SK286560B6 - A method for producing smooth surface silica gel stienspheric particles from serpentinite - Google Patents
A method for producing smooth surface silica gel stienspheric particles from serpentinite Download PDFInfo
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- SK286560B6 SK286560B6 SK75-2005A SK752005A SK286560B6 SK 286560 B6 SK286560 B6 SK 286560B6 SK 752005 A SK752005 A SK 752005A SK 286560 B6 SK286560 B6 SK 286560B6
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- silica gel
- sio
- silica
- serpentinite
- alkali metal
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000000741 silica gel Substances 0.000 title claims abstract description 28
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title description 7
- 239000002245 particle Substances 0.000 title description 7
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims abstract description 9
- 238000007710 freezing Methods 0.000 claims abstract description 7
- 230000008014 freezing Effects 0.000 claims abstract description 7
- 238000002386 leaching Methods 0.000 claims abstract description 7
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 7
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 239000012798 spherical particle Substances 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 27
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 8
- 239000011707 mineral Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000010257 thawing Methods 0.000 claims description 3
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000000017 hydrogel Substances 0.000 abstract description 8
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract description 4
- 238000006068 polycondensation reaction Methods 0.000 abstract description 4
- 238000001291 vacuum drying Methods 0.000 abstract description 3
- 229910052681 coesite Inorganic materials 0.000 abstract description 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 2
- 229910052682 stishovite Inorganic materials 0.000 abstract description 2
- 229910052905 tridymite Inorganic materials 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 230000003467 diminishing effect Effects 0.000 abstract 1
- 229960001866 silicon dioxide Drugs 0.000 description 26
- 239000000243 solution Substances 0.000 description 10
- 239000011148 porous material Substances 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000004115 Sodium Silicate Substances 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052911 sodium silicate Inorganic materials 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 238000004440 column chromatography Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- -1 alkali metal salts Chemical class 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 235000015110 jellies Nutrition 0.000 description 2
- 239000008274 jelly Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
Spôsob výroby silikagélu s hladkými stenami sférických častíc spočíva v tom, že na tuhý oxid kremičitý SiO2 s obsahom nad 98,5 hmotn. %, získaný zo serpentinitu a anorganickej kyseliny, sa pôsobí roztokom hydroxidu alkalického kovu za vzniku kremičitanového roztoku alkalického kovu. Zo vzniknutého koloidného roztoku na báze kyseliny hydrogénkremičitej sa polykondenzáciou vylúči hydrogél. Kontrolovaným režimom chladenia, mrazenia a podtlakového sušenia, zdrobnením a lúhovaním v anorganickej kyseline, premývaním destilovanou vodou do dosiahnutianeutrálneho pH a sušením pri teplote 105 °C vznikne silikagél s deklarovanými vlastnosťami.The process for producing silica with smooth walls of spherical particles is based on SiO2 having a content of above 98.5 wt. %, obtained from serpentinite and inorganic acid, is treated with an alkali metal hydroxide solution to form an alkali metal silicate solution. A hydrogel is deposited from the resulting silica-based colloidal solution by polycondensation. A controlled mode of cooling, freezing and vacuum drying, diminishing and leaching in inorganic acid, washing with distilled water to reach neutral pH and drying at 105 ° C results in silica gel with declared properties.
Description
Spôsob výroby silikagélu s hladkým povrchom stien sférických častíc z oxidu kremičitého SiO2 zo serpentinitovej nerastnej suroviny spadá do oblasti spracovania nerastných surovín.The process for the production of silicagel having a smooth surface of the spherical silica SiO 2 particles from a serpentinite mineral raw material falls within the field of mineral processing.
Doterajší stav technikyBACKGROUND OF THE INVENTION
V patente č. SK 283183 je uvedený spôsob výroby oxidu kremičitého SiO2 s obsahom do 98 hmotn. % oxidu kremičitého SiO2 zo serpentinitovej nerastnej suroviny lúhovaním kyselinou chlorovodíkovou HCI.U.S. Pat. SK 283183 discloses a process for producing SiO 2 with up to 98 wt. % Of silica SiO 2 of serpentine mineral raw material leaching with hydrochloric acid HCl.
Získavanie reaktívneho pórovitého a vláknitého silikagélu zo serpentinitu je riešené v japonskom dokumente JP 89147, v ktoromje uvedený spôsob spracovania serpentinitu anorganickými kyselinami.The recovery of reactive porous and fibrous silica from serpentinite is solved in Japanese document JP 89147, which discloses a process for treating serpentinite with inorganic acids.
V stave techniky je známy aj postup získania silikagélu alkalickou geláciou zmesi alkalického kremičitanu a hydroxidu (US 3 959 174, dokument zverejnený v roku 1973).It is also known in the art to obtain silica gel by alkaline gelling a mixture of an alkali silicate and a hydroxide (U.S. Pat. No. 3,959,174, published in 1973).
Guľôčkový silikagél sa podľa patentovej prihlášky PP 601-94 vyrába rozstrekovaním presne zmiešaných roztokov kremičitanu sodného a kyseliny do systému, pozostávajúceho z vrstvy organickej kvapaliny ncmicšateľnej s vodou, pod ktorou sa nachádza vodná vrstva.The bead silica gel according to patent application PP 601-94 is produced by spraying precisely mixed solutions of sodium silicate and acid into a system consisting of a layer of a water-immiscible organic liquid under which an aqueous layer is located.
Rozširovanie pórov úzkopórovitého silikagélu s priemerom pórov 1 až 30 nm kontrolovaným a kombinovaným účinkom vysokej teploty, soli a alkálie prebieha podľa patentu č. 281593 tak, že póry' východiskového silikagélu sa vyplnia zmesou neutrálnej anorganickej soli, ktorá v priebehu procesu pôsobí ako výstuž a anorganickej soli, ktorá pri žíhaní uvoľňuje alkálie, potom nasleduje žíhanie na teplotu 600 až 800 °C počas 2 - 5 hodín. Po skončení žíhania sa soli zo systému vymyjú vodou a silikagél s rozšírenými pórmi sa vysuší. Princíp prípravy sférických častíc silikagélu s vysokou čistotou a riadenou veľkosťou pórov podľa patentovej prihlášky PP 1998-4027 je v tom, že vhodne zriedená koloidná disperzia oxidu kremičitého s prídavkom alkalického kremičitanu sa vnesie do prostredia organickej fázy, ktorá je zložená zo zmesi alifatických a aromatických uhľovodíkov alebo ich derivátov nemiešateľných s vodou a alkydovej živice a po rozmiešaní sa k emulzii pridá také množstvo kyseliny miešateľnej s použitou organickou a vodnou fázou, aby sa po difúzii kyseliny do kvapiek vodnej fázy vytvorili podmienky vzniku hydrogélu.The pore expansion of narrow-pored silica gel with a pore diameter of 1 to 30 nm controlled and combined by the effect of high temperature, salt and alkali takes place according to U.S. Pat. 281593 by filling the pores of the starting silica gel with a mixture of a neutral inorganic salt that acts as a reinforcement during the process and an inorganic salt which releases alkali upon annealing, followed by annealing to 600-800 ° C for 2-5 hours. After the annealing is complete, the salts are washed out of the system with water and the expanded pore silica gel is dried. The principle of preparation of spherical silica particles of high purity and controlled pore size according to patent application PP 1998-4027 is that a suitably diluted colloidal silica dispersion with the addition of an alkali silicate is introduced into an organic phase consisting of a mixture of aliphatic and aromatic hydrocarbons or water-immiscible derivatives and alkyd resins thereof, and after mixing, an amount of acid miscible with the organic and aqueous phases used is added to the emulsion to form hydrogel formation conditions upon diffusion of the acid into the aqueous phase droplets.
Silikagél s makroporéznou štruktúrou sa podľa patentu č. 265 588 pripravuje pôsobením kyseliny boritej alebo jej zmesí so soľami alkalických kovov na mikroporézny silikagél pri vysokých teplotách.Silica gel with macroporous structure according to U.S. Pat. 265 588 prepares microporous silica gel by treatment with boric acid or mixtures thereof with alkali metal salts at high temperatures.
Sférické častice oxidu kremičitého SiO2 získané riadeným lúhovaním s požadovanou veľkosťou a povrchom sa podľa patentu GB 369283 A 19310401 získavajú pri lúhovaní olivínu.According to GB 369283 and 19310401, the spherical SiO 2 particles obtained by controlled leaching with the desired size and surface are obtained by leaching olivine.
Nevýhodou doteraz známych spôsobov výroby silikagélu je, že nevyužívajú možnosť kontrolovaného režimu chladenia, mrazenia a podtlakového sušenia a následného čistenia. Oxid kremičitý SiO2 získaný spracovaním serpentinitovej nerastnej suroviny minerálnymi kyselinami sa ďalej nespracováva na silikagél s obsahom SiO2 nad 99 %, ktorého častice by mali sférický tvar, riadenú veľkosť a hladkosť stien, a ktorý by bol vhodný na výrobu rôznych produktov v špeciálnom odvetví sklárskeho priemyslu na výrobu kremenného skla a v stĺpcovej chromatografii.A disadvantage of the previously known processes for the production of silica gel is that they do not make use of the controlled cooling, freezing and vacuum drying and subsequent purification modes. The silica SiO 2 obtained by treating the serpentinite mineral with mineral acids is not further processed into silica gel with a content of SiO 2 above 99%, the particles of which have a spherical shape, controlled size and wall smoothness, and which would be suitable for various products in the specialty glass industry the silica glass industry and column chromatography.
Podstata vynálezuSUMMARY OF THE INVENTION
Podstatou vynálezu je spôsob výroby silikagélu s hladkým povrchom stien sférických častíc zo serpentinitu a jeho kontrolovaný režim chladenia, mrazenia a sušenia, ktoré majú významný vplyv na spájanie pórov, ich sferoidizáciu a vznik hladkého povrchu stien. Silikagél s hladkým povrchom stien sférických častíc sa získa z kremičitanového roztoku alkalického kovu a jeho polykondenzáciou, ktorému predchádza príprava oxidu kremičitého SiO2 s obsahom nad 98 hmotn. % oxidu kremičitého SiO2 pôsobením anorganickej kyseliny na oxid kremičitý SiO2 s obsahom do 98 hmotn. % oxidu kremičitého SiO2 pri teplote 80 °C až 105 °C. Vzniknutá suspenzia oxidu kremičitého SiO2 a anorganickej kyseliny sa po odstránení prímesí oxidu kremičitého SiO2 ochladí a prefiltruje. Kvapalný produkt reakcie obsahuje stopové množstvá solí železa, hliníka, vápnika a ďalších chemických prvkov. Tuhý zvyšok po lúhovaní s obsahom nad 98,5 hmotn. % oxidu kremičitého SiO2 sa odfiltruje, premýva destilovanou vodou do dosiahnutia neutrálneho pH a suší pri teplote 105 °C.SUMMARY OF THE INVENTION The present invention is directed to a process for the production of smooth wall surface silica gel from serpentinite and its controlled cooling, freezing and drying mode, which have a significant effect on pore bonding, spheroidization and smooth wall surface formation. Silica gel with a smooth surface of the walls of the spherical particles is obtained from an alkali metal silicate solution and its polycondensation, which is preceded by the preparation of SiO 2 with a content above 98 wt. % Of silica SiO 2 by treatment with a mineral acid to the silicon dioxide SiO 2 with up to 98 wt. % SiO 2 silica at 80 ° C to 105 ° C. The resulting slurry of SiO 2 and inorganic acid is cooled and filtered after removal of the SiO 2 additive. The liquid reaction product contains trace amounts of iron, aluminum, calcium and other chemical elements. The solid residue after leaching above 98.5 wt. % SiO 2 is filtered off, washed with distilled water to neutral pH and dried at 105 ° C.
Kremičitanový roztok alkalického kovu s pH 13 bez nerozpustených prímesí sa získa chemickou reakciou oxidu kremičitého SiO2 s obsahom nad 98,5 hmotn. % oxidu kremičitého SiO2 s roztokom hydroxidu alkalického kovu v mólových pomeroch od 1 : 2 do 4 : 1 a filtráciou pri teplote do 60 °C. Zníženie pH na 10 kremičitanového roztoku alkalického kovu sa dosiahne pridaním oxidačného činidla a silnej anorganickej kyseliny. Koloidný roztok na báze kyseliny hydrogénkremičitej, z ktorého sa polykondenzáciou vylúči bielomliečny rôsolovitý gél - hydrogél, sa vytvorí okyslenim kremičitanového roztoku alkalického kovu. Kvapalná časť roztoku obsahujúca soľ alkalického kovu sa filtráciou oddelí od gélovitej zrazeniny.An alkali metal silicate solution of pH 13 without undissolved impurities is obtained by chemical reaction of SiO 2 with a content above 98.5 wt. % SiO 2 with an alkali metal hydroxide solution in molar ratios of 1: 2 to 4: 1 and filtration at a temperature of up to 60 ° C. The pH is lowered to 10 with an alkali metal silicate solution by adding an oxidizing agent and a strong inorganic acid. The colloidal silicic acid solution, from which a white-milk jelly gel-hydrogel is precipitated by polycondensation, is formed by acidifying the alkali metal silicate solution. The liquid part of the solution containing the alkali metal salt is separated from the gel-like precipitate by filtration.
Podstatou vynálezu je kontrolovaný režim chladenia, mrazenia a sušenia, ktorý vplýva na spájanie pórov, sferoidizáciu častíc a hladkosť povrchu stien a je podstatou silikagélu s hladkým povrchom stien sférických častíc z oxidu kremičitého SiO2 zo serpentinitu. Rovnomerné znižovanie teploty hydrogélu na teplotu 4 až 0,5 °C má rýchlosť cca l'Cmin/1 a zmrazovanie na teplotu nižšiu ako -15 °C konštantnú rýchlosť 2 - 4 “Crnin.1. Silikagél vzniká samovoľným rozmrazením hydrogélu uvoľnením viazanej vody, ktorá sa odfiltruje. Silikagél s hladkým povrchom stien sférických častíc vzniká riadeným sušením pri teplote 105 °C a podtlaku. Zvýšenie obsahu oxidu kremičitého SiO2 nad 99 hmotn. % v silikagéli sa dosiahne jeho zdrobnením a lúhovaním v anorganickej kyseline, premývaním destilovanou vodou do dosiahnutia neutrálneho pH a sušením pri teplote 105 °C.The present invention provides a controlled cooling, freezing, and drying regime that affects pore bonding, particle spheroidization, and wall surface smoothness and is the essence of silica gel with a smooth wall surface of spherical SiO 2 particles of serpentinite. Evenly lowering the temperature of the hydrogel to a temperature of 4 to 0.5 ° C has a rate of about 1'Cmin / L and freezing to a temperature below -15 ° C a constant rate of 2-4 ° C. 1 . Silica gel is formed by spontaneously thawing a hydrogel by releasing bound water, which is filtered off. Silica gel with a smooth surface of the walls of spherical particles is produced by controlled drying at 105 ° C and vacuum. Increasing the SiO 2 content above 99 wt. % in silica gel is obtained by crumbling and leaching in inorganic acid, washing with distilled water to neutral pH and drying at 105 ° C.
Výhodou vynálezu je spôsob výroby silikagélu s hladkým povrchom stien sférických častíc s obsahom SiO2 nad 99 hmotn. % a merným povrchom do 200 m2g_I, ktorý je vhodný na využitie v stĺpcovej chromatografii a vo výrobe kremenných skiel na optické účely, optoelektronické účely, špeciálne vrstvy v oblasti elektroniky a kremenné kapiláry.An advantage of the invention is a process for the production of silica gel having a smooth surface of the walls of spherical particles with SiO 2 content above 99 wt. % and a specific surface area of up to 200 m 2 g- I , which is suitable for use in column chromatography and in the production of quartz glasses for optical purposes, optoelectronic purposes, special layers in the field of electronics and quartz capillaries.
Príklady uskutočnenia vynálezuDETAILED DESCRIPTION OF THE INVENTION
Silikagél s hladkými stenami sférických častíc, s obsahom 99,3 hmotn. % oxidu kremičitého SiO2 a s merným povrchom 190 m2g’', sa získa, ak sa na oxid kremičitý s obsahom 97,8 hmotn. % pôsobí 20 % kyselinou chlorovodíkovou HCl v hmotnostnom pomere oxidu kremičitého SiO2 a kyseliny chlorovodíkovej HCl 1 : 4 počas 2 hod. pri teplote 105 °C za súčasného miešania suspenzie. Suspenzia tuhého oxidu kremičitého SiO2 a rozpustených chloridov sa ochladí a prefiltruje. Tuhý zvyšok oxidu kremičitého SiO2 s obsahom 98,9 hmotn. % sa premýva destilovanou vodou do neutrálneho pH a suší pri teplote 105 °C.Silica gel with smooth walls of spherical particles, containing 99.3 wt. % SiO 2 silica and a specific surface area of 190 m 2 g -1 is obtained when a silica content of 97.8 wt. % Treated with 20% hydrochloric acid HCI in a ratio by weight of silica SiO2 and hydrochloric acid HCl 1: 4 in 2 hours. at 105 ° C while stirring the suspension. The slurry of solid SiO 2 and dissolved chlorides was cooled and filtered. A solid residue of SiO 2 containing 98.9 wt. % was washed with distilled water to neutral pH and dried at 105 ° C.
Roztok kremičitanu sodného Na2SiO3 bez nerozpustných zvyškov, ktorého pH je 13, sa získa chemickou reakciou oxidu kremičitého SiO2 s obsahom 98,9 hmotn. % s roztokom hydroxidu sodného NaOH s koncentráciou 1 mol. dm'3 v mólovom pomere 1 : 2 pri teplote 60 °C a filtráciou.An insoluble residue sodium silicate solution of Na 2 SiO 3 , whose pH is 13, is obtained by a chemical reaction of SiO 2 with a content of 98.9% by weight. % with a 1 mol. dm ' 3 at a molar ratio of 1: 2 at 60 ° C and filtration.
Filtrácia kremičitanu sodného Na2SiO2 prebieha ihneď po skončení reakcie, pretože pôsobením oxidu uhličitého CO2 zo vzduchu sa začne vo výluhu tvoriť kyselina kremičitá vo forme rôsolu. Filtráciou sa odstránia nerozpustené zvyšky SiO2 a prípadné nečistoty.Filtration of the sodium silicate Na 2 SiO 2 takes place immediately after completion of the reaction, as the action of the CO2 in the air is started in the extract to form silica in gel form. Filtration removes undissolved SiO 2 residues and any impurities.
K roztoku kremičitanu sodného Na2SiO3 sa pridá oxidačné činidlo peroxid vodíka H2O2 a jeho okyslením kyselinou chlorovodíkovou HCl čistoty p. a. na pH 10 polykondenzáciou vzniká koloidný roztok na báze kyseliny hydrogénkremičitej, z ktorého sa neskôr vylúči bielomliečny rôsolovitý gél - hydrogél a roztok chloridu sodného NaCl, ktorý sa odfiltruje.To the sodium silicate solution of Na 2 SiO 3 , the oxidizing agent hydrogen peroxide H 2 O 2 is added and acidified with hydrochloric acid HCl of purity pa to pH 10 by polycondensation to form a colloidal silicic acid solution, which later precipitates a white milky jelly gel-hydrogel. NaCl, which was filtered off.
Rovnomerné chladenie celého objemu gélovitej zrazeniny hydrogélu z laboratórnej teploty na teplotu 0,5 °C prebieha rýchlosťou cca 1 °C min.'1. Nasledujúce zmrazenie celého objemu gélovitej zrazeniny na teplotu -15 °C prebieha konštantou rýchlosťou 3 °C min.’1 počas 3 hod. Samovoľným rozmrazením gélovitej zrazeniny pri laboratórnej teplote sa vylúči časť vody viazanej v géli a hydrogél sa stáva aktívny silikagél. Uvoľnená voda sa odfiltruje od nerozpustného silikagélu. Nasleduje riadené podtlakové sušenie pri teplote 105 °C a podtlaku pod 0,1 kPa, pričom vzniká amorfný dehydratovaný silikagél.The entire volume of the gel-like hydrogel precipitate is uniformly cooled from room temperature to 0.5 ° C at a rate of about 1 ° C min. 1 . The following freezing of the entire gel precipitate to -15 ° C is carried out at a constant rate of 3 ° C min. 1 for 3 hours By self-thawing the gel precipitate at room temperature, some of the gel-bound water precipitates and the hydrogel becomes active silica gel. The liberated water is filtered off from insoluble silica gel. This is followed by controlled vacuum drying at 105 ° C and a vacuum below 0.1 kPa to give amorphous dehydrated silica gel.
Čistenie tuhého nerozpustného silikagélu sa uskutočňuje po rozdrobení silikagélu za stáleho miešania v 30 % kyseline dusičnej HNO3. Vyčistený silikagél, ktorého obsah oxidu kremičitého SiO2 je 99,3 hmotn. %, sa odfiltruje, prímesi dusičnanov ostávajú v kvapalnom filtráte. Silikagél sa premýva destilovanou vodou až do neutrálneho pH a suší pri teplote 105 °C. Výsledkom sú sférické častice amorfného dehydratovaného silikagélu s hladkou povrchovou morfológiou, obsahom oxidu kremičitého 99,3 hmotn. % a merným povrchom 190 m2g ', ktoré sú vhodné na výrobu kremenných skiel alebo v stĺpcovej chromatografii.Purification of the solid insoluble silica gel is carried out after comminution of the silica gel with stirring in 30% nitric acid HNO 3 . Purified silica gel having a SiO 2 content of 99.3 wt. %, the nitrate admixtures remain in the liquid filtrate. The silica gel is washed with distilled water to neutral pH and dried at 105 ° C. The result is spherical particles of amorphous dehydrated silica gel with a smooth surface morphology with a silica content of 99.3 wt. % and a specific surface area of 190 m 2 g ', which are suitable for the production of quartz glasses or in column chromatography.
Priemyselná využiteľnosťIndustrial usability
Spôsob výroby silikagélu s hladkým povrchom stien sférických častíc z oxidu kremičitého SiO2 zo serpentinitovej nerastnej suroviny je možné využívať v priemysle.The process for producing silicagel having a smooth wall surface of spherical SiO 2 particles from a serpentinite mineral can be used in industry.
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