a large bulk mass can be handled.
Majhno prevajanje toplote skozi stene vrtljive cevne peči zaradi njene dobre izolacije deluje pri postopku v smislu izuma proti nagnjenju natrijevega silikata k lepljenju.Due to its good insulation, a small heat transfer through the walls of the rotary tube furnace works in the process of the invention against the tendency of sodium silicate to adhere.
Pri postopku v smislu izuma je potrebna uporaba mehanskega mlina s počasnim tekom (npr. kolutnega mlina, udarnega mlina, mlina s kladivi ali valjčnega mlina), da preprečimo obrabo železa z mlevskih orodij.The process of the invention requires the use of a slow-motion mechanical mill (e.g., a mill mill, a hammer mill, a hammer mill or a rolling mill) to prevent the wear of the iron from grinding tools.
Če uporabljamo pri postopku po izumu krogelni mlin s keramično oblogo ali nihalni mlin ali mlin na zračni curek za najfinejše produkte, t.j. s premeri od 6 do 10 μτη, prav tako ne pride do onesnaženja natrijevega silikata zaradi obrabe kovine.If a ball mill with a ceramic coating or a pendulum or air jet mill is used in the process according to the invention for the finest products, i.e. with diameters of 6 to 10 μτη, there is also no contamination of sodium silicate due to metal wear.
Z istočasnim odsesavanjem odpadnega plina, ki vsebuje prah, v srednjem področju vrtljive cevne peči in v področju njenega konca na dodajalni strani pri postopku v smislu izuma znatno zmanjšamo obremenitev s prahom v odpadnem plinu, ker se prah sprosti predvsem pri dodajanju natrijevega silikata v vrtljivo cevno peč in ker se hitrost plina v dodajalnem področju amorfnega natrijevega silikata, ki vsebuje vodo, zmanjša.By simultaneously aspirating the waste gas containing the dust in the middle region of the rotary tube furnace and in the region of its end on the inlet side of the process according to the invention, the dust load in the waste gas is significantly reduced, since the dust is released mainly by adding sodium silicate to the rotary tube and because the gas velocity in the feed area of amorphous sodium silicate containing water decreases.
S postopkom po izumu dobimo s kompaktiranjem proti obrabi odporen granulat, ki v vodi zelo hitro razpade.By the process of the invention, a wear-resistant granulate is obtained by compacting against wear and tear, which breaks down very quickly in water.
Preostale trdote, navedene v primerih 2 in 3, smo ugotovili po temle predpisu.The remaining hardnesses listed in cases 2 and 3 were determined according to this regulation.
V 1000 ml vodovodne vode z 18°dH (ustreza vsebnosti 85 mg Ca in 15 mg Mg na liter) smo suspendirali 2,5 g natrijevega silikata. Suspenzijo smo mešali 30 minut pri 60°C z magnetnim mešalom z okoli 500 vrt./min. Po hitrem ohlajenju v ledeni vodi na 20°C smo suspenzijo filtrirali preko membranskega filtra (širina por 0,045 μτη). V bistrem filtratu smo z atomsko absorpcijo določili vsebnosti kalcija in magnezija.2.5 g of sodium silicate were suspended in 1000 ml of tap water at 18 ° dH (corresponding to 85 mg Ca and 15 mg Mg per liter). The suspension was stirred for 30 minutes at 60 ° C with a magnetic stirrer at about 500 rpm. After rapid cooling in ice water at 20 ° C, the suspension was filtered through a membrane filter (pore width 0.045 μτη). Atoms of calcium and magnesium were determined by atomic absorption in the clear filtrate.
Primer 1 (po stanju tehnike)Example 1 (state of the art)
Iz raztopine topnega stekla z vsebnostjo trdne snovi 45% smo izdelali v razpršilnem stolpu na vroči zrak (temperatura odpadnega plina : 154°C) amorfen natrijev disilikat, kije kazal izgubo pri žarjenju pri 700°C 19% in nasipno maso 220g/l.From a solution of soluble glass with a solids content of 45%, amorphous sodium disilicate was produced in a hot air spray tower (waste gas temperature: 154 ° C), which showed an annealing loss at 700 ° C of 19% and a bulk density of 220g / l.
V direktno kurjeno vrtljivo cevno peč (dolžina 5 m, premer 78 cm, nagib 1,2°) smo na njenem koncu, ki leži nasproti plamena, dodajali preko dozirnega polža 60 kg/h amorfnega natrijevega disilikata z vsebnostjo vode (določeno kot izguba pri žaljenju pri 700°C) 18 mas.% in 15 kg/h povratnega materiala, ki smo ga dobili z drobljenjem produkta, dobljenega v eni od prejšnjih šarž, na manj kot 250 μτη, medtem ko smo kristalinični produkt iznašali na plamenski strani. Temperatura na najbolj vročem mestu vrtljive cevne peči je znašala 740°C.A 60 kg / h amorphous sodium disilicate with a water content (determined as the loss in the direct flame rotary tube furnace (length 5 m, diameter 78 cm, slope 1.2 °) at its end opposite the flame was added via a metering auger). insult at 700 ° C) 18% by weight and 15 kg / h of return material obtained by crushing the product obtained in one of the preceding batches to less than 250 μτη while the crystalline product was removed on the flame side. The temperature at the hottest place of the rotary tube furnace was 740 ° C.
Na steni vrtljive cevne peči se ni tvorilo nič prilepkov; iznešeni natrijev disilikat je bil daljnosežno prahast.Nothing pasted on the wall of the rotary tube furnace; the disoded sodium disilicate was far-reaching powdery.
Primer 2 (po izumu)Example 2 (Invention)
V valjast avtoklav z oblogo iz niklja z mešalno pripravo smo napolnili pesek (99 mas.% SiO2; zrnavost: 90% < 0,5 mm) in 50 mas.%-ni natrijev lug v molskem razmeiju med SiO2 in Na2O 2,15 : 1. Mešanico v avtoklavu smo med mešanjem z vkomprimiranjem vodne pare (16 bar) segreli na 200°C in jo vzdrževali pri tej temperaturi 60 minut. Nato smo vsebino avtoklava preko izparilne posode dekomprimirali v drugo posodo in za ločitev netopnega po dodatku 0,3 mas.% Perlita kot pomožnega filtrirnega sredstva filtrirali pri 90°C preko ploščnega tlačnega filtra. Kot filtrat smo dobili bisto raztopino topnega stekla z molskim razmerjem med SiO2 in Na2O 2,04 : 1. Z razredčenjem z vodo smo naravnali vsebnost trdne snovi na 50%.Sand (99% by weight SiO 2 ; granularity: 90% <0.5 mm) and 50% by weight - no sodium hydroxide in the molar ratio between SiO 2 and Na 2 O were filled into a cylindrical autoclave with a nickel plating mixer. 2.15: 1. The mixture in the autoclave was heated to 200 [deg.] C. while stirring by compressing the steam (16 bar) and maintained at this temperature for 60 minutes. The contents of the autoclave were then decompressed via a evaporation vessel into another vessel and, to separate the insoluble, by the addition of 0.3 wt.% Perlite, as an auxiliary filtering agent, was filtered at 90 ° C via a plate pressure filter. The filtrate was obtained as a clear solution of soluble glass with a molar ratio of SiO 2 to Na 2 O 2.04: 1. By dilution with water, the solids content was adjusted to 50%.
V razpršilni stolp z vročim zrakom, opremljen s centrifugalnim ploščnim razprševalnikom, ki smo ga segrevali preko plinsko kurjene zgorevalne komore in ki je bil za ločitev produkta povezan z vrečastim filtrom s pnevmatskim čiščenjem, smo razpršili raztopino topnega stekla, pri čemer smo zgorevalno komoro naravnali tako, da je imel vroči plin, ki vstopa pri vrhu stolpa, temperaturo 260°C. Množino raztopine topnega stekla, ki jo je bilo treba razpršiti, smo naravnali tako, da je znašala temperatura zmesi silikata in plina, kije zapuščala razpršilni stolp, 105°C. Iz volumna razpršilnega stolpa in iz množine pretoka plina skozi razpršilni stolp smo izračunali zadrževalni čas 16 sekund. V vrečastem filtru izločeni amorfni natrijev disilikat je imel pri majhni nagnjenosti k prašenju nasipno maso 480g/l, vsebnost železa 0,01 mas.%, razmerje SiO2 : Na2O 2,04 : 1 in vsebnost vode (določeno kot izguba pri žarjenju pri 700°C) 19,4%; njegov srednji premer delcev je znašal 52/im.In a hot air spray tower equipped with a centrifugal plate sprayer, which was heated via a gas-fired combustion chamber and connected to the bag filter by pneumatic cleaning to separate the product, a solution of soluble glass was sprayed, adjusting the combustion chamber by , that the hot gas entering the top of the tower had a temperature of 260 ° C. The amount of soluble glass solution to be sprayed was adjusted to the temperature of the mixture of silicate and gas leaving the spray tower at 105 ° C. A residence time of 16 seconds was calculated from the volume of the spray tower and the amount of gas flow through the spray tower. In the bag filter, the amorphous sodium disilicate extract eliminated, with a low propensity to dust, a bulk mass of 480g / l, an iron content of 0.01% by weight, a SiO ratio of 2 : Na 2 O 2.04: 1 and a water content (determined as annealing loss at 700 ° C) 19.4%; its mean particle diameter was 52 / im.
V primeru 1 opisana vrtljiva cevna peč je bila z večplastno mineralno volno in pločevinastim plaščem izolirana tako, da je pri temperaturi 390°C v notranjosti vrtljive cevne peči znašala temperatura na njeni zunanji površini največ 38°C. V to vrtljivo cevno peč smo vnašali 60 kg amorfnega natrijevega disilikata na uro, pri čemer se ni tvorilo nič prilepkov. Amorfni natrijev disilikat (Na2Si2O5), ki je zapuščal vrtljivo cevno peč in ki je imel vsebnost vode 0,7 mas.% (določeno kot izguba pri žarjenju pri 700°C), smo s pomočjo mehanskega drobilnika zdrobili na zrnavost manj kot 6 mm in po vmesnem hlajenju zmleli na kolutnem mlinu (premer 30 cm) pri 400 min'1 do srednjega premera delcev 95 /im, pri čemer je ostala vsebnost železa v zmletem produktu enaka vsebnosti železa v natrijevem disilikatu, ki smo ga vnašali v vrtljivo cevno peč.In Example 1, the rotary tube furnace described was insulated with a multi-layer mineral wool and sheet metal so that at a temperature of 390 ° C, the inside surface of the rotary tube furnace had a maximum temperature of 38 ° C. 60 kg of amorphous sodium disilicate per hour were introduced into this rotary tube furnace, with no pasting. Amorphous sodium disilicate (Na 2 Si 2 O 5 ) leaving a rotary tube furnace and having a water content of 0.7% by weight (determined as annealing loss at 700 ° C) was ground to a grain size using a mechanical shredder. less than 6 mm and after intermediate cooling ground on a disc mill (30 cm diameter) at 400 min -1 to a mean particle diameter of 95 / im, leaving the iron content of the ground product equal to the iron content of the sodium disilicate introduced. into a rotary tube furnace.
Odpadni plin vrtljive cevne peči smo odsesali v vnašalnem področju za amorfni natrijev disilikat z vsebnostjo vode (določeno kot izguba pri žarjenju pri 700°C) 19,4 mas.% in ga dovajali v pralni stolp. Z odpadnim plinom smo iznašali 3 kg natrijevega disilikata na uro.The waste gas of the rotary tube furnace was aspirated in the inlet area for amorphous sodium disilicate with a water content (determined as annealing loss at 700 ° C) of 19.4% by weight and was fed to the washing tower. Waste gas was extracted with 3 kg of sodium disilicate per hour.
Preostala trdota tako pripravljenega natrijevega disilikata je znašala 2,5 mg/1 Ca in manj kot 1 mg/1 Mg.The residual hardness of the sodium disilicate thus prepared was 2.5 mg / 1 Ca and less than 1 mg / 1 Mg.
Primer 3 (po izumu)Example 3 (Invention)
Primer 2 smo ponovili s spremembo, da je znašala temperatura v notranjosti vrtljive cevne peči 300°C in na njeni zunanji površini 35°C. Pri tem je imel amorfni natrijev disilikat, ki je zapuščal vrtljivo cevno peč, vsebnost vode (določeno kot izguba pri žarjenju pri 700°C) 5 mas.%.Example 2 was repeated with the change that the temperature inside the rotary tube furnace was 300 ° C and on its outer surface was 35 ° C. The amorphous sodium disilicate leaving the rotary tube furnace had a water content (determined as annealing loss at 700 ° C) of 5% by weight.
Preostala trdota tako pripravljenega natrijevega disilikata je znašala 3,5 mg/1 Ca in 1,5 mg/1 Mg.The residual hardness of sodium disilicate thus prepared was 3.5 mg / 1 Ca and 1.5 mg / 1 Mg.
Primer 4 (po izumu)Example 4 (Invention)
Po primeru 2 dobljeni produkt s srednjim premerom delcev 95 μτη smo še dalje drobili s pomočjo protistrujnega mlina s fluidiziranim slojem z vgrajeno mehansko klasirno pripravo. V odvisnosti od nastavljenega števila vrtljajev klasirne priprave smo dobili natrijev disilikat brez obrabe s srednjim premerom delcev 2 do 15 μτη.According to Example 2, the resulting product with a mean particle diameter of 95 μτη was further crushed by means of a fluidized bed antistatic mill with a built-in mechanical clustering device. Depending on the set speed of the cluster preparation, sodium disilicate without wear was obtained with a mean particle diameter of 2 to 15 μτη.
Primer 5 (po izumu)Example 5 (Invention)
Po primeru 2 dobljeni produkt smo še dalje drobili s pomočjo krogelnega mlina s porcelansko oblogo, napolnjenega s korundnimi kroglami. Dobili smo natrijev dis7 ilikat brez obrabe s srednjim premerom delcev od 5 do 14 /im, odvisnim od trajanja mletja.In Example 2, the resulting product was further crushed using a porcelain-coated ball mill filled with corundum spheres. We obtained sodium dis7 illicite without wear with a mean particle diameter of 5 to 14 [mu] m, depending on the duration of milling.
Primer 6 (po izumu)Example 6 (Invention)
Po primeru 2 dobljeni produkt smo v valjčni kompaktirni pripravi s pritisnim tlakom kompaktirnih valjev 30 kN/cm širine valja in temu sledečim drobljenjem dobljenega materiala v granulatoiju s siti predelali v granulat brez prahu s srednjim premerom delcev 900 gm, nasipno maso 870 g/1 in veliko odpornostjo proti obrabi.In Example 2, the resulting product was rolled into a compacting roller with a compaction pressure of 30 kN / cm of roller width, and the subsequent crushing of the obtained material in granules with sieves was transformed into a powderless granulate with a mean particle diameter of 900 gm, a bulk mass of 870 g / l, and high abrasion resistance.
Za določitev odpornosti proti obrabi smo obdelovali 50 g granulata v kotalnem krogelnem mlinu (dolžina 10 cm; premer 11,5 cm; 8 jeklenih krogel s premerom 2 cm) 5 minut pri vrtilni hitrosti 100 vrtljajev min'1.To determine the abrasion resistance, we treated 50 g of granulate in a rolling mill (length 10 cm; diameter 11.5 cm; 8 steel balls 2 cm in diameter) for 5 minutes at a rotational speed of 100 rpm min ' 1 .
Po izvedbi obrabnega testa je znašal srednji premer delcev še 720 /im, kar ustreza zmanjšanju za okoli 20%.After the wear test, the mean particle diameter was still 720 / im, which corresponds to a reduction of about 20%.
Primer 7 (po izumu)Example 7 (Invention)
Primer 2 smo ponovili s spremembo, da smo odpadni plin iz vrtljive cevne peči odsesavali na dveh mestih in sicer na področju vnašanja amorfnega natrijevega disilikata z vsebnostjo vode 19,4 mas.%, dodatno pa še na mestu vrtljive cevne peči, ki je bilo oddaljeno od navedenega področja vnašanja okoli 2 m v smeri osi vrtljive cevne peči. Oba toka odpadnega plina smo združili in trdno snov, ki sta jo vsebovala, ločili s pomočjo proti vročini odpornega vrečastega filtra. Ločeno trdno snov smo skupaj z amorfnim natrijevim disilikatom z vsebnostjo vode 19,4 mas.% ponovno vnesli v vrtljivo cevno peč tako, da ni šlo v izgubo nič natrijevega disilikata. S tem se je povečala proizvodnja vrtljive cevne peči na 70 kg/h, vendar pa se v notranjosti vrtljive cevne peči ni pojavilo nič prilepkov.Example 2 was repeated by modifying that the exhaust gas from the rotary tube furnace was aspirated in two places, in the area of introduction of amorphous sodium disilicate with a water content of 19.4% by weight, and additionally at the location of the rotary tube furnace, which was distant from said inlet area about 2 m in the direction of the axis of the rotary tube furnace. Both waste gas streams were combined and the solid contained therein was separated by a heat-resistant bag filter. The separated solid, together with the amorphous sodium disilicate with a water content of 19.4% by weight, was re-introduced into the rotary tube furnace so that no sodium disilicate was lost. This increased the production of the rotary tube furnace to 70 kg / h, but no adhesions appeared inside the rotary tube furnace.
Primer 8 (primerjalni primer)Example 8 (Comparative Example)
Primer 2 smo ponovili s spremembo, da je imel vroči plin, ki je vstopal na vrhu razpršilnega stolpa z vročim zrakom, temperaturo 330°C. Temperatura zmesi silikata in plina, ki je zapuščala razpršilni stolp, je znašala 140°C. V vrečastem filtru izločeni natrijev disilikat je imel nasipno maso 250 g/1, vsebnost vode (določeno kot izguba pri žaljenju pri 700°C) 17,9 mas.% in srednji premer delcev 60 μτη. Ta natrijev disilikat seje močno prašil.Example 2 was repeated with the change that the hot gas entering the top of the hot air spray tower had a temperature of 330 ° C. The temperature of the mixture of silicate and gas leaving the spray tower was 140 ° C. The bagged sodium disilicate extract had a bulk density of 250 g / l in the bag filter, a water content (determined as an insult loss at 700 ° C) of 17.9% by weight, and a mean particle diameter of 60 μτη. This sodium disilicate is heavily dusted.
Primer 9 (primerjalni primer)Example 9 (Comparative Example)
Primer 2 smo ponovili s spremembo, da je bila vrtljiva cevna peč izolirana samo tako, da je pri temperaturi 490°C v notranjosti vrtljive cevne peči znašala temperatura na njeni zunanji površini največ 150°C. Zaradi tega so se trvorili na notranji steni vrtljive cevne peči na velikih ploskvah prilepki, ki jih je bilo treba pogosto mehansko odbijati. Iz vrtljive cevne peči smo iznašali produkt, ki je imel deloma velikost nogometne žoge in ga je bilo z mehanskim drobilnikom le težko zdrobiti.Example 2 was repeated with the change that the rotary tube furnace was insulated only so that at a temperature of 490 ° C inside the rotary tube furnace the temperature at its outer surface was at most 150 ° C. As a result, there were adhesions on the inner wall of the rotary tube furnace on large surfaces that often had to be mechanically repelled. From the rotary tube furnace, we extracted a product that was partly the size of a soccer ball and was difficult to crush with a mechanical shredder.
Primer 10 (primerjalni primer)Example 10 (Comparative Example)
Primer 2 smo ponovili s spremembo, da smo s pomočjo mehanskega drobilnika zdrobljeni natrijev disilikat zmleli ob uporabi mlina z udarnimi krožniki pri 10.000 min4 na srednji premer delcev 83 μτη. Zmleti produkt je imel siv odtenek in vsebnost železa 0,02 mas.%.Example 2 was repeated with the change that, using a mechanical shredder, the crushed sodium disilicate was ground using a shock mill at 10,000 min 4 to a mean particle diameter of 83 μτη. The ground product had a gray tint and an iron content of 0.02% by weight.
Claims (9)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3935464 | 1989-10-25 | ||
| DE4004625 | 1990-02-15 | ||
| YU200090A YU200090A (en) | 1989-10-25 | 1990-10-24 | PROCEDURE FOR OBTAINING SODIUM SILICATE |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SI9012000A true SI9012000A (en) | 1997-12-31 |
Family
ID=25886412
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SI9012000A SI9012000A (en) | 1989-10-25 | 1990-10-24 | Method for preparation of sodium silicates |
Country Status (17)
| Country | Link |
|---|---|
| EP (1) | EP0425427B1 (en) |
| JP (1) | JPH0669891B2 (en) |
| KR (1) | KR0143991B1 (en) |
| AR (2) | AR243478A1 (en) |
| BR (1) | BR9005386A (en) |
| CA (1) | CA2025073C (en) |
| DE (1) | DE4031849A1 (en) |
| DK (1) | DK0425427T3 (en) |
| ES (1) | ES2047897T3 (en) |
| FI (1) | FI905210A0 (en) |
| HR (1) | HRP921199B1 (en) |
| LV (1) | LV10764B (en) |
| NO (1) | NO904604L (en) |
| PT (1) | PT95664A (en) |
| RU (1) | RU2039701C1 (en) |
| SI (1) | SI9012000A (en) |
| TR (1) | TR24995A (en) |
Families Citing this family (44)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8904007D0 (en) * | 1989-02-22 | 1989-04-05 | Procter & Gamble | Stabilized,bleach containing,liquid detergent compositions |
| DE4107231A1 (en) * | 1991-03-07 | 1992-09-10 | Hoechst Ag | METHOD FOR PRODUCING SODIUM SILICATE |
| DE4330868A1 (en) * | 1993-09-11 | 1995-03-16 | Hoechst Ag | Process for preparing granular sodium silicate |
| DE4400024A1 (en) * | 1994-01-03 | 1995-07-06 | Henkel Kgaa | Silicate builders and their use in detergents and cleaning agents as well as multi-component mixtures for use in this field |
| US5691295A (en) * | 1995-01-17 | 1997-11-25 | Cognis Gesellschaft Fuer Biotechnologie Mbh | Detergent compositions |
| JP3312816B2 (en) | 1994-07-14 | 2002-08-12 | 株式会社トクヤマ | Amorphous sodium silicate powder and method for producing the same |
| DE19509303A1 (en) * | 1995-03-15 | 1996-09-19 | Henkel Kgaa | Silicate builder by tempering piece glass |
| DE19515072A1 (en) * | 1995-04-28 | 1996-10-31 | Cognis Bio Umwelt | Detergent containing cellulase |
| ES2150696T3 (en) | 1995-11-09 | 2000-12-01 | Akzo Pq Silica Vof | COMPACT SODIUM SILICATE. |
| DE19545729A1 (en) | 1995-12-08 | 1997-06-12 | Henkel Kgaa | Bleach and detergent with an enzymatic bleaching system |
| DE19600018A1 (en) | 1996-01-03 | 1997-07-10 | Henkel Kgaa | Detergent with certain oxidized oligosaccharides |
| DE19605688A1 (en) * | 1996-02-16 | 1997-08-21 | Henkel Kgaa | Transition metal complexes as activators for peroxygen compounds |
| DE19620411A1 (en) | 1996-04-01 | 1997-10-02 | Henkel Kgaa | Transition metal amine complexes as activators for peroxygen compounds |
| EP0891415A1 (en) | 1996-04-01 | 1999-01-20 | Henkel Kommanditgesellschaft auf Aktien | Cleaning agent with oligoammine activator complexes for peroxide compounds |
| DE19616693A1 (en) * | 1996-04-26 | 1997-11-06 | Henkel Kgaa | Enol esters as bleach activators for detergents and cleaning agents |
| DE19713852A1 (en) | 1997-04-04 | 1998-10-08 | Henkel Kgaa | Activators for peroxygen compounds in detergents and cleaning agents |
| DE19732749A1 (en) | 1997-07-30 | 1999-02-04 | Henkel Kgaa | Detergent containing glucanase |
| DE19732750A1 (en) | 1997-07-30 | 1999-02-04 | Henkel Kgaa | Cleaning agent containing glucanase for hard surfaces |
| DE19732751A1 (en) | 1997-07-30 | 1999-02-04 | Henkel Kgaa | New Bacillus beta glucanase |
| DE19824705A1 (en) | 1998-06-03 | 1999-12-09 | Henkel Kgaa | Detergents and cleaning agents containing amylase and protease |
| DE19914811A1 (en) | 1999-03-31 | 2000-10-05 | Henkel Kgaa | Detergent compositions containing a bleaching agent include a combination of a cyanomethyl ammonium salt bleach activator and an enzyme |
| DE10058645A1 (en) | 2000-11-25 | 2002-05-29 | Clariant Gmbh | Use of cyclic sugar ketones as catalysts for peroxygen compounds |
| DE10102248A1 (en) | 2001-01-19 | 2002-07-25 | Clariant Gmbh | Use of transition metal complexes with oxime ligands as bleach catalysts |
| CN1575308B (en) | 2001-10-22 | 2010-04-28 | 汉高两合股份公司 | Cotton active, dirt removing urethane-based polymers |
| DE102005026544A1 (en) | 2005-06-08 | 2006-12-14 | Henkel Kgaa | Reinforcement of cleaning performance of detergents by polymer |
| DE102005039580A1 (en) | 2005-08-19 | 2007-02-22 | Henkel Kgaa | Color protecting detergent |
| DE102006012018B3 (en) | 2006-03-14 | 2007-11-15 | Henkel Kgaa | Color protecting detergent |
| DE102007023874A1 (en) | 2007-05-21 | 2008-11-27 | Henkel Ag & Co. Kgaa | Use of polycarbonate, polyurethane and/or polyurea polyorganosiloxane compounds or their acid addition compound and (1,3)-dioxolan-2-one or (1,3)-diazepan-2-one compound and polymer for fixing fragrance on hard and/or soft surfaces |
| DE102007023870A1 (en) | 2007-05-21 | 2008-11-27 | Henkel Ag & Co. Kgaa | Use of an active agent containing (1,3)dioxolan-2-one compound or (1,3)diazepan-2-one compound, and a polymer, for strengthening the primarily washing power of the detergent in the washing of textile oil- and/or fat-containing dirt |
| DE102007038456A1 (en) | 2007-08-14 | 2009-02-19 | Henkel Ag & Co. Kgaa | Use of polycarbonate, polyurethane and/or polyurea-polyorganosiloxane compounds or their acid addition compounds and/or salts to improve the cleaning efficiency of laundry detergents during washing textiles |
| DE102007038453A1 (en) | 2007-08-14 | 2009-02-19 | Henkel Ag & Co. Kgaa | Use of polycarbonate, polyurethane and/or polyurea polyorganosiloxane compounds or their acid addition compound and (1,3)-dioxolan-2-one or (1,3)-diazepan-2-one compound and polymer for fixing fragrance on hard and/or soft surfaces |
| DE102007023827A1 (en) | 2007-05-21 | 2008-11-27 | Henkel Ag & Co. Kgaa | Use of polycarbonate, polyurethane and/or polyurea-polyorganosiloxane compounds or their acid addition compounds and/or salts to improve the cleaning efficiency of laundry detergents during washing textiles |
| DE102007016391A1 (en) | 2007-04-03 | 2008-10-09 | Henkel Ag & Co. Kgaa | Detergent or cleaning agent for preventing transfer of textile color of colored textiles from uncolored or different colored textiles in laundry, particularly in tenside containing aqueous solution, has color transfer inhibitor |
| DE102007016383A1 (en) | 2007-04-03 | 2008-10-09 | Henkel Ag & Co. Kgaa | Use of (1,3)dioxolan-2-one or (1,3)-diazepan-2-one compound for the fixation of fragrances on hard and/or smooth surfaces e.g. textiles |
| DE102011010818A1 (en) | 2011-02-10 | 2012-08-16 | Clariant International Ltd. | Use of transition metal complexes as bleaching catalysts in detergents and cleaners |
| MX338995B (en) | 2012-02-21 | 2016-05-09 | Henkel Ag & Co Kgaa | Color protection detergent. |
| DE102012220241A1 (en) | 2012-11-07 | 2014-05-08 | Henkel Ag & Co. Kgaa | Polymers with polar groups as soil release assets |
| ES2562109T3 (en) | 2013-05-22 | 2016-03-02 | Henkel Ag&Co. Kgaa | Detergent with color protection |
| EP3209760B1 (en) | 2014-10-20 | 2018-08-01 | Henkel AG & Co. KGaA | Colour protection detergent |
| US20170233682A1 (en) | 2014-10-21 | 2017-08-17 | Henkel Ag & Co. Kgaa | Anti-grey detergent |
| EP3680317B1 (en) | 2019-01-11 | 2022-08-24 | Henkel AG & Co. KGaA | Colour protection detergents |
| EP4105306A1 (en) | 2021-06-15 | 2022-12-21 | Henkel AG & Co. KGaA | Super-concentrated dilutable manual dishwashing detergent composition |
| EP4105305A1 (en) | 2021-06-15 | 2022-12-21 | Henkel AG & Co. KGaA | Stable viscous dilutable cleaning composition |
| EP4186969A1 (en) | 2021-11-26 | 2023-05-31 | Henkel AG & Co. KGaA | Super-concentrated dilutable powder for dishwashing application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1517891A (en) * | 1922-09-01 | 1924-12-02 | Ind Waste Products Corp | Powdered sodium silicate and process of preparing the same |
| US3838192A (en) * | 1971-10-28 | 1974-09-24 | Huber Corp J M | Production of alkali metal polysilicates |
| US4586177A (en) * | 1983-11-15 | 1986-04-29 | M/A-Com Dcc, Inc. | Integrated narrowband and wideband TDMA networks |
| DE3423945A1 (en) * | 1984-06-29 | 1986-01-09 | Henkel KGaA, 4000 Düsseldorf | METHOD AND DEVICE FOR THE CONTINUOUS HYDROTHERMAL PRODUCTION OF SODIUM SILICATE SOLUTIONS |
| DE3718350A1 (en) * | 1987-06-01 | 1988-12-22 | Hoechst Ag | METHOD FOR PRODUCING CRYSTALLINE SODIUM SILICATES WITH LAYER STRUCTURE |
-
1990
- 1990-09-11 CA CA002025073A patent/CA2025073C/en not_active Expired - Fee Related
- 1990-10-08 EP EP90710027A patent/EP0425427B1/en not_active Expired - Lifetime
- 1990-10-08 DK DK90710027.5T patent/DK0425427T3/en active
- 1990-10-08 ES ES90710027T patent/ES2047897T3/en not_active Expired - Lifetime
- 1990-10-08 DE DE4031849A patent/DE4031849A1/en not_active Withdrawn
- 1990-10-23 AR AR90318163A patent/AR243478A1/en active
- 1990-10-23 TR TR90/1034A patent/TR24995A/en unknown
- 1990-10-23 KR KR1019900016931A patent/KR0143991B1/en not_active IP Right Cessation
- 1990-10-23 FI FI905210A patent/FI905210A0/en not_active IP Right Cessation
- 1990-10-23 AR AR90318162A patent/AR247369A1/en active
- 1990-10-24 JP JP2284528A patent/JPH0669891B2/en not_active Expired - Lifetime
- 1990-10-24 BR BR909005386A patent/BR9005386A/en not_active IP Right Cessation
- 1990-10-24 NO NO90904604A patent/NO904604L/en unknown
- 1990-10-24 SI SI9012000A patent/SI9012000A/en unknown
- 1990-10-24 RU SU904831297A patent/RU2039701C1/en active
- 1990-10-24 PT PT95664A patent/PT95664A/en not_active Application Discontinuation
-
1992
- 1992-11-06 HR HRP-2000/90A patent/HRP921199B1/en not_active IP Right Cessation
-
1993
- 1993-05-04 LV LVP-93-278A patent/LV10764B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| LV10764A (en) | 1995-08-20 |
| NO904604D0 (en) | 1990-10-24 |
| DE4031849A1 (en) | 1991-05-02 |
| KR910007804A (en) | 1991-05-30 |
| FI905210A0 (en) | 1990-10-23 |
| RU2039701C1 (en) | 1995-07-20 |
| NO904604L (en) | 1991-04-26 |
| JPH0669891B2 (en) | 1994-09-07 |
| CA2025073A1 (en) | 1991-04-26 |
| EP0425427A2 (en) | 1991-05-02 |
| LV10764B (en) | 1995-12-20 |
| HRP921199B1 (en) | 1998-04-30 |
| DK0425427T3 (en) | 1994-02-21 |
| AR243478A1 (en) | 1993-08-31 |
| EP0425427A3 (en) | 1992-03-11 |
| PT95664A (en) | 1991-09-13 |
| AR247369A1 (en) | 1994-12-29 |
| HRP921199A2 (en) | 1995-08-31 |
| TR24995A (en) | 1992-09-01 |
| CA2025073C (en) | 1995-07-18 |
| BR9005386A (en) | 1991-09-17 |
| ES2047897T3 (en) | 1994-03-01 |
| EP0425427B1 (en) | 1993-12-15 |
| KR0143991B1 (en) | 1998-07-15 |
| JPH03170320A (en) | 1991-07-23 |
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