CS209389B1 - Method of preparation of diamminosilver tetraborate - Google Patents

Method of preparation of diamminosilver tetraborate Download PDF

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CS209389B1
CS209389B1 CS168280A CS168280A CS209389B1 CS 209389 B1 CS209389 B1 CS 209389B1 CS 168280 A CS168280 A CS 168280A CS 168280 A CS168280 A CS 168280A CS 209389 B1 CS209389 B1 CS 209389B1
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solution
borohydride
diammonium
application
enamel
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CS168280A
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Czech (cs)
Slovak (sk)
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Jan Lezovic
Jozef Kasa
Jan Medved
Mirek Filak
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Jan Lezovic
Jozef Kasa
Jan Medved
Mirek Filak
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(54) Sposob přípravy roztoku štvorboritanu diamostriebomého(54) Method for preparing a diammonium borohydride solution

Vynález sa týká spósobu přípravy roztoku štvorboritanu diamostriebomého vzorca:The present invention relates to a process for the preparation of a solution of diammonium borohydride of the formula:

II H \ ZII H \ Z

H-N — Ag — N —H / vH-N-Ag-N-H / v

HOHO

B.B.

OHOH

II

B — Β--“ \B - Β-- "\

B — OHB - OH

2OH ktorý možno použit’ v stomatologii ako prevenčný prostriedok proti zubnému kazu a mikrobiálnemu zápalu slizníc ústnej dutiny a parodontálnych chobotov.2OH which can be used in dentistry as a preventive measure against caries and microbial inflammation of oral mucosa and periodontal trunks.

Boritany sú zlúčeniny, ktorých základnými štruktúmymi jednotkami aniónov sú trojuholníkové skupiriy BO3 alebo tetraedrické skupiny BO4. Tieto skupiny sa spájajú spoločnými atómami kyslíka a vytvárajú tak polyméme reťazce alebo kruhové útvary.Borates are compounds whose basic anionic structural units are the BO 3 triangular groups or the BO 4 tetrahedral groups. These groups are joined by common oxygen atoms to form polymer chains or ring shapes.

Pripravujú sa reakciami roztokov kyseliny trihydroboritej s hydroxidmi alkalických kovov, alebo tavením kyseliny trihydroboritej s kysličníkmi, připadne hydroxidmi kovov (J. Gažo et al. Všeobecná a anorganická chémia, Bratislava 1974; H. Remy, Anorganická chemie, I díl, Praha 1971). Vo vodě sa rozpúšťajú len boritany alkalických kovov.They are prepared by reaction of borohydride solutions with alkali metal hydroxides, or by melting borohydride acid with oxides or metal hydroxides (J. Gažo et al. General and Inorganic Chemistry, Bratislava 1974; H. Remy, Inorganic Chemistry, Part I, Prague 1971). Only alkali metal borates dissolve in water.

Štvorboritan dvojstriebomý je biela kryštalická látka, vo vodě slabo rozpustná, rozpustná v kyselinách (R. C. Weast, Handbook of Chemistťý and Physics, Cleveland 1969). Kyslé roztoky však nie sú vhodné pre použitie v stomatologii, nakolko kontaminujú tkanivá ústnej dutiny.Dichloromethane is a white crystalline substance, slightly soluble in water, soluble in acids (R. C. Weast, Handbook of Chemist & Physics, Cleveland 1969). However, acidic solutions are not suitable for use in dentistry as they contaminate oral tissues.

Vyššie uvedené nedostatky sú odstránené podlá vynálezu, ktorého podstata spočívá v tom, že 1 mol štvorboritanu dvojstriebomého sa rozpustí v 4 moloch 10 až 25 %-nom hydroxide amónnom. Vzniklý roztok štvorboritanu diamostriebomého upravíme zriedením destilovanou vodou s výhodou na 3 až 5 %-ný hmot. %-ný roztok, pretože koncentrovanejšie roztoky sú nestále. Sposob prí209389 pravý a použitie štvorboritanu diamostriebomého v stomatologii nebolo zatial v Uteratúre opísané.The aforementioned drawbacks are eliminated according to the invention, which consists in dissolving 1 mol of dibasic borohydride in 4 moles of 10 to 25% ammonium hydroxide. The resulting diammonium borohydride solution is adjusted to 3 to 5 wt.% By dilution with distilled water. % solution because more concentrated solutions are unstable. The method of genuine and the use of diammonium borohydride in dentistry has not yet been described in Uteratura.

Spósobom podlá vynálezu sa získá roztok štvorboritanu diamostrieborného o koncentráeii 3 až 5 hmot. %-nej, ktorý je vyznačený oxidoredukčnými vlastnosťami, preto nesmie prísť do styku s kovmi a organickými zlúčeninami, ktoré majú redukčně vlastnosti. 3 až 5 hmot. %-ný roztok je stály pri vyiúčení ultrafialovej a viditelnej oblasti 5 světla (o vlnovej dížke od 200 nm do 750 nm) a pri í teplotách od 0 do 20 °C. Výrobný postup je jednoduchý, nevyžaduje náročné výrobně zariadenia a energiů.According to the invention, a solution of diammonium borohydride having a concentration of 3 to 5% by weight is obtained. %, which is characterized by oxidative reduction properties, must therefore not come into contact with metals and organic compounds having reducing properties. 3 to 5 wt. The% solution is stable at the ultraviolet and visible region 5 of light (wavelength from 200 nm to 750 nm) and at temperatures from 0 to 20 ° C. The manufacturing process is simple, it does not require demanding production equipment and energy.

Příklad 1.Example 1.

407,01 g štvorboritanu dvojstriebomého Ag2[B4O5(OH)4] (1 mol) sa rozpustí v 560,736 g 25 %-néhó roztoku NH4OH (4 moly), za stálého miešania pri červenom svetle (o vlnovej dížke nad 750 nm), pretože vzniknutá komplexná zlúčenina štvorboritanu diamostriebomého je pri svetle o vlnovej dížke od 200 nm do 750 nm nestála, pričom dochádza k jej redukcii. Získaný roztok štvorboritanu diamostriebomého zriedime 8975,7 ml destilovanej vody na kóncentráciu 5 hmot. %-nú. Analýza:Dissolve 407,01 g of Ag 2 [B 4 O 5 (OH) 4 ] borohydride (1 mol) in 560,736 g of a 25% NH 4 OH solution (4 moles), with stirring under red light (wavelength) above 750 nm), because the resulting diammonium borohydride complex compound is unstable in light with a wavelength of from 200 nm to 750 nm and is reduced. The resulting diammonium borohydride solution is diluted with 8975.7 ml of distilled water to a concentration of 5 wt. % Sequence. analysis:

ml roztoku štvorboritanu diamostriebomého sa zríedilo 200 ml destilovanej vody a mřeme okyslilo kys. dusičnou. Získaný roztok sa zahrial temer k varu a za stálého miešania sa přidávala 5 %-ná kyselina chlorovodíková tak dlho, až sa dalším přidáváním kyseliny přestane tvoriť zrazenina chloridu striebomého. Roztok só zrazeninou sa, nechal ná trriavom mieste vychladnúť. Zrazenina sa odfiltrovala céz filtračný téglik a premývala destilovanou vodou slabo okyslenou kys. dusičnou, ked už filtrát nereaguje s roztokom dusičňanu striebomého na chloridy. Nakoniec sa zrazenina chloridu striebomého v tégliku ešte premyla čistou destilovanou vodou a vysušila pri 130 °C do konštantnej váhy. Priemer z troch stanovení Ag vo form.e AgCl = 3,5780 g, čo odpovedá teoretické,,mu obsahu Ag v 5 hmot. %-nonji roztoku štvorbo; ritánta diamostriebomého.ml of diammonium borohydride solution was diluted with 200 ml of distilled water and acidified with acid. nitric acid. The resulting solution was heated to near boiling and 5% hydrochloric acid was added with stirring until the addition of the acid no longer formed the silver chloride precipitate. The precipitate solution was allowed to cool in a frost-free place. The precipitate was filtered through a filter crucible and washed with distilled water with slightly acidified acid. nitric acid when the filtrate no longer reacts with the silver nitrate solution to the chloride. Finally, the silver chloride precipitate in the crucible was still washed with pure distilled water and dried at 130 ° C to constant weight. The average of three Ag determinations in the form of AgCl = 3.5780 g, which corresponds to a theoretical Ag content of 5 wt. % of non-quaternary solution; ritánta diamostriebomého.

'........II! ' FyZikálno-chemické vlastnosti:'........ II! 'Physical-chemical properties:

jimot. %-ný roztok štvorboritanu diamostrieborriého je bezfarebná číra kvapalina, je citlivá na světlo; o vlnovej dížke od 200 nm do 750 nm, pričom sa rozkládá za vzniku tmavých kovových povíakov. Ďalej sa redukuje niektórými kovmi,Jimo. The di-diammonium borohydride solution is a colorless, clear, light-sensitive liquid; having a wavelength from 200 nm to 750 nm, decomposing to form dark metal binders. It is further reduced by nectal metals,

Claims (3)

PREDMETSUBJECT Spósob přípravy roztoku štvorboritanu diamostriebomého vzorca “x ijí-N — Ag — N — H ' / κProcess for preparing a di-ammonium borohydride solution of the formula xi-N-Ag-N-H '/ κ H XH organickými a anorganickými zlúčeninami majúcimi redukčně vlastnosti až na kovové striebro. Roztok je stály pri vylúčení světla o vlnovej dížke od 200 nm do 750 nm a teplóte od 0 °C do 20 °C. Má báktericídne vlastnosti.H X H organic and inorganic compounds having reducing properties down to metallic silver. The solution is stable to the exclusion of light having a wavelength of from 200 nm to 750 nm and a temperature of from 0 ° C to 20 ° C. It has bactericidal properties. Prjklad 2.Example 2. 407,01 g štvorboritanu dvojstriebomého407.01 g of dibasic borohydride A^2[B4OS(OH)4] (1 mol) sa rozjpustí v 1401,84 g 10 %-néhó NH4OH (4 moly) ochladeného na 5 °C zaf stálého miešania pri červenou svetle (o vlnovej dížke nad 750 nm), pretože vzniknutá komplexná zlúčenina štvorboritanu diamostriebomého je pri svetle o vlnovej dížke od 200 nm do 750 nm nestála a rozkládá sa. Získaný roztok štvorboritanu diamostriebomého sa zriedi 14 461,2 ml destilovanou vodou na 3 hmot. %-nú kóncentráciu.A ^ 2 [B 4 O S (OH) 4 ] (1 mol) was dissolved in 1401.84 g of 10% NH 4 OH (4 mol) cooled to 5 ° C with stirring under red light (wavelength) above 750 nm), since the resulting diammonium borohydride complex compound is unstable and decomposes under light at 200 nm to 750 nm. The resulting diammonium borohydride solution was diluted with 14,461.2 ml of distilled water to 3 wt. % concentration. Z 3 až 5 hmot' %-ného roztoku štvorboritanu diartiostriebomého sa připraví aplikačný 10-4 až ÍO-2 hmot. %-ný roztok štvorboritanu diamostriebomého vo formě vodného alebo 15 až 40 %-ného vodnoetanolického roztoku pre stomatologické účely. Tieto roztoky nie sú toxické, sú báktericídne a í majú adsorpčné schopnosti na plak zubnej skloviny a zubnú sklovinu..An application rate of 10 -4 to 10 -2 wt.% Is prepared from a 3 to 5 wt. % diammonium borohydride solution in the form of an aqueous or 15 to 40% aqueous ethanol solution for dental purposes. These solutions are non-toxic, are bactericidal and have adsorptive properties on enamel plaque and enamel. Toxicita aplíkačného 10-4 až 10-2 hmot. %-ného .roztoku štvorboritanu diamostriebomého vo formě vodného roztoku bola testovaná na pokusných myšiach intravenózne a peroláme (1 ml aplíkačného roztoku na 20 g žívej váhy), pričom sa _ zistjlo, že látka nepósobí toxicky.Toxicity of application 10 -4 to 10 -2 wt. The diammonium tetrachloride borohydride solution in the form of an aqueous solution was tested in experimental mice intravenously and perol (1 ml of application solution per 20 g body weight), and the substance was found not to be toxic. Baktéricídnosť aplíkačného roztoku štvorboritanu niarriostrietodriiéHo (10~4 až 10-2 hmot. %) vo foipie 15 % -ného vodnoetanolického roztoku bola testovaná na aeróbnu a anaeróbnu mikroflóru ústnej dutiny, ktorej kyslé produkty spósobujú kazivosť zubov, zápal slizníc a parodontálnych choboťov,’ pričom sa zistilo, že k uhynutiu mikroflóry dochádza za 30 sekúnd, bez toho, že by nastala kontaminácia slizníc ústnej dutiny.Baktéricídnosť štvorboritanu niarriostrietodriiéHo treatment solution (~ 10 4 to 10 -2 wt.%) In 15% strength FoIP vodnoetanolického solution was tested for aerobic and anaerobic microflora of the oral cavity, wherein the acid product of the process tooth decay, periodontal and mucosal inflammation trunk, "the Microflora death was found to occur within 30 seconds without contamination of the oral mucosa. Adsorpcia aplíkačného roztoku štvorboritanu diamostriebomého na plak zubnej skloviny a zubnjú sklovinu sa dokázala stanovením Ag pomoeou elektrónovej mikrosondy (RTG — mikroanalýza) a spektrochemicky.The adsorption of the diammonium borohydride application solution to enamel plaque and dental enamel was determined by Ag determination by electron micro-probe (X-ray microanalysis) and spectrochemically. Stabilita 3 až 5 hmot. %-ného roztoku štvorboritanu diamostriebomého z ktorého sa pripravujú • aplikačně roztoky sa kontrolovala stanovením Ag gravimetricky v jednomesačných intervaloch po dobu 2 rokov, pričom sa jeho 3 až 5 hmot. %-ná i koncentrácia prakticky nezměnila.Stability of 3 to 5 wt. % of the di-ammonium borohydride solution from which the application solutions are prepared was checked by Ag determination gravimetrically at one-month intervals for 2 years, with its 3 to 5 wt. The concentration was practically unchanged. -.«·-. "· VYNÁLEZU /OF THE INVENTION / HO — BHO - B ΌΌ OHOH I — B — \ \I - B - B — OH zB - OH z 2209389 vyznačujúci sa tým, že štvorboritan dvojstrieborný vzorca Ag2[B4O5(OH)4] sa nechá zreagovať s 10 až 35 %-ným vodným roztokom hydroxidu amonného v molámom pomere 1 :4, získaný roztok štvorboritanu diamostriebomého sa popřípadě .2209389, characterized in that the bivalent silver borohydride of formula Ag 2 [B 4 O 5 (OH) 4 ] is reacted with a 10 to 35% aqueous ammonium hydroxide solution in a molar ratio of 1: 4, the resulting diammonium borohydride solution optionally. upraví zriedením destilovanou vodou s výhodou na 3 až 5 %-nú koncentráciu, pričom celý postup sa vykonává pri červenám svetle o vlnovej dížke nad 750 nm.by dilution with distilled water, preferably to a concentration of 3-5%, the whole process is carried out in red light with a wavelength above 750 nm.
CS168280A 1980-03-12 1980-03-12 Method of preparation of diamminosilver tetraborate CS209389B1 (en)

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