NO794092L - PROCEDURE FOR SEMI-CONTINUOUS PREPARATION OF ZEOLITE A - Google Patents
PROCEDURE FOR SEMI-CONTINUOUS PREPARATION OF ZEOLITE AInfo
- Publication number
- NO794092L NO794092L NO794092A NO794092A NO794092L NO 794092 L NO794092 L NO 794092L NO 794092 A NO794092 A NO 794092A NO 794092 A NO794092 A NO 794092A NO 794092 L NO794092 L NO 794092L
- Authority
- NO
- Norway
- Prior art keywords
- solution
- zeolite
- silicon
- sodium silicate
- aluminate
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 19
- 238000002360 preparation method Methods 0.000 title description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 31
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 27
- 239000010457 zeolite Substances 0.000 claims description 27
- 229910021536 Zeolite Inorganic materials 0.000 claims description 26
- 239000004115 Sodium Silicate Substances 0.000 claims description 19
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 19
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 18
- -1 Ca++ ions Chemical class 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- 239000011575 calcium Substances 0.000 claims description 9
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 8
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 7
- 230000014759 maintenance of location Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000010924 continuous production Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 2
- 229910000676 Si alloy Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910021471 metal-silicon alloy Inorganic materials 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 238000010306 acid treatment Methods 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 235000019351 sodium silicates Nutrition 0.000 claims 1
- 230000002269 spontaneous effect Effects 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 23
- 239000000047 product Substances 0.000 description 12
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000011734 sodium Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical class [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241000288724 Talpa europaea Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 125000004436 sodium atom Chemical group 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000000209 wet digestion Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Description
Foreliggende oppfinnelse angår fremstilling av zeolitt A ved en halv-kontinuerlig prosess. The present invention relates to the production of zeolite A by a semi-continuous process.
Anvendelsen av zeolitter er basert på de velkjente egenskaper som kation byttere som f.eks. er beskrevet i "Comprehensive treatise on inorganic and. theoretical; chem-istry" ved J.W.Mellor, vol. VI, del 2, Longman Editors 1925, side 575-579, og spesielt på muligheten for å utbytte na-, triumatomer mot kalsiumioner. The use of zeolites is based on the well-known properties as cation exchangers such as e.g. is described in "Comprehensive treatise on inorganic and. theoretical; chemistry" by J.W.Mellor, vol. VI, part 2, Longman Editors 1925, pages 575-579, and especially on the possibility of exchanging sodium atoms for calcium ions.
I IDen hyppigst benyttede zeolitt er- zeolitt A med fqrmelen Na20, A^O^, 2 SiOg/x E^ O , hvori x kan variere fr,a 1 til 8 avhengig av produktets tørkebetingelser, den me|st hyppig benyttede verdi er x = 4 til 5. In ID, the most frequently used zeolite is zeolite A with the formula Na20, A^O^, 2 SiOg/x E^ O , where x can vary from 1 to 8 depending on the product's drying conditions, the most frequently used value is x = 4 to 5.
For å fremme Ca<++>'utbyttingsegenskapene og _selektiv-itjeten for zeolitten bør denne være så ren som mulig og således være grundig krystallisert, hvorved enhver urenhet enten er inaktiv eller mindre selektiv. In order to promote the Ca<++>' recovery properties and the selectivity of the zeolite, this should be as pure as possible and thus be thoroughly crystallized, whereby any impurity is either inactive or less selective.
Når til slutt denne zeolitt er innarbeidet i; et vaskepulver er det vesentlig at den granulometriske fordeling er godt samlet rundt en midlere diameter på 2 til 3 When finally this zeolite is incorporated into; a washing powder, it is essential that the granulometric distribution is well gathered around an average diameter of 2 to 3
u, noe som er lite nok til å forhindre produktet fra. å bli holdt tilbake i tekstilfibrehe, men stort nok til å tillate lett faststoff-væske separering under fremstillingen. u, which is small enough to prevent the product from to be retained in textile fibers, but large enough to allow easy solid-liquid separation during manufacture.
Syntesen og ioneutbyttingsegenskapene for syntetiske zeolitter og spesielt zeolitt A har vært velkjent i mange: år(se"Ion exchange" av Friedrich Helfferich, 1962, McGraw-Hill Book Company, kapittel 2, sidene 10-16.) The synthesis and ion exchange properties of synthetic zeolites and especially zeolite A have been well known for many: years (see "Ion exchange" by Friedrich Helfferich, 1962, McGraw-Hill Book Company, Chapter 2, pages 10-16.)
Syntese prosessene utføres alle diskontinuerligThe synthesis processes are all carried out discontinuously
ved å blande elementene Si, Al og Na, tilsatt i forskjellige former, for å oppnå en silisiumaluminat gel som felles ut. Denne gel krystalliseres deretter til zeolitt A i det den mettes i moderluten-inneholdene en mengde fri soda og opp-løselig aluminiumoksyd som er forenelig med den oppnådde type zeolitt. Slike prosesser er beskrevet f.eks. i. US-patentet 2.8H1.471 og 2.847.280, B.F. 1.1404 . 467 , B.E. by mixing the elements Si, Al and Na, added in different forms, to obtain a silicon aluminate gel that precipitates. This gel is then crystallized into zeolite A as it saturates the mother liquor contents with an amount of free soda ash and soluble aluminum oxide which is compatible with the type of zeolite obtained. Such processes are described e.g. i. US Patent 2,8H1,471 and 2,847,280, B.F. 1.1404. 467 , B.E.
813.581 og DAS 2.517.218. 813,581 and DAS 2,517,218.
Disse diskontinuerlige utfellinger fører til;vesen-tlige variasjoner av innholdet av Na2jJ^12°3°^Si02: i væskene som oppnås fra blandingene. Dette resulterer i en betydelig heterogenitet i det oppnådde produkt med henblikk på partikkelstørrelse, krystallinitet og bytteselektivitet These discontinuous precipitations lead to substantial variations in the content of Na2jJ^12°3°^SiO2: in the liquids obtained from the mixtures. This results in a significant heterogeneity in the obtained product with regard to particle size, crystallinity and exchange selectivity
(porestørrelse).(pore size).
En helt kontinuerlig fremgangsmåte, søkt beskyttetA completely continuous procedure, sought protected
av foreliggende søkere i fransk søknad nr. 77.23373v mulig-gjør at Na siliciumaluminat gel fremstilles fra en blanding med konstant sammensetning, men mangelen ved denne prosess erj at det er nødvendig med et relativt stort antall metnings-beholdere, anordnet i en kaskade, er nødvendig for å unngå kortslutning av spesielle andeler av friskt utfelt gel og således oppnå den ønskede partikkelstørrelse. of the present applicants in French application no. 77.23373v makes it possible for Na silicon aluminate gel to be produced from a mixture with a constant composition, but the shortcoming of this process is that it requires a relatively large number of saturation containers, arranged in a cascade, necessary to avoid short-circuiting of particular proportions of freshly precipitated gel and thus achieve the desired particle size.
Etter fortsatt arbeid på dette området er det nå opp-daget og perfeksjonert en fremgangsmåte for fremstilling av zeolitt der de forskjellige problemer er overvunnet. Denne prosess består i fremstilling ved øyeblikkelig utfelling av et, natrium siliciumaluminat gel fra oppløsninger av. natrium silikat og natrium aluminat, blandet samtidig og kontinuerlig, ved hjelp av et egnet apparatur. Kvaliteten i det oppnådde produkt avhenger av kvaliteten av den kontinuerlige fremstillingen av blandingen. After continued work in this area, a method for the production of zeolite has now been discovered and perfected in which the various problems have been overcome. This process consists in the production by immediate precipitation of a sodium silicon aluminate gel from solutions of. sodium silicate and sodium aluminate, mixed simultaneously and continuously, using a suitable apparatus. The quality of the product obtained depends on the quality of the continuous preparation of the mixture.
Således må blandingen utføres hurtig og den må være effektiv nok til å sikre at det ikke på noen tid er lokali-serte overskudd av silicium oksyd i forhold til aluminium oksyd (antall mol A^O.,, bør være lik > 2 mol SiC^). Et overskudd av silicium oksyd, selv et øyeblikkelig, vil føre til en forringelse av kvaliteten av produktet ved å initiere utfelling og krystallisering av et silicium aluminat for-skjellig fra zeolitt A. Thus, the mixing must be carried out quickly and it must be efficient enough to ensure that there are no localized excesses of silicon oxide in relation to aluminum oxide at any time (the number of moles of A^O.,, should be equal to > 2 moles of SiC^ ). An excess of silicon oxide, even momentarily, will lead to a deterioration of the quality of the product by initiating precipitation and crystallization of a silicon aluminate different from zeolite A.
Blandingen utføres kontinuerlig i en reaktor utstyrt med et røreverksystem som tillater perfekt og øyeblikkelig homogenisering, slik som. f.eks. en turbinrører eller hvilken som helst annen egnet rører. Kapasiteten for reaktoren er beregnet for å oppnå en midlere oppholdstid på mellom 30 sek. og 20 minutter, noe som er vesentlig'for å.sikre total dan-nelse av gelen. The mixing is carried out continuously in a reactor equipped with an agitator system that allows perfect and instant homogenization, such as. e.g. a turbine stirrer or any other suitable stirrer. The capacity of the reactor is calculated to achieve an average residence time of between 30 sec. and 20 minutes, which is essential to ensure total formation of the gel.
Tilsetningen av de to reaksjonsoppløsninger hvis strømningshastigheter reguleres, skjer i sonen med sterkt sug dannet av turbinen. Virkningen av denne turbin økes ytter-ligere hvis den er anbrakt i en "hylse" som er fast med eller roterer samtidig som turbinen. The addition of the two reaction solutions whose flow rates are regulated takes place in the zone of strong suction formed by the turbine. The effect of this turbine is further increased if it is placed in a "sleeve" which is fixed with or rotates at the same time as the turbine.
Denne hylse består av to plater hvis konkavitet er vendt mot turbinen. Disse to plater innelukker et volum hvori de to reaksjonsoppløsninger injiseres eller suges. This sleeve consists of two plates whose concavity faces the turbine. These two plates enclose a volume into which the two reaction solutions are injected or sucked.
Den natrium silicium aluminat gel som. således kontinuerlig fremstilles dekanteres ved overløp til en andre reaktor, utstyrt med et rørverk og som holdes ved en konstant temperatur innen området 75° til 100°C, for å mulig-gjøre krystalliseringen av den ønskede zeolitt A. Denne krystallisering skjer således diskontinuerlig, fordelen ved dette er at krystallinitetsnivået som er nødvendig og par-tikkelstørrelsen for sluttproduktet kan justeres etter hvert ved å påvirke metningsperioden eller omrøringsbetingelsén. The sodium silicon aluminate gel which. thus continuously produced is decanted by overflow to a second reactor, equipped with a pipework and which is kept at a constant temperature within the range of 75° to 100°C, to enable the crystallization of the desired zeolite A. This crystallization thus occurs discontinuously, the advantage of this is that the level of crystallinity required and the particle size of the final product can be adjusted over time by influencing the saturation period or stirring conditions.
i Den kontinuerlige fremstilling av natrium silicium aiuminat gel kan bevirkes ved på den ene side å gå ut fra natrium aluminat-oppløsninger som karakteriseres ved.et. mol forhold mellom Al^ O^ og Na20 på mellom 0.3 og 0.8, og et forhold mellom E^ O og Na^O på mellom 5 og 150, disse opp-løsninger oppnås enten ved å påvirke hydratisert aluminiumoksyd med en natrium hydroksyd oppløsning eller ved å opp- i The continuous production of sodium silicon aluminate gel can be effected by, on the one hand, starting from sodium aluminate solutions which are characterized by.et. mole ratio between Al^O^ and Na2O of between 0.3 and 0.8, and a ratio between E^O and Na^O of between 5 and 150, these solutions are obtained either by affecting hydrated aluminum oxide with a sodium hydroxide solution or by to up-
nå den fra en Bayer syklus for fremstilling av aluminiumoksyd, og på den annen side karakteriseres natriumsilikat-oppløsningene ved et mol forhold mellom SiC^og Na20.på mellom 2 og 3>5og et forhold mellom H^ O og Na20 på mellom 25 og 100. Disse oppløsninger kan fremstilles fra råsili-cium og soda materialer som varierer i henhold til økonom-iske kriterier, enten industrielt natriumsilikat i pulver-form eller industrielle natriumsilikat-lut, eller siliciumoksyd inneholdt i sand og soda, enten soda og siliciumdioksyd gel gjenvunnet fra en fluorsilicium sur rest fra et anlegg for fremstilling av aluminiumfluorid eller hydrogen-fluorsyre, eller et-behandlingsanlegg for gasser som-fri-gjøres under behandling av naturlige fosfater, eller natrium-silikat oppnådd fra et anlegg for avsiliciering av bauksitter før behandling i aiuminium-oksydproduserende fabrikker, eller restsiliciumoksyd oppnådd ved fremstilling av aluminiumsalt-er ved våtoppslutning på naturlige siliciumaluminater, slik som kaolin eller leirer, eller siliciumoksyd oppnådd.termisk, f.eks. ved fremstilling av magnesium, silicium-metall eller silicjumlegeringer. now it from a Bayer cycle for the production of alumina, and on the other hand, the sodium silicate solutions are characterized by a molar ratio between SiC^ and Na2O of between 2 and 3>5 and a ratio between H^O and Na2O of between 25 and 100 These solutions can be prepared from raw silicon and soda materials that vary according to economic criteria, either industrial sodium silicate in powder form or industrial sodium silicate lye, or silicon oxide contained in sand and soda, either soda and silicon dioxide gel recovered from a fluorosilicic acid residue from a plant for the production of aluminum fluoride or hydrofluoric acid, or a treatment plant for gases released during the treatment of natural phosphates, or sodium silicate obtained from a plant for the desilication of bauxite before treatment in aluminum oxide-producing factories, or residual silicon oxide obtained from the production of aluminum salt-is by wet digestion of natural silicon aluminates, such as olin or clays, or silica obtained thermally, e.g. in the production of magnesium, silicon metal or silicon alloys.
Blandingen som oppnås ved tilsetting av disse natriumaluminat- og silikatoppløsninger bør ha et mol forhold mellom Al^ O^ og Si02på mellom 0.5 og 0.2 og Na20 innholdet bør justeres slik at sodakonsehtrasjonen i væsken hvori krystalliseringen gjennomføres etter utfellingen ikke er The mixture obtained by adding these sodium aluminate and silicate solutions should have a mole ratio between Al^ O^ and SiO2 of between 0.5 and 0.2 and the Na20 content should be adjusted so that the soda concentration in the liquid in which the crystallization is carried out after the precipitation is not
mer enn 135 g/l NaOH for å unngå krystallisering av. sili-ciumaluminatene.av den inaktive feltspattypen, men ikke er mindre enn 26 g/l NaOH for å sikre at krystalliserihgshas-tigheten for zeolitt A er forenelig med industriell prod-uksjon.. Etter at natrium silicium aluminat gelen som frem-spilles som beskrevet ovenfor er mettet blir det oppnådd eri suspensjon av krystallisert zeolitt A som separeres fra mqderluten på en hvilken som helst egnet måte for væske-fast-st|offseparasjon (dekantering, filtrereing osv.), og deretter vasket og tørket. more than 135 g/l NaOH to avoid crystallization of. the silicon aluminates. of the inactive feldspar type, but is not less than 26 g/l NaOH to ensure that the crystallization rate of zeolite A is compatible with industrial production. After the sodium silicon aluminate gel produced as described above is saturated, a suspension of crystallized zeolite A is obtained which is separated from the mqderlut by any suitable method for liquid-solid separation (decanting, filtration, etc.), and then washed and dried.
Den zeolitt A fremstillet ved den fremgangsmåte som beskrevet ovenfor har følgende egenskaper: - smal partikkelstørrelse fordeling, 90% av part-iklene er ca. 4 \ i for en midlere diameter på mellom 1 og 10 The zeolite A produced by the method described above has the following properties: - narrow particle size distribution, 90% of the particles are approx. 4 \ in for a mean diameter of between 1 and 10
y som kan justeres i følge den for ønsket brukj y which can be adjusted according to the desired usej
ionebyttekapasiteten ér større enn 100 mg: Ca + +/g tørt produkt. the ion exchange capacity is greater than 100 mg: Ca + +/g dry product.
Den således oppnådde zeolitt A er spesielt egnet for bruk i vaskepulvere for å mykgjøre hårdt vann. The zeolite A thus obtained is particularly suitable for use in washing powders to soften hard water.
De følgende eksempler illustrerer oppfinnelsen utenThe following examples illustrate the invention without
å begrense den.to limit it.
Eksempel 1Example 1
Ved å oppslutte hydratisert aluminium med NaOH opp-løsning ved 100°C oppnås det oppløsning Å av natriumaluminat inneholdene 5^,3 g Al^ O^ og 8l.l g Na20 pr. liter (d.v.s. mol forhold mellom Al^O-^og Na20 og. henholdsvis H^O -og Na20 på 0.40 henholdsvis 42). By dissolving hydrated aluminum with NaOH solution at 100°C, a solution Å of sodium aluminate containing 5^.3 g of Al^O^ and 8l.l g of Na2O per liter (i.e. mole ratio between Al^O-^and Na2O and respectively H^O -and Na2O of 0.40 and 42 respectively).
Ved å oppløse pulverisert natriumsilikat av industrikvalitet i vann, oppnås en oppløsning B av natriumsiiicat inneholdene 137-4 g Si02og 47,2 g Na20 pr. liter (d.v.s. , forhold mellom Si02og Na20 henholdsvis H20 og Na20 på 3 henholdsvis 69)• Det fremstilles en natriumsilicium-aluminat gel der forholdet mellom A^O^ og SiC^er 0,6 ved samtidig, å føre . 0,86 1 oppløsning A og 0.344 1 oppløsning B til en reaktor By dissolving powdered sodium silicate of industrial quality in water, a solution B of sodium silicate containing 137-4 g SiO 2 and 47.2 g Na 2 O per liters (i.e. , ratio between SiO2 and Na20 respectively H20 and Na20 of 3 and 69 respectively)• A sodium silicon aluminate gel is produced in which the ratio between A^O^ and SiC^ is 0.6 by simultaneously leading . 0.86 1 solution A and 0.344 1 solution B to a reactor
av deri ovenfor beskrevne type, ved en temperatur ved 90°C.of the type therein described above, at a temperature of 90°C.
i in
i jdet volumet er beregnet til å gi en gjennomsnittlig opp-, holdstid på 45 sekunder. Den således oppnådde gel dekanteres ved overløp til metningsreaktoren. Denne operasjonen gj;ennomføres i 10 minutter. Metningen av den således oppnådde gel gjennomføres iQden sistnevnte reaktor som holdes ved en temperatur ved 90 C og er utstyrt med et røreverk som-umuliggjør at zeolitten holdes effektivt i suspensjon under i jdet volume is calculated to give an average holding time of 45 seconds. The gel thus obtained is decanted by overflow to the saturation reactor. This operation is carried out for 10 minutes. The saturation of the gel thus obtained is carried out in the latter reactor which is kept at a temperature of 90 C and is equipped with a stirrer which makes it impossible for the zeolite to be effectively kept in suspension under
i krystalliseringen. in the crystallization.
I i Etter 6 timer separeres zeolitten fra moderluten' ved filtrering, vaskes deretter og tørkes i en ovn ved 90°C. Dét oppnås 140 g produkt og røntken difraksjonsdiagrammet vijser at det dreier seg om krystallinsk zeolitt A.. Partik-kelstørrelsen er mellom 1.5 og 10 p med en gjennomsnittlig diameter på ca. 2.9 y. After 6 hours, the zeolite is separated from the mother liquor by filtration, then washed and dried in an oven at 90°C. 140 g of product is obtained and the X-ray diffraction diagram shows that it is crystalline zeolite A. The particle size is between 1.5 and 10 µm with an average diameter of approx. 2.9 y.
Ca<++>ione sekvesteringskraften er 115 rog Ca pr. gram vannfritt produkt og den således oppnådde zeolitt A hadde følgende granulometriske kurve: The Ca<++>ion sequestration power is 115 rog Ca per gram of anhydrous product and the zeolite A thus obtained had the following granulometric curve:
Eksempel 2 Example 2
Oppløsning A av natriumaluminat fremstilles som tid-ligere ved å oppslutte hydratisert aluminium med en natrium hydroksydoppløsning og inneholder 53 g A^O^ °& ^ NagO pr. liter (tilsvarende forhold mellom AlgO^og Na20 hen-' holdsvis Hn0 og Nao0 på 0.40 henholdsvis 44). Solution A of sodium aluminate is prepared as time-liger by dissolving hydrated aluminum with a sodium hydroxide solution and contains 53 g of A^O^ °& ^ NagO per liter (corresponding ratio between AlgO^ and Na20 respectively Hn0 and Nao0 of 0.40 and 44 respectively).
Oppløsning B av- natrium silikat fremstilles fra ét siliciumoksyd kjent som I-^SiFg som har den fordel at det er meget rimelig da det er en rest fra aluminiumfluoridfrem- stillingsanlegget. Dette sterkt reaktive siliciumoksyd Solution B of sodium silicate is produced from a silicon oxide known as I-^SiFg which has the advantage that it is very reasonable as it is a residue from the aluminum fluoride manufacturing plant. This highly reactive silicon oxide
. kan lett sluttes opp med en NaOH oppløsning ved 100°C og man oppnår en natrium-silikat-oppløsning inneholdende 12-?.9-g Si02og 37-8 g Na20 pr. liter (tilsvarende forhold mellom Si02 og Na20 , henholdsvis H20 og Na20 på 3.5 henholdsvis 88).. ' . can be easily added with a NaOH solution at 100°C and a sodium silicate solution is obtained containing 12-?.9-g SiO2 and 37-8 g Na2O per liter (corresponding ratio between SiO2 and Na20, respectively H20 and Na20 of 3.5 and 88 respectively)..'
I 0.78 1 oppløsning A og 0.313 1 oppløsning B behand-1 In 0.78 1 solution A and 0.313 1 solution B treat-1
le.s ved den i eksempel 1 beskrevne metode. Den ferdige ■ zeolitt A har en sekvesteringskraft på 111 mg Ca<++>/gram vannfritt produkt og en partikkelstørrelse på mellom 3 og 15' M med en gjennomsnittlig diameter på 6\ i : , le.s by the method described in example 1. The finished ■ zeolite A has a sequestering power of 111 mg Ca<++>/gram of anhydrous product and a particle size of between 3 and 15' M with an average diameter of 6\ in : ,
Eksempel 3 Example 3
Oppløsning A av natrium-aluminat består av en opp-løsning kjent som "clear from Ist washer", tatt fra en al-uminiumoksydproduksjonsenhet som arbeider på Bayer prinsip-pet, og inneholder 59 g A120^og 62.1 g Na20 pr. liter (tilsvarende forhold mellom kl^ O-^ og Na20, henholdsvis H2QSolution A of sodium aluminate consists of a solution known as "clear from Ist washer", taken from an alumina production unit working on the Bayer principle, and contains 59 g Al 2 O 2 and 62.1 g Na 2 O per liter (corresponding ratio between kl^ O-^ and Na2O, respectively H2Q
og Na20 på 0.58 henholdsvis 56). and Na2O of 0.58 and 56 respectively).
Oppløsning B av natriumsilikat oppnås ved å oppløse pulverisert natriumsilikat av industrikvalitet i vann og inneholder 137 g Si02og 40 g Na20 pr. liter (tilsvarende forhold mellom Si02 og Na20 , henholdsvis H20 og Na20 på Solution B of sodium silicate is obtained by dissolving powdered sodium silicate of industrial quality in water and contains 137 g SiO2 and 40 g Na20 per liter (corresponding ratio between SiO2 and Na20, respectively H20 and Na20 on
3-5 henholdsvis 82).3-5 respectively 82).
1.270 1 oppløsning A og 0.410 1 oppløsning B (tilsvarende et forhold mellom A120^og Si02på 0.8 i den ferdr-ige reaksjonsblanding) behandles ved den i eksempel 1 bes^-krevne måte. Den ferdige zeolitt A som oppnås har en sekvesteringskraft.på 120 mg Ca<+>+pr. gram vannfritt produkt, 1.270 1 solution A and 0.410 1 solution B (corresponding to a ratio between Al 2 O 2 and SiO 2 of 0.8 in the four-phase reaction mixture) are treated in the manner described in example 1. The finished zeolite A that is obtained has a sequestering power of 120 mg Ca<+>+ per grams of anhydrous product,
og en partikkelstørrelse på mellom 2 og 8 p, med en gjennom- and a particle size of between 2 and 8 p, with a through-
snittelig diameter på 4.8 y: average diameter of 4.8 y:
Eksempel 4 Oppløsning A av natrium-aluminat fremstilles fra en'oplpløsning kjent som "de.composed liquor" tatt fra et Bayer aluminiumoksydanlegg, inneholdende 98.3 g Al-^O^ og 165-5 g Na20 pr., liter (tilsvarende forhold mellom A120^ og Na20, henholdsvis H .cl 0 og Na do.0 på 0.36 henholdsvis 21), nybeladet med A120-^ved tilsetning av hydratisert aluminiumoksyd ved 100°C og fortynnet til en sluttsammensetning på 58.5 g A12'0^ og 66.4 g Na20 pr. liter (tilsvarende forhold mellom A120^og Na20, henholdsvis H20 og Na20 på 0.53>henholdsvis 52). Oppløsning B av natrium-silikat er identisk med den som er beskrevet i eksempel 3. Example 4 Solution A of sodium aluminate is prepared from a solution known as "decomposed liquor" taken from a Bayer alumina plant, containing 98.3 g Al-^O^ and 165-5 g Na2O per liter (corresponding ratio of A120 ^ and Na20, respectively H .cl 0 and Na do.0 of 0.36 and 21 respectively), freshly charged with Al20-^by addition of hydrated alumina at 100°C and diluted to a final composition of 58.5 g Al2'0^ and 66.4 g Na20 per liter (corresponding ratio between A120^ and Na20, respectively H20 and Na20 of 0.53>respectively 52). Solution B of sodium silicate is identical to that described in example 3.
1.220 liter oppløsning A og 0.430 liter oppløsning1,220 liters of solution A and 0,430 liters of solution
B (tilsvarende et forhold mellom A120^og Si02på 0.8 i den ferdige reaksjonsblanding) behandles i følge den i eksempel 1 beskrevne metode. Den ferdige zeolitt A som oppnås har en sekvesteringskraft på 120 mg Ca<++>pr. gram vannfritt produkt og en partikkelstørrelse på mellom 2 og 10 y med en gjennomsnittlig diameter på 4.7 y.. B (corresponding to a ratio between Al 2 O 2 and SiO 2 of 0.8 in the finished reaction mixture) is treated according to the method described in example 1. The finished zeolite A that is obtained has a sequestering power of 120 mg Ca<++>per. grams of anhydrous product and a particle size of between 2 and 10 y with an average diameter of 4.7 y..
Eksempel 5 Oppløsning A ble fremstilt som beskrevet i eksempel 1 fra hydratisert aluminiumoksyd og natriumhydroksyd og inneholder 55 g pr. liter AlgO^og 77 gram pr. liter Na20 (til-syarende forhold mellom kl^ O^ og Na20, henholdsvis H20 og Na20 på 0.43 henholdsvis 63). Example 5 Solution A was prepared as described in example 1 from hydrated aluminum oxide and sodium hydroxide and contains 55 g per liter AlgO^and 77 grams per liter of Na20 (adjusting ratio between kl^ O^ and Na20, respectively H20 and Na20 of 0.43 and 63 respectively).
I Oppløsning B ble fremstilt ved å oppløse natrium-silikat av industrikvalitet i vann og inneholdt 138 gram pr. liter SiOj.og 42 gram pr. liter Na20 (tilsvarende forhold mellom Si02og Na20, henholdsvis H20 og Na20 på 3•4, henholdsvis 78). 1 t ! iDet fremstilles en natriumsiliciumaluminat-gel med et forhold mellom A120^og Si02på 1.1 ved samtidig å føre 12,7 1 oppløsning A og 27 1 oppløsning B ved en temperatur av] 90°C til en reaktor av den ovenfor beskrevne type, hvori volumet er konstruert for å oppnå en midlere oppholdstid på 4 minutter. Den således oppnådde gel dekanteres ved overløp til metningsreaktoren. Denne operasjon fortsettes i; 90 minutter . I Solution B was prepared by dissolving industrial grade sodium silicate in water and contained 138 grams per liter SiOj. and 42 grams per liter Na20 (corresponding ratio between SiO2 and Na20, respectively H20 and Na20 of 3•4, respectively 78). 1 h ! A sodium silicon aluminate gel is prepared with a ratio between A120^ and SiO2 of 1.1 by simultaneously feeding 12.7 1 of solution A and 27 1 of solution B at a temperature of] 90°C to a reactor of the type described above, in which the volume is designed to achieve an average residence time of 4 minutes. The gel thus obtained is decanted by overflow to the saturation reactor. This operation is continued in; 90 minutes.
Den således oppnådde gel mettes, og etter 6 timer'ved 90°C under omrøring filtreres zeolitten av, vaskes og tørkes. The gel thus obtained is saturated, and after 6 hours at 90°C with stirring, the zeolite is filtered off, washed and dried.
Det oppnås 11 kg zeolitt A med en sekvesteringskraft på 120 mg Ca<++>pr. gram vannfritt produkt og en partikkel-størrelse' på mellom 1.5 og 15y med en gjennomsnittlig diameter på 3 y • 11 kg of zeolite A with a sequestering power of 120 mg Ca<++>per is obtained. grams of anhydrous product and a particle size of between 1.5 and 15y with an average diameter of 3y •
Claims (1)
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FR7835344A FR2444005A1 (en) | 1978-12-15 | 1978-12-15 | INDUSTRIAL PROCESS FOR THE SEMI-CONTINUOUS MANUFACTURE OF ZEOLITE A |
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NO794092L true NO794092L (en) | 1980-06-17 |
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NO794092A NO794092L (en) | 1978-12-15 | 1979-12-14 | PROCEDURE FOR SEMI-CONTINUOUS PREPARATION OF ZEOLITE A |
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JP (1) | JPS5585416A (en) |
BE (1) | BE880533A (en) |
BR (1) | BR7908222A (en) |
CA (1) | CA1142501A (en) |
CH (1) | CH641128A5 (en) |
DE (1) | DE2950086A1 (en) |
DK (1) | DK532479A (en) |
ES (1) | ES486941A0 (en) |
FI (1) | FI793923A (en) |
FR (1) | FR2444005A1 (en) |
GB (1) | GB2038301B (en) |
GR (1) | GR66001B (en) |
HU (1) | HU181898B (en) |
IT (1) | IT1119601B (en) |
LU (1) | LU81989A1 (en) |
NO (1) | NO794092L (en) |
PL (1) | PL125174B1 (en) |
PT (1) | PT70474A (en) |
RO (1) | RO78900A (en) |
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JPS6049130B2 (en) * | 1980-12-27 | 1985-10-31 | 日本化学工業株式会社 | Manufacturing method of A-type zeolite |
DK164097C (en) * | 1982-09-20 | 1992-10-05 | Tosoh Corp | PROCEDURE FOR THE MANUFACTURE OF ZEOLITES |
DE3926400A1 (en) * | 1988-08-12 | 1990-02-22 | Degussa | Sodium A zeolite with small particle size - used as phosphate substitute and in liq. washing compsn. |
DK0490011T3 (en) * | 1990-12-14 | 1994-11-07 | Foret Sa | Process for the preparation of zeolite 4A from bauxite |
RS58490B1 (en) | 2011-02-11 | 2019-04-30 | Zs Pharma Inc | Use of a zirconium silicate for the treatment of hyperkalemia |
US9943637B2 (en) | 2012-06-11 | 2018-04-17 | ZS Pharma, Inc. | Microporous zirconium silicate and its method of production |
CN104968336A (en) * | 2012-07-11 | 2015-10-07 | Zs制药公司 | Microporous zirconium silicate for the treatment of hyperkalemia in hypercalcemic patients and improved calcium-containing compositions for the treatment of hyperkalemia |
US10695365B2 (en) | 2012-10-22 | 2020-06-30 | ZS Pharma, Inc. | Microporous zirconium silicate for the treatment of hyperkalemia |
AU2013334776B2 (en) | 2012-10-22 | 2017-08-31 | ZS Pharma, Inc. | Microporous zirconium silicate for treating hyperkalemia |
US11053143B2 (en) | 2015-02-20 | 2021-07-06 | Usalco, Llc | Stable concentrated polyaluminum chlorosilicate solutions |
US9592253B1 (en) | 2015-10-14 | 2017-03-14 | ZS Pharma, Inc. | Extended use zirconium silicate compositions and methods of use thereof |
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FR1280877A (en) * | 1961-01-14 | 1962-01-08 | Socony Mobil Oil Co | Process for preparing crystalline zeolites |
GB1115489A (en) * | 1964-07-31 | 1968-05-29 | Deputy Minister | A process to manufacture crystalline synthetic zeolites for use as molecular sieves |
US3425800A (en) * | 1967-10-05 | 1969-02-04 | Aluminum Co Of America | Production of crystalline zeolites |
AT322511B (en) * | 1970-06-15 | 1975-05-26 | Martinswerk G M B H Fuer Chem | PROCESS FOR THE DIRECT MANUFACTURING OF A PURE CRYSTALLINE ZEOLITHIC MOLECULAR SCREEN WITH A PORE WIDTH OF 4Å. |
DD107428B3 (en) * | 1973-11-05 | 1992-12-10 | Chemie Ag Bittrfeld Wolfen | METHOD AND DEVICE FOR PRODUCING SYNTHETIC ZEOLITE |
DE2447021C3 (en) * | 1974-10-02 | 1984-03-22 | Degussa Ag, 6000 Frankfurt | Type A crystalline zeolite powder and the process for its preparation |
DE2651445A1 (en) * | 1976-11-11 | 1978-05-18 | Degussa | TYPE A II CRYSTALLINE ZEOLITE POWDER |
DE2651384C2 (en) * | 1976-11-11 | 1984-03-15 | Degussa Ag, 6000 Frankfurt | Process for processing waste dusts containing silicon dioxide into crystalline zeolitic molecular sieves of type A. |
-
1978
- 1978-12-15 FR FR7835344A patent/FR2444005A1/en active Granted
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- 1979-11-26 GB GB7940829A patent/GB2038301B/en not_active Expired
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- 1979-12-11 BE BE0/198501A patent/BE880533A/en not_active IP Right Cessation
- 1979-12-12 SE SE7910247A patent/SE7910247L/en not_active Application Discontinuation
- 1979-12-12 CA CA000341755A patent/CA1142501A/en not_active Expired
- 1979-12-13 JP JP16090979A patent/JPS5585416A/en active Pending
- 1979-12-13 LU LU81989A patent/LU81989A1/en unknown
- 1979-12-13 DE DE19792950086 patent/DE2950086A1/en not_active Withdrawn
- 1979-12-14 CH CH1112679A patent/CH641128A5/en not_active IP Right Cessation
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RO78900A (en) | 1982-12-06 |
PL220420A1 (en) | 1980-10-06 |
HU181898B (en) | 1983-11-28 |
GR66001B (en) | 1981-01-13 |
DE2950086A1 (en) | 1980-06-19 |
BR7908222A (en) | 1980-07-22 |
IT1119601B (en) | 1986-03-10 |
PT70474A (en) | 1979-12-01 |
IT7969413A0 (en) | 1979-12-14 |
YU296179A (en) | 1983-01-21 |
FR2444005B1 (en) | 1984-05-11 |
SE7910247L (en) | 1980-06-16 |
JPS5585416A (en) | 1980-06-27 |
CH641128A5 (en) | 1984-02-15 |
BE880533A (en) | 1980-06-11 |
LU81989A1 (en) | 1981-07-23 |
FI793923A (en) | 1980-06-16 |
PL125174B1 (en) | 1983-04-30 |
ES8101516A1 (en) | 1980-12-16 |
GB2038301A (en) | 1980-07-23 |
DK532479A (en) | 1980-06-16 |
GB2038301B (en) | 1983-02-09 |
FR2444005A1 (en) | 1980-07-11 |
ES486941A0 (en) | 1980-12-16 |
CA1142501A (en) | 1983-03-08 |
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