LT3003B - Process for preparing powdered 4A type ceolite. - Google Patents
Process for preparing powdered 4A type ceolite. Download PDFInfo
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- LT3003B LT3003B LTIP209A LTIP209A LT3003B LT 3003 B LT3003 B LT 3003B LT IP209 A LTIP209 A LT IP209A LT IP209 A LTIP209 A LT IP209A LT 3003 B LT3003 B LT 3003B
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- 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
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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
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
- C01B33/2807—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures
- C01B33/2815—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L)
- C01B33/2823—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L) from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Detergent Compositions (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Description
Išradimas liečia labai· dispersiškus kristalų pavidalo 4A tipo ceolitų miltelius su iš anksto numatyta granulometrine sudėtimi (apibūdinama d50 reikšme), mažesne nei 3 p.m, taip pat jų gavimo būdą ir ' panaudojimą vietoj fosfato skystuose detergentuos’e bei skalavimo priemonėse arba prieduose ..prie -'keraminių glazūrų ir sukepusių masių (fritų).The present invention relates to highly dispersible crystalline zeolite type 4A powders with a predetermined granulometric composition (defined as d 50 ) of less than 3 µm, as well as their preparation and use in place of phosphate in liquid detergents and detergents or additives. at -'ceramic glazes and sintered masses (frits).
VFR paraiškoje Nr.2856209, kl. CO1B 33/28, 1982 m.VFR Application No. 2856209, Cl. CO1B 33/28, 1982.
aprašytas labai dispersiškų ,4A tipo ceolitų gavimo būdas, artimiausias šiam išradimui. Norint gauti granųlometrinę sudėtą, kurios d50 reikšmė mažesnė nei 3 μιη, reagentai viehas su kitu sumaišomi ir išpurškiami panaudojant mechanines priemones, pavyzdžiui, tūtas.describes a process for preparing highly dispersible zeolites of type 4A closest to the present invention. To obtain a granulometric composition with a d 50 value less than 3 μιη, the reagents are mixed and sprayed using mechanical means such as nozzles.
Tam, kad neūžs’iterštų tūtos, savaime susidarius nuosėdoms reaguojant natrio aliuminato tirpalui su skysto stiklo tirpalu, į abu tirpalus įvedamas kalio oksidas) kuris stabdo nusėdimą.' Šį būdą geriau .realizuoti dviem stadijomis, t.y. pirma abu tirpalai reaguoja, . esant žemai temperatūrai, po to gautam produktui leidžiama išsikristalizuoti temperatūrą pakėlus. Gaunami šiuo būdu molekuliniai sietai gali detergentuose kalcį surišti kiekiu apie 160 mg/g ceolito.In order to keep the nozzles free from contamination, the solution is spontaneously formed by reacting a solution of sodium aluminate with a liquid glass solution in which potassium oxide is added to both solutions, which prevents deposition. ' This method is better realized in two stages, i.e. first both solutions react, -. at low temperature, the resulting product is then allowed to crystallize by raising the temperature. The resulting molecular sieves can bind calcium in detergents in an amount of about 160 mg / g of zeolite.
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Šio išradimo tikslas - pašalinti minėtų būdų trūkumus ir sukurti paprastą būdą gauti labai dispersiškus kristalinius 4A tipo ceolitus, gerai·surišančius kalcį. Šiame būde naudojamos tokios pigios medžiagos kaip skaidrus šarmas, atsirandantis gaunant aliuminio hidroksidus Bajerio metodu, ir skystas techninis stiklas (natrio silikatas). Siūlomu būdu gauti ceolito milteliai turi būti kristalų pavidalo, vienalyčiai fazinio būvio požiūriu ir neturėti grito. Be to, naujo būdo dėka jie turi pasižymėti tiksliai reguliuojama granulometrine sudėtimi.The object of the present invention is to overcome the drawbacks of the above mentioned methods and to provide a simple way to obtain highly dispersed calcium-bound calcium zeolites of type 4A. This process uses inexpensive materials such as clear alkali resulting from the production of aluminum hydroxides by the Bavarian method and liquid technical glass (sodium silicate). The zeolite powder obtained in the proposed manner must be in the form of crystals, homogeneous in terms of phase and free from grit. In addition, due to the new method they have to have a precisely controlled granulometry.
Siūlomas būdas remiasi tuo, kad natrio aliuminato tirpalas (I ' tirpalas) savaime reaguoja su natrio silikato tirpalu (II tirpalu) ir taip susidaro amorfinės nuosėdos, priklausomai nuo temperatūros- lėtai.The proposed process is based on the fact that the sodium aluminate solution (solution I ') spontaneously reacts with the sodium silicate solution (solution II) to form an amorphous precipitate slowly depending on the temperature.
virstančios į kristalinį miltelių pavidalo* ceolitą.· *converting to crystalline powder * zeolite. *
Brendimo procesą, t. y. produkto perėjimą iš amorfinio būvio į. kristalinį, lydi būdingi persikristaližavimui reiškiniai.Maturation process, vol. y. product transition from amorphous to. crystalline, accompanied by characteristic phenomena of recrystallization.
Pagal siūlomą būdą, kristalizacijos procesas veikiamas, .10 sukuriant mikroaglomera.tus. Tai užtikrina «gaunamo ceolito miltelių ^smulkų dispersiškumą. Mikroaglomeratai , gaunami, deramai reguliuojant I ir II tirpalų koncentraciją, kartu purškiant 1 nustatyto dydžio lašeliais. Šie smulkios dispersijos lašeliai, turintys- nusodinamas kietas daleles, sąlygoja tai, kad susidaro vienalyčiai smulkaus dispersiškumo ceolito milteliai.According to the proposed method, the crystallization process is operated by .10 creating a microagglomer.tus. This ensures a fine dispersion of the resulting zeolite powder. Microagglomerates obtained by the appropriate adjustment of the concentration of solutions I and II, co-sprayed with 1 droplet size. These finely dispersed droplets having - precipitated solid particles, is determined that is formed in small homogeneous dispersibility of zeolite powders.
Siūlomas būdas pranašesnis todėl, kad ceolito· miltelių dalelių stambumą apsprendžia nusodinimo - sąlygos, ir jis ' galutinai nustatomas brendimo proceso metu.The proposed method is advantageous because the bulk size of the zeolite powder particles is determined by the deposition conditions and is finally determined during the maturation process.
» *»*
Vietoj I tirpalo, turinčio Na2O ir A1*2O3 galima naudoti bet kokį tirpalą,, turintį nė. mažiau 20 g/1 Na2O ir ne mažiau 130 g/1- Α12Ω3, d tinkamas molinis santykisInstead of solution I containing Na 2 O and A1 * 2 O 3, any solution containing none can be used. less than 20 g / l Na 2 O and not less than 130 g / l Α 1 2 Ω 3 , d an appropriate molar ratio
Na2O ’ A12O3 sudaro' 1,3-4,0, tinkamiausias 1,40-1-,56.Na 2 O 'A1 2 O 3 forms' 1,3-4,0, most preferably 1,40-1-, 56.
I · tirpalu dažniausiai vartoja skaidrų šarmą, susidarantį gaminant Bajerio būdu aliuminio hidroksidą. Esant būtinybei, šarmas skiedžiamas iki · reikalingos koncentracijos.The most common solution used in the solution is the clear alkali formed by the Bavarian method of producing aluminum hydroxide. If necessary, dilute the alkali to the required concentration.
II tirpalu, turinčiu Na2O ir Si02, tikslinga naudoti skiestą natrio silikato tirpalą, turintį ne mažiau' 34,7 g/1 Na2O ir ne mažiau 119 g/1 Si02, o molinis santykis Na2O : SiO2 - 0,25-1,0. Daugiausia tai standartinis techninis skysto stiklo 1,36 kg/1 tankio tirpalas, kuris skiedžiamas vandeniu.For solution II containing Na 2 O and SiO 2 , it is appropriate to use dilute sodium silicate solution containing not less than '34.7 g / l Na 2 O and not less than 119 g / l SiO 2 and a molar ratio of Na 2 O: SiO 2 0.25-1.0. It is mainly a standard technical solution of liquid glass at a density of 1.36 kg / l and diluted with water.
Skiedinių serijos ruošimui tikslingiau naudoti vahdens Kondensatą .arba dejonizuotą vandenį.For preparation of mortar series it is more appropriate to use condensate of vahdens or deionized water.
Nusodinimo reakciją tikslinga vykdyti temperatūros intervale .tarp 70 ir S0° Č, geriausiai prie 75° C. Svarbų šiam metodui, reagentų purškimą geriau atlikti viena ar keliomis tūtomis,,It is expedient to carry out the precipitation reaction in a temperature range of between 70 and S0 ° C, preferably at 75 ° C.
P.agal vieną iš siūlomo būdo .variantą I ' tirpalas intensyviai maigomas, palaikant tinkamą nusodinimui temperatūrą,. o II tirpalas, faktiškai turintis tokią pat temperatūrą, 0,5-5 vai.· paduodamas per vieną ar kelias tūtas; tinkamiausias laikas -- 2~3 vai. Tinka visokios tūtos, kurios, esant reikalingam skysčio debitui, įgalina purkšti 'skiedinį vidutiniškai apie 0,05 mm skersmens lašeliais. Čia galima ‘naudoti tiek tūtas, skirtas tik skiediniui purkšti, tiek ir tūtas, kurios, esant reikalingam skysčio debitui, leidžia purkšti skiedinį vidutiniškai apie 0,05 mm skersmens lašeliais-. Galima naudoti · tūtas, purŠkiančias tik patį tirpalą, ir tūtas, kartu purŠkiančias ir pagalbinę terpę. Be to, tirpalą smulkiai purkšti -galima· ir panaudojant ultragarsą. Ta’čau tikslingiau naudoti tūtas, vienu metu purŠkiančias du komponentus, t. y. tirpalą, ir pagalbinę terpę - suspaustą orą. Purškiamą skiedinį geriausiai nukreipti į įdubimo, atsirandančio intensyviai maišant pradinį tirpalą, zoną.According to one embodiment of the invention, the solution I 'is vigorously agitated at a temperature suitable for precipitation. o Solution II, having the same temperature, 0.5 to 5 hours · fed through one or more nozzles; best time - 2 ~ 3 hours. Suitable for all nozzles which, at the required fluid flow rate, allow the mortar to be sprayed with an average droplet diameter of about 0.05 mm. Both mortar-only nozzles and nozzles which, at the required fluid flow rate, allow the mortar to be sprayed with an average droplet diameter of about 0.05 mm can be used. Nozzles that spray only the solution itself and nozzles that simultaneously spray with auxiliary media may be used. In addition, fine spraying of the solution is also possible with ultrasound. However, it is more appropriate to use nozzles that simultaneously spray two components, y. solution, and auxiliary medium, compressed air. Spray mortar is best directed to the depression area resulting from vigorous mixing of the stock solution.
Pagal kitą, pranašesnį išradimo realizavimo variantą, I tirpalas, maišomas taip, kad tekėdamas per tinkamą įtaisą, sudarytų plėvelę, į kurią per tūtą purškiamas II tirpalas.According to another preferred embodiment of the invention, solution I is agitated so as to form, through a suitable device, a film into which solution II is sprayed through the nozzle.
Naudojant siūlomą būdą, nepridedant kalio, paprasčiau gaunama molekulinio sieto smulkios dispersijos suspensija. Kadangi išeities tirpalas intensyviai maišomas, į purškiamo tirpalo zoną nuolat paduodamas šviežias, dar pilnai nesureagavęs tirpalas. Tūtos neužteršiamos, nes naudojama tik viena tūta.The proposed process simplifies the preparation of a fine sieve suspension of the molecular sieve without the addition of potassium. Due to the vigorous stirring of the stock solution, a fresh solution which has not yet fully reacted is continuously fed into the spray solution area. Nozzles are not contaminated because only one nozzle is used.
Tolimesnis brendimo procesas tęsiamas 3- 20 vai.Further maturation is continued for 3 to 20 hours.
* intensyviai maišant prie 70 - r80°C temperatūros, geriausiai apie 75°· C. Šis procesas gali būti vykdomas pačiame reaktoriuje arba atskirame brandinimo bake.* Intense stirring at 70 - R 80 ° C, preferably about 75 ° ° C. This process can be carried out in the reactor or in a separate maturation tank.
5.Pagal siūlomą būdą, išradimo tikslas pagrindinai l5. According to the method of the invention, the object of the invention is essentially l
pasiekiamas . griežtai· prisilaikant pastovios temperatūros,’t.y. reakcijos·temperatūra’ turi svyruoti ribose, ne didesnėse kaip ±2°C. , Todėl šilumą, pakeliančią reakcijos temperatūrą daugiau nei 6°C,reachable. strictly · at a constant temperature, i.e. the reaction temperature must be within ± 2 ° C. Therefore heat raising the reaction temperature above 6 ° C,
10. reikia nuvesti. Tai labai svarbu, nes virš 83°C labai išauga galimybė^ susidaryti sodalitui. Nors šis mineralas yra vienas iš pagrindinių ceolito · 4A struktūrinių elementų, pats jis neturi jokios jonų mainų galios ir jam sūsįdarant, nežiūrint į aukštą kpiatalingumą, nepadidėja gebėjimas surišti kalcį.10. need to be led away. This is very important because above 83 ° C the likelihood of formation of sodalite is greatly increased. Although one of the major structural elements of zeolite · 4A, this mineral has no ion-exchange capacity and does not increase calcium-binding capacity despite its high cationic capacity.
ir, esant, klampumui, tai, . kadand, in the case of viscosity,. that
Pasiekus reikalingą, granulometrinę sudėtį, kristalų pavidalo produktas filtruojant atskiriamas nuo nuovarvų, išplaunamas ir, priklausomai nuo numatomos paskirties, žinomu būdu perdirbamas. Miltelių pavidalo 4A tipo ceolitas, gautas siūlomu būdu · ir atitinkantis išradimo · užduotį, ypač <panaudotinas skystuose dėtergentuose ir skalavimo priemonėse atitinkamam prėparizuotos priemonės faktiškai nelinkęs nusėsti. Nežiūrint skiedinio purškimui naudojamos tūtos su maža {mažiau nei 1 mm skersmens} anga, gali susidaryti stambūs lašai, jei smulkūs lašeliai susijungs. Tokie lašai turi tiek nusodinamos kietos medžiagos, kad, pradėjus liestis jiems su intensyviai maišomu pradiniu· tirpalu, susidaro stambi amorfinė dalelė. Iš jos brendimo procese susidaro kristalai, kurie iš tikrųjų yra kelių pradinių smulkių kristalitų sąaugos. Pastarosios. ir sudaro nepageidaujamą ceolito gritų dalį.·Once the required granulometry is achieved, the crystalline product is filtered off from the precipitate, washed and, depending on its intended use, recycled in a known manner. The powdered zeolite type 4A obtained according to the present invention and in accordance with the object of the invention is particularly suitable for use in liquid loading agents and rinse aids and is not prone to precipitation of the corresponding paraffinic agent. Despite the use of mortar nozzles with small openings (less than 1 mm diameter), large drops can form if small droplets are combined. Such drops contain a solid that is so precipitated that a large amorphous particle is formed upon contact with the vigorously agitated stock solution. It produces crystals during the maturation process, which are in fact a few small crystallite deposits. The latter. and forms an undesirable part of the Zeolite grit. ·
Pagal vi-eną iš siūlomo būdo variantų^ šie kristalitai malami rutuliniame malūne su maišiklįu. Malti galima po dozavimo arba tuoj praėjus brandinimo laikui.According to one of the embodiments of the present invention, these crystallites are milled in a ball mill with a mixer. Grinding can be carried out after dosing or immediately after maturation.
.5 . 5
Toliau siūlomu būdu gautus, ceolito. miltelius tikslinga įmaišyti į keramines mases, pavyzdžiui, tam, kad paveiktume glazūros ar sukepusių masių spalvą.The following is the zeolite obtained in the proposed manner. it is expedient to mix the powder into the ceramic masses, for example, to influence the color of the glaze or sintered masses.
Toliau siūlomo būdo esmė paaiškinama pavyzdžiais.The essence of the proposed method is explained below by examples.
pavyzdys.example.
į 200 1 talpos maišymo katilą pakraunama 90. 1 skiesto skaidraus, susidariusio naudojant Bajerio metodą, šarmo,' kuriame yra 150 g/1 Na2O ir 125 g/1 A12O3 (I tirpalas), ir jis, kaitinamas iki 75°C temperatūros. Toks pat kiekis atskiesto natrio silikato tirpalo, turinčio 34,7 g/l· Na2O ir 119,3 g/1 SiO2 (II tirpalo), irgi įkaitinto iki 75°C, tūta paduodama į zoną, kur yra didžiausias greitaeigiu maišytuvu intensyviai maišomo skaidraus šarmo tekėjimo greitis ^sukimosi greitis 3000 min-1) . Purškimui panaudota plokščios čiurkšlės ·-’ * - · .90 liters of 1 dilute clear alkali containing 150 g / l Na 2 O and 125 g / l Al 2 O 3 (solution I) are added to a 200 L mixing boiler and heated to 75 ° C. An equal volume of dilute sodium silicate solution containing 34.7 g / l · Na 2 O and 119.3 g / l SiO 2 (solution II), also heated to 75 ° C, is fed to the zone where it is highest by means of a high speed mixer flow rate of vigorously agitated clear alkali ^ rotation speed 3000 min -1 ). Flat jet · - '* - · was used for spraying.
tūta (Firma Lechler, tipas 652.404.17). Dozavimo laikas • *nozzle (Firm Lechler, type 652.404.17). Dosing time • *
- 2,5 vai.- 2.5 or.
Liečiantis II tirpalui su I tirpalu savaime susidaro * · amorfiškas kietas kūnas, kuris, stechiometrijos požiūriu/ jau atitiko pageidaujamam 4A tipo ceolitui, tačiau jo kristalingumas dar buvo nepakankamas. Todėl jis buvo dar’ 4 vai. brandinamas. Subrandinus, filtruojant nuo nuovarvų atskirtas, nusėdęs produktas turėjo tik Na2O ir SiO2, tačiau nuo SiO2 jis buvo praktiškai laisvas ir po kelių plovimo stadijų produktas išdžiovinamas.Contacting solution II with solution I spontaneously produces a * · amorphous solid which, from a stoichiometric point of view, already corresponded to the desired type 4A zeolite, but its crystallinity was still insufficient. Therefore he was still '4 hours old. maturing. After maturation, the product separated from the fat by filtration had only Na 2 O and SiO 2 , but was practically free from SiO 2 and after several washing steps the product was dried.
Gauta produkto granulometrinė sudėtis, nustatyta sedigrafo pagalba ir išreikšta d50 reikšme, lygia 2, 9 μιη.The granulometric composition of the product, determined by sedigraphy and expressed as a value of d 50 of 2, 9 μιη is obtained.
Šio pavyzdžio produktas gali surišti kalcį' kiekiu 167 mg CaO/g ceolito.The product of this example can bind calcium in an amount of 167 mg CaO / g zeolite.
pavyzdys,.example,.
Bandymui panaudota aparatūra ir procedūra, analogiška 1 pavyzdžiui su tuo skirtumu, kad pridedama tik 90%. II.Apparatus and procedure analogous to Example 1 were used for the test, except that only 90% was added. II.
tirpalo, nurodyto 1 pavyzdyje. Produkto brandinimo laikas 7'20 valandų.of the solution given in Example 1. Product ripening time 7'20 hours.
. Ir šiuo atveju nufiltruota, išplauta ir išdžiovinta medžiaga buvo kristalinis 4A tipo ce&litas, kurio d5Q lygus 2,0 pm.. Here again, the filtered, washed, and dried material was crystalline type 4A zeolite with a d 5Q of 2.0 µm.
Ši medžiaga gali surišti kalci kiekiu - 170 mg CaO/g ceolito.This substance can bind to calcium - 170 mg CaO / g zeolite.
3 pavyzdys.Example 3.
Elgtasi analogiškai 1 pavyzdžiui su tuo skirtumu, kad pakrauta 140% I tirpalo’ kiekio, nurodyto 1 pavyzdyje, taip pat atskiesto.Analogous to Example 1, the same procedure was followed except that 140% of the amount of Solution I in Example 1 was also diluted.
''
Gauta kristalinė medžiaga, kurios d50 =1,5 pm.A crystalline material having a d 50 = 1.5 µm is obtained.
ii
Gebėjimas surišti kalcį šiame pavyzdyje -.161 mg CaO/g ceolito.The ability to bind calcium in this example is -.161 mg CaO / g zeolite.
* pavyzdys.* example.
Elgtasi analogiškai 1 pavyzdžiui su tuo skirtumu, kad II tirpalas purkštas panaudojant dviejų komponentų tūtą (Firma Šlik, tipas 772-K-I). Šiuo atveju suspaustas'iki · 6 barų -oras buvo pagalbine terpe, sudariusia smulkius lašelius. Po 5 valandų brandinimo gautas 4A . tipo ceolitas, kurio d50 = 2,9 pm. Gebėjimas sur.išti kalcį buvo'163 mg CaO/g ceolito.The same procedure as Example 1 was followed except that Solution II was sprayed using a two-component nozzle (Firma Šlik, type 772-KI). In this case, the compressed to 6 bar was an auxiliary medium that formed fine droplets. After 5 hours of maturation, 4A was obtained. type zeolite with d 50 = 2.9 pm. The ability to bind calcium was' 163 mg CaO / g zeolite.
pavyzdys (palyginamasis pavyzdys).example (comparative example).
• 7• 7
Elgtasi analogiškai 1 pavyzdžiui, su skirtumu, kad I ir II tirpalų' temperatūra buvo 85°C. Praėjus dozavimo ir brandinimo periodams gautas kristalinis produktas, kuris be ceolito, kurio. -d50 2,8 ųm, turėjo ęlar ir nepageidaujamą dali, sčdalito·.. Medžiagos gebėjimas surišti kalcį - 110 mg CaO/g ceolito.The procedure of Example 1 was followed analogously, except that Solutions I and II had a temperature of 85 ° C. After dosing and maturation, a crystalline product was obtained which, in the absence of zeolite. -d 50 2.8 um, had lar and undesirable part, sicdalite · .. The ability of the substance to bind calcium is 110 mg CaO / g zeolite.
Claims (4)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH135089 | 1989-04-10 | ||
| SU904743562A RU2005692C1 (en) | 1989-04-10 | 1990-04-09 | Process for preparing powdery 4a type zeolite |
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| Publication Number | Publication Date |
|---|---|
| LTIP209A LTIP209A (en) | 1994-03-25 |
| LT3003B true LT3003B (en) | 1994-08-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| LTIP209A LT3003B (en) | 1989-04-10 | 1992-08-28 | Process for preparing powdered 4A type ceolite. |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0392400B1 (en) |
| DD (1) | DD292432A5 (en) |
| DE (1) | DE59010399D1 (en) |
| DK (1) | DK0392400T3 (en) |
| GE (1) | GEP19970903B (en) |
| HU (1) | HU207969B (en) |
| LT (1) | LT3003B (en) |
| LV (1) | LV10070B (en) |
| RU (1) | RU2005692C1 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0490011B1 (en) * | 1990-12-14 | 1994-09-07 | Foret, S.A. | A process to obtain zeolite 4A starting from bauxite |
| DE4128426A1 (en) * | 1991-08-27 | 1993-03-04 | Henkel Kgaa | LIQUID DETERGENT WITH ZEOLITE |
| WO1994000545A1 (en) * | 1992-06-25 | 1994-01-06 | Unilever N.V. | Machine dishwashing composition |
| FR2804103B1 (en) * | 2000-01-26 | 2002-03-01 | Commissariat Energie Atomique | PROCESS FOR THE CONDITIONING OF NEPHELINE SODIUM EFFLUENTS |
| JP2003012322A (en) * | 2001-06-29 | 2003-01-15 | Furukawa Electric Co Ltd:The | Method for utilizing waste discharged from aluminum manufacturing factory or optical fiber manufacturing factory as zero emission type utilization and manufactured zeolite |
| NL1033269C2 (en) * | 2007-01-23 | 2008-07-24 | Ertecee B V | Aqueous gel-forming composition, e.g. as fire retardant coating to substrate, comprises aluminosilicate and organic liquid, where aluminosilicate comprises alkali metal aluminate and alkali metal silicate each having specified molar ratio |
| EP2108022A2 (en) * | 2007-01-23 | 2009-10-14 | PQ Silicas UK Limited | Aqueous compositions, precursor systems and application systems |
| CN100577565C (en) * | 2007-08-03 | 2010-01-06 | 中国铝业股份有限公司 | Method for producing 4A zeolite |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2856209A1 (en) | 1978-12-27 | 1980-07-10 | Degussa | Continuous finely divided aluminosilicate prodn. - from aq. silicate and aluminate solns. in spray device, useful, in cleaning compsns. |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2856278A1 (en) * | 1978-12-27 | 1980-07-10 | Degussa | METHOD FOR PRODUCING FINE-PARTICLE SODIUM ALUMINUM SILICATES |
| FR2454997A1 (en) * | 1979-04-24 | 1980-11-21 | Ugine Kuhlmann | ZEOLITE CRYSTALLIZATION DURING INDUSTRIAL MANUFACTURING PROCESSES |
-
1990
- 1990-03-13 DD DD90338644A patent/DD292432A5/en not_active IP Right Cessation
- 1990-04-06 DK DK90106700.9T patent/DK0392400T3/en not_active Application Discontinuation
- 1990-04-06 DE DE59010399T patent/DE59010399D1/en not_active Expired - Fee Related
- 1990-04-06 EP EP90106700A patent/EP0392400B1/en not_active Expired - Lifetime
- 1990-04-09 HU HU902124A patent/HU207969B/en not_active IP Right Cessation
- 1990-04-09 RU SU904743562A patent/RU2005692C1/en active
-
1992
- 1992-08-10 LV LVP-92-90A patent/LV10070B/en unknown
- 1992-08-28 LT LTIP209A patent/LT3003B/en not_active IP Right Cessation
- 1992-09-03 GE GEAP1992160A patent/GEP19970903B/en unknown
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2856209A1 (en) | 1978-12-27 | 1980-07-10 | Degussa | Continuous finely divided aluminosilicate prodn. - from aq. silicate and aluminate solns. in spray device, useful, in cleaning compsns. |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0392400A2 (en) | 1990-10-17 |
| DK0392400T3 (en) | 1996-07-29 |
| HU207969B (en) | 1993-07-28 |
| HU902124D0 (en) | 1990-07-28 |
| LV10070A (en) | 1994-05-10 |
| DE59010399D1 (en) | 1996-08-08 |
| LV10070B (en) | 1995-02-20 |
| GEP19970903B (en) | 1997-03-24 |
| DD292432A5 (en) | 1991-08-01 |
| EP0392400B1 (en) | 1996-07-03 |
| EP0392400A3 (en) | 1991-04-10 |
| HUT53841A (en) | 1990-12-28 |
| RU2005692C1 (en) | 1994-01-15 |
| LTIP209A (en) | 1994-03-25 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PC9A | Transfer of patents |
Free format text: 20010904 * MARTINSWERK GMBH,DE |
|
| MM9A | Lapsed patents |
Effective date: 20020828 |