CS268589B1 - The method of regenerating the phosphate cat - Google Patents

The method of regenerating the phosphate cat Download PDF

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Publication number
CS268589B1
CS268589B1 CS8829A CS2988A CS268589B1 CS 268589 B1 CS268589 B1 CS 268589B1 CS 8829 A CS8829 A CS 8829A CS 2988 A CS2988 A CS 2988A CS 268589 B1 CS268589 B1 CS 268589B1
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Czechoslovakia
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phosphate
sludge
reaction mixture
phosphoric acid
phosphating
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CS8829A
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Czech (cs)
Slovak (sk)
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CS2988A1 (en
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Ernest Ing Hradsky
Jan Hudak
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Hradsky Ernest
Jan Hudak
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Priority to CS8829A priority Critical patent/CS268589B1/en
Publication of CS2988A1 publication Critical patent/CS2988A1/en
Publication of CS268589B1 publication Critical patent/CS268589B1/en

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Abstract

Resenie sa týká sposobu regenerácle a spltnáho využitie fosfátového katu ako technologického odpadu prt chealckej úprava povrchu kovových Materlálov fosfátovaní· obsahujůcl převážná fosforečnan železltý a připadne fosforečnan zlnočnatý a/alebo fosforečnan aenganetý v poaere podlá zaatúpenla v základnej fosfátovecej zaesl. Podía rleienla sa na kal, zrjedený vodou v poaere 1 ku 0,5 až 0,6 posobl technickou kyselinou sirovou o anožstve v roztahu 101 až 102 X haotnostných voči jej teoretlckáau anožstvu zodpovedajúceau obsahu fosforu v kale a to za neustálého ■leianla reakčnej zaesl a jej zohrlevanla po dobu odpařeni» 70 až 75 X objeau. 5aí lej sa reakčná zaet achladzuje po dobu vytvorenla kryltálov síranu železitého, prlčoa aa filtrát kyseliny fosforečnej odsává a odvádza do zásobnlka pře dalile použitie. Filtrát .kyseliny fosforečnej ta Sálej zahustuje a doplňuje ostatnýal ztožkaal fosfátovacej zaesl s prlvádza sa k spotřebičů.The solution concerns the method of regeneration and full utilization of phosphate sludge as a technological waste for the chelating treatment of the surface of metal phosphating materials containing mainly iron phosphate and possibly sulfur phosphate and/or ferrous phosphate in the air according to the quenching in the basic phosphate feed. The stage was based on the sludge, diluted with water in the air 1 to 0.5 to 0.6, supplemented with technical sulfuric acid with a concentration in the range of 101 to 102 X relative to its theoretical concentration corresponding to the phosphorus content in the sludge, and this was carried out under a constant reaction mixture and heated for an evaporation period of 70 to 75 X volume. After that, the reaction mixture is cooled until the ferric sulfate crystals have formed, and the phosphoric acid filtrate is sucked off and transferred to a reservoir for further use. The phosphoric acid filtrate thickens and replenishes the rest of the phosphatizing agent and is transported to the appliances.

Description

Vynález sa týká aposobu regeneráde fosfátového kalu najal ako technologického odpadu pri chemickej úprav· povrchu kovových materiálov fosfátovaní· například pr«d elektroforéznom nenálanl lakov na radiátory a rleli probléa spltného využltia jeho zložiek.The invention relates to a process for the regeneration of phosphate sludge hired as a technological waste in the chemical surface treatment of metallic materials by phosphating, for example before electrophoretic non-nanopainting varnishes for radiators and solving the problem of full utilization of its components.

Doteraz používané technologické postupy fosfátového a prs chemická ůprsvu kovového povrchu poskytujů ako technologický odpad foafátový kal tvořený prevážne fosforečnanoa železltým v aprlevode nepodstatného množstva fosforečnanu zinočnatého, a/alebo aanganatáho, podta použitého foafátového přípravku. Uvedený kel ako technologický odped pri chemickej úpravě kovových výrobkov, najal ocetových, ako například karosérii automobilov, panelových doškových radlátorov o pod. doslat neaá použitie e vynáža sa na kalové depónie a haldy, kde znečlstuje okolie. Nevyužitý fosfatizačný kel obsehuje pritoa cennú kyselinu fosforečná, 1ba dovážená.Previously used technological processes of phosphate and breast chemical surface of the metal surface provide as technological waste folate sludge consisting mainly of phosphate and iron in water and in insignificant amounts of zinc phosphate, and / or agananate, according to the used folate preparation. The said tusk, as a technological waste in the chemical treatment of metal products, hired vinegar, such as car bodies, thatched panel radiators, etc. send its use to sludge landfills and heaps where it pollutes the environment. Unused phosphating sludge contains very valuable phosphoric acid, which is imported.

Uvedený probléa rleii sposob regenerácie fosfátového kalu ako technologického odpadu pře uvedený áčel podta vynálezu. Podstata vynálezu spoiiva v toa, že na fosfátový kal, po zrledenl vodou v poaere 1 ku 0,5 až 0,6 sa posobl technickou kysel lnou'*1novou o anožstve v.rozsahu 101 až 102 X haotnostných voči jej teoretickéau množstvu zodpovedajácemu obsahu fosforu v kale. Přidávaní# kyseliny sirovej ss deje za neustálého eieiania reakčnej zmesi e jej zohrievanla po dobu odparenia 70 až 75 X jej objemu. Sálej sa reakčná zaes schladzuje po dobu vytvorenia kryitálov síranu železitého a filtrát kyseliny fosforečnej ss odsává a odvédza do zásobnika pře taille použitie. S výhodou sa filtrát kyseliny fosforeinej dalej zahustuje a po doplněni ostatnýai zložkaai fosfátovacej zaesl, sa prlvádza k spotřebičů.Said problem is a method of regenerating phosphate sludge as technological waste according to the present invention. The essence of the invention is that the phosphate sludge, after glazing with water in an amount of 1 to 0.5 to 0.6, was treated with technical acid of a quantity in the range of 101 to 102% by weight relative to its theoretical amount corresponding to the phosphorus content. v kale. The addition of # sulfuric acid is carried out while constantly stirring the reaction mixture and heating it to an evaporation time of 70 to 75% of its volume. The reaction mixture is cooled until ferric sulfate crystals are formed and the phosphoric acid filtrate is filtered off with suction and taken up in a container for pre-use. Preferably, the phosphoric acid filtrate is further concentrated and, after replenishing the other phosphate components, is passed to the appliances.

Hlavnou výhodou sposobu podta vynálezu je jednoduchá regenerácia kyseliny fosforečnej bez vysokých nárokov na regeneračné zariadenie e úspora tejto deflcitnej suroviny pre přípravu fosfátbvacej zaesl. Pritoa je aožné využit technická alebo inak opotřebovaná kyaeHnu sírová a v konečnou’dósledku zlepienie ekologických podalenok a zážitkovanle odpadného produktu na daliie rózne využitie ako sá kvapalné odhrdzovače, pevné brásne pasty alebo eko hnojivo pre potnohospodárske áčely.The main advantage of the process according to the invention is the simple regeneration of phosphoric acid without the high demands on the regeneration device and the saving of this deficient raw material for the preparation of the phosphating salt. It is possible to use technical or otherwise worn kyaeHnu sulfur and, ultimately, to improve the ecological subsoil and experience of the waste product for various uses such as liquid rust removers, solid soil pastes or eco-fertilizer for agricultural purposes.

PřikladExample

Boto použité fosfátového kalu, vysuSeného pri 105 °C. Obsah P v kale podte analýzy bol 15,66 X. Z uvedeného kalu sa nevážilo 300 g e v sklenej kádinko sa k nesu přidalo 150 al vody a postupné po aalých dávkách 128 al 98 X HgSO^ o hustotě 1,84, za intenzlvneho aieianla reakčnej zmesi. Reakčná zaes.sa potom zahriala do jej teploty varu a za občasného premielanla skleněnou tyčinkou sa zmes zahustila na 1/4 povodního objemu. Odparenie vody prebfehalo po dobu 1 h a 40 minůt. Po ochládáni reakčnej zmesi sa vykryčtalizovaný síran železitý odfiltroval na papierovoa filtri pomocou vákua. Získaný surový stran železitý sa použil ako základná surovina pre Callie použitie. Získaný filtrát obsahuje kyselinu fosforečná s výtažkem - 150 g H^PO^ /98 X výtažok/.Phosphate sludge dried at 105 ° C was used. The content of P in the sludge according to the analysis was 15.66 X. From the said sludge was not weighed 300 g in a glass beaker was added 150. . The reaction mixture was then heated to reflux and, occasionally stirred with a glass rod, the mixture was concentrated to 1/4 flood volume. Evaporation of water took place for 1 hour and 40 minutes. After cooling the reaction mixture, the crystallized ferric sulfate was filtered off on a paper filter under vacuum. The obtained ferrous ferric side was used as a basic raw material for Callie use. The filtrate obtained contains phosphoric acid in a yield of 150 g of H 2 PO 4 (98% yield).

Claims (1)

PREDMET VYNXlEZUSUBJECT OF EXPRESSION Sposob regenerácie fosfátového kalu najali ako technologického odpadu pri chaaickaj úprava povrchu kovových materiálov fosfátovaní· obsahujůceho převážná fosforečnan železitý a připadne fosforečnan zinočnatý a/alebo fosforečnan aanganatý v pomere podlá zaatúpenia v základna) fosfátovacej zatli, vyznačujůei sa tým, že na kal zriedaný vodou v haotnostnom pomere 1 ku 0,5 až 0,6 sa posobi technickou kyselinou sirovou o množstvo v rozsshu 101 >ž 102 X hmotnostných voči jej teoretickému množstvu zodpovedajůcemu obsahu fosforu v kale a to za neustálého mieiania reakčnej změti a jej zohrievania po dobu odparenia 70 až 75 X Jej objemu, 3alej sa raakčná zmes schladzuje po dobu vytvořeni· kryJtálov sirénu železitého a odsává sa filtrát kyseliny fosforečnej.The method of regeneration of phosphate sludge has been hired as a technological waste in the chaotic surface treatment of metallic materials by phosphating · containing predominantly ferric phosphate and possibly zinc phosphate and / or agananate phosphate in proportion to the base load) of the phosphating sludge, characterized by quartz water The ratio of 1 to 0.5 to 0.6 is treated with technical sulfuric acid in an amount ranging from 101 to 102% by weight relative to its theoretical amount corresponding to the phosphorus content of the sludge, stirring the reaction mixture continuously and heating for 70 to 75%. In addition to its volume, the reaction mixture is cooled while the ferric siren crystals are formed and the phosphoric acid filtrate is filtered off with suction.
CS8829A 1988-01-03 1988-01-03 The method of regenerating the phosphate cat CS268589B1 (en)

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