LT4384B - Process for the preparation of aluminium hydroxychloride - Google Patents

Process for the preparation of aluminium hydroxychloride Download PDF

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Publication number
LT4384B
LT4384B LT96-172A LT96172A LT4384B LT 4384 B LT4384 B LT 4384B LT 96172 A LT96172 A LT 96172A LT 4384 B LT4384 B LT 4384B
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LT
Lithuania
Prior art keywords
aluminum
aluminium
reactor
oxychloride
reaction
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LT96-172A
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Lithuanian (lt)
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LT96172A (en
Inventor
Arūnas Laurinaitis
Aleksandras Senuta
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Akcinė bendrovė "ACHEMA"
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Priority to LT96-172A priority Critical patent/LT4384B/en
Publication of LT96172A publication Critical patent/LT96172A/en
Publication of LT4384B publication Critical patent/LT4384B/en

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Abstract

Invention belongs to aluminium oxychloride manufacturing technology that may be used for wastewater treatment. The aluminium oxychloride is being produced by mixing aluminium hydroxide with salt acid at 1/4-4.5 ratio and sulphur acid is being used as reaction initiator, amount of which is 1.5-2 per cent of the non-reacting substance total mass. Before introducing initiator into reaction it is being dissolved in salt acid and substance containing aluminium is being introduced into reactor at a solvent temperature not less than as 40 degrees by Celsius. Letting steam of 100-110 degrees by Celsius temperature through water over barboter and maintaining pressure in the reactor at 1-1.03 ata. Mixing is provided by oxygen containing gases, air, for instance. Using this production method of aluminium oxychloride does not release hydrogen and there is no blast danger.

Description

Yra žinomi būdai kur aliuminio hidroksido pradinę suspensiją maišo su sieros rūgštimi ir procesą atlieka 130 - 200“1 C temperatūroje [SU 450780 G 01F 7/00], Šio proceso trukumas - aukšta temperatūra bei reikalingas aukštas slėgis.There are known methods wherein the starting aluminum hydroxide suspension was stirred with sulfuric acid, and performs the process from 130 to 200 "C for 1 [SB 450780 G 01F 7/00] disadvantage of this process - and the necessary high temperature under high pressure.

Yra žinomi būdai, kur aliuminio oksichioridui gauti naudoja druskos rūgštį ir geležies osidą bei trivalentį titaną [JP 93 - 314791 C 01F 7/00], o išradime [WO 9511197 C 01F 7/00] polialiuminio chloridą. Šie būdai taip pat reikalauja aukštu temperatūrų.There are known methods of using hydrochloric acid and ferric oside and trivalent titanium [JP 93 - 314791 C 01F 7/00] for the production of aluminum oxychioride, and in the invention [WO 9511197 C 01F 7/00] polyaluminium chloride. These techniques also require high temperatures.

Yra būdai, kur naudojamas grynas aliuminis ir pastarasis sąveikauja su aliuminio chlorido tirpalu druskos rūgštyje [JP 70 - 452645 C 01F 7/56], Šio būdo trūkumas, kad čia naudojama labai brangi žaliava aliuminis.There are methods where pure aluminum is used and the latter interacts with a solution of aluminum chloride in hydrochloric acid [JP 70 - 452645 C 01F 7/56]. The disadvantage of this method is that it uses a very expensive raw material, aluminum.

Bendras minėtų būdų trukūmas, kad proceso metu išsiskiria vandenilis, sudarantis didelę sprogimo grėsmę.The general disadvantage of the above techniques is that hydrogen is released during the process, which poses a major explosion hazard.

Patentuojamame išradime minėtų trukūmų išvengiama tuo, kad aliuminio hidroksidas maišomas su druskos rūgštimi ir reakcijos iniciatoriumi naudojama sieros rūgštis, kurios kiekis sudaro nuo 1,5 iki 2 % reaguojančių medžiagų masės kiekio, reagentų sąveika vyksta 1 -1,03 ata slėgyje ir 100-110 ° C temperatūroje, mišinys maišomas cirkuliaciniu būdu. Prieš įvedantį reakcijos zoną iniciatorių, jj ištirpina druskos rūgštyje, o aliuminio turinčią medžiagą įveda j reaktorių esant tirpalo temperatūrai ne mažesnei kaip 40 u G, reagentas vanduo įvedamas garų pavidalu, o reagentai maišomi dujomis, turinčiomis deguonies, pavyzdžiui oru.The disadvantages mentioned in the patented invention are avoided by mixing aluminum hydroxide with hydrochloric acid and sulfuric acid in an amount of 1.5 to 2% by weight of the reactants, reactant interaction at a pressure of 1 -1.03 and 100-110 At a temperature of 0 ° C, the mixture is circulated. Prior to the introduction of the reaction zone, the initiator is dissolved in hydrochloric acid and the aluminum-containing material is introduced into the reactor at a solution temperature of at least 40 u G, the reagent water is introduced in the form of steam and the reactants are mixed with gas containing oxygen such as air.

Būdas įgyvendinamas taip.The method is implemented as follows.

Aliuminio hidroksidas AI(OH)3 maišomas su druskos rūgštimi ir su'reakcijos iniciatoriaus mišiniu santykiu 1:4- 4,5, pavyzdžiui sieros rūgštimi, 1,5 - 2% nuo reaguojančių medžiagų masės. Sieros rūgštis pagreitina cheminės reakcijos pradžiąThe aluminum hydroxide Al (OH) 3 is mixed with hydrochloric acid and the reaction initiator mixture in a ratio of 1: 4 to 4.5, for example sulfuric acid, 1.5 to 2% by weight of the reactants. Sulfuric acid accelerates the onset of a chemical reaction

Al(OH)3 + 3HCI H2SO4 Al Ci3 + 3 H2 O (1)Al (OH) 3 + 3HCl H 2 SO 4 Al Ci 3 + 3 H 2 O (1)

AlC-b + H2O -» A1(OH)C12 + HC!AlC-b + H 2 O - »A1 (OH) C1 2 + HCl!

V“/V "/

Procesą atlieka taip. j reaktorių vamzdžiu paduoda sieros ir druskos rūgšties mišinį, santykiu 1 : 4 -f 4,5, o aliuminio nidroksidą įveda, kai mišinio temperatūra reaktoriuje būna ne mažesnė kaip 40 ° C. Toks gamybos būdo dalinimas padidina produkto išeigą. Temperatūrą reaktoriuje kelia paduodami per barboterį vandens garus nuo 100 iki 110° C temperatūros. Slėgį reaktoriuje palaiko nuo 1 iki 1,03 ata. Reagentų maišymą atiteka deguonį turinčiomis dujomis, pavyzdžiui oru. Reakcija baigiama pasiekus šiuos reakcijos mišinio rodiklius: pH ne mažiau 0,8 ir tankis 1,21 g/cm3. Po reakcijos galutinė produkto kokybė patikrinama laboratorijoje, t. y., nustatoma AI2Qs masės dalis ir pH bei tankis,The process is as follows. The reactor is fed with a 1: 4 -f 4.5 mixture of sulfuric and hydrochloric acid into the reactor, and aluminum hydroxide is introduced when the temperature of the mixture in the reactor is at least 40 ° C. The temperature in the reactor is raised by supplying water vapor from 100 to 110 ° C through a bubbler. The pressure in the reactor is maintained between 1 and 1.03 ata. Agitation of the reactants is effected with oxygen-containing gases such as air. The reaction is terminated when the pH of the reaction mixture is at least 0.8 and the density is 1.21 g / cm 3 . After the reaction, the final quality of the product is checked in the laboratory, that is, by weight and pH and density of AI 2 Qs,

Pavyzdys kg aliuminio hidroksido, 4 kg druskos rūgšties bei 0,075 kg sieros rūgšties maišomi barboteryje su 100 ° C temperatūros vandens garais. Reaktoriuje palaikomas slėgis 1 ata, Maišymo procesą atlieka oru. Reakcija baigiama esant reakcjos mišinio pH = 0,8, tankiui 1,.21 g/cm3, reakcijos trukmė 40 min, aliuminio oksichlorido išeiga 4,94 kg.Sample kg of aluminum hydroxide, 4 kg of hydrochloric acid and 0.075 kg of sulfuric acid are mixed in a bubbler with water vapor at 100 ° C. The reactor is maintained at a pressure of 1 ata, and the agitation is performed by air. The reaction mixture was completed at pH = 0.8, density 1, .21 g / cm 3 , reaction time 40 min, yield 4.94 kg of aluminum oxychloride.

Pavyzdys kg aliuminio hidroksido, 4,3 kg druskos rūgšties bei 0,09 kg sieros rūgšties maišomi barboteryje su 105 ° C temperatūros vandens garais. Reaktoriuje palaikomas slėgis 1,02 ata. Maišymo procesą atlieka oru. Reakcija baigta esant pH - 1,3, tankisSample kg of aluminum hydroxide, 4.3 kg of hydrochloric acid and 0.09 kg of sulfuric acid are mixed in a bubbler with water vapor at 105 ° C. The reactor is maintained at a pressure of 1.02 ata. The mixing process is performed by air. The reaction was completed at pH 1.3, density

1.23 g/cm3, reakcijos trukmė 30 min, aliuminio oksichlorido išeiga 5,23 kg.1.23 g / cm 3 , reaction time 30 min, yield 5.23 kg aluminum oxychloride.

Pavyzdys i kg aliuminio hidroksido, 4,5 kg druskos rūgšties bei 0,11 kg sieros rūgšties maišomi barboteryje su 110u C temperatūros vandens garais. Reaktoriuje palaikomas slėgis 1,03 ata. Maišymo procesą atlieka oru. Reakcija baigta esant pH = 1,5, tankis 1,25 g/cm3, reakcijos trukmė 28 min. aliuminio chlorido išeiga 5,43 kg, vExample I per kilogram of aluminum hydroxide, 4.5 kg of hydrochloric acid and 0.11 kg of sulfuric acid mixed with 110 u Barbot C water vapor. The reactor maintains a pressure of 1.03 ata. The mixing process is performed by air. The reaction was completed at pH = 1.5, density 1.25 g / cm 3 , reaction time 28 min. yield of aluminum chloride 5.43 kg, v

Šiuo budu gaminant aliuminio oksichloridą neišsiskiria vandenilis ir nesusidaro grėsmė sprogimui. Didėjant pH - didėja aliuminio chlorido, kaip reagento, efektyvumas t. y., esant mažesnėms koogulianto dozėms tolygiau nusiskaidrina vanduo bei padidėja transportavimo ir sandėliavimo saugumas.In this way, the production of aluminum oxychloride does not release hydrogen and there is no risk of explosion. As the pH increases, the efficiency of aluminum chloride as a reagent increases. that is, lower doses of coagulant provide a smoother clearing of water and increased transport and storage safety.

Aliuminio oksichiorido gamybos proceso pateiktų pavyzdžių rezultatai pateikti lentelėje lentelėThe results of the examples presented in the alumina production process are shown in the following table

Pa- vyz- dys Pa- virgin dys Medžiagos kiekis, kg Quantity of material, kg Garų tempe- ratūra, °C Steam tempe- ratification, ° C Slėgis, ata Pressure, ata Reak- cijos trukmė, min Reaction- cations duration, min pH pH tankis, g/cm3 density, g / cm 3 Išeiga, kg Yield, kg AI(OH)3 Al (OH) 3 HCl HCl H2SO4 H 2 SO 4 1 1 1 1 4 4 0,075 0.075 100 100 1 1 40 40 0,9 0.9 1,21 1.21 4,94 4.94 2 2 1 1 4,3 4.3 0,09 0.09 105 105 1,02 1.02 30 30th 1,3 1.3 1,23 1.23 5,23 5.23 3 3 1 1 4,5 4.5 0,11 0.11 110 110 1,03 1.03 28 28th 1,5 1.5 1,25 1.25 5,43 5.43

Claims (4)

Išradimo apibrėžtisDefinition of the Invention 1. Aliuminio oksichiorido gamybos būdas, naudojant metaiinj aliuminį, aliuminio junginius ar aliuminio hidroksidą, maišant junginius su druskos rūgštimi ir vandeniu, naudojant reakcijos iniciatorių bei filtravimą, b esiskiriantis tuo, kad reagentų sąveiką vykdo nuo 1 iki i ,03 ata slėgyje ir nuo 100 iki 110 °C temperatūroje, mišinį maišant cirkuliaciniu būdu.A process for the production of aluminum oxychloride using annual aluminum, aluminum compounds or aluminum hydroxide, by mixing the compounds with hydrochloric acid and water using a reaction initiator and filtration, characterized in that the reactants are interacted at a pressure of from 1 to i, 03 at 100 up to 110 ° C with stirring. 2. Aliuminio oksichiorido gamybos būdas pagal 1 punktą, b esiskiriantis tuo, kad procese iniciatoriaus funkciją atlieka sieros rūgštis, kurios kiekis sudaro nuo 1,5 iki 2% nuo reaguojančių medžiagų masės.Process for the production of aluminum oxychloride according to claim 1, characterized in that the process is carried out by sulfuric acid in an amount of from 1.5 to 2% by weight of the reactants. S.Aiiuminio oksichiorido gamybos būdas pagal 1 ir 2 punktus, b esi skiriant i s tuo, kad prieš įvedant j reakciją iniciatorių, jj ištirpina druskos rūgštyje, o aliuminį turinčią medžiagą įveda j reaktorių esant tirpaio temperatūrai ne mažesnei kaip 40 ° C.S. A process for the production of aluminum oxychloride according to claims 1 and 2, characterized in that it is dissolved in hydrochloric acid prior to the introduction of the initiator and the aluminum-containing material is introduced into the reactor at a temperature of at least 40 ° C. 4. Aliuminio oksichiorido gamybos būdas pagal 1 - 3 punktus, besiskiri an-t i s tuo, kad vandenį įveda garų pavidalu ir maišymą atlieka deguonį turinčiomis /*31 «r r»·* MUJ VHU-O.A process for the production of aluminum oxychioride according to claims 1 to 3, characterized in that the water is introduced in the form of a vapor and the mixing is carried out with oxygen-containing / * 31 «r r» · * MUJ VHU-O. 5. Aiiuminio oksichiorido gamybos būdas pagal 4 punktą, besiskiri antis tuo, kad reagentams maišyti nadoja orą.5. A process for the production of aluminum oxychioride according to claim 4, wherein the reactants are air-stirred.
LT96-172A 1996-12-12 1996-12-12 Process for the preparation of aluminium hydroxychloride LT4384B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU450780A1 (en) 1971-02-19 1974-11-25 Кали-Хеми Аг (Фирма) The method of obtaining basic aluminum chlorides
JPH052645A (en) 1991-06-26 1993-01-08 Kawasaki Steel Corp Ordered filtering method
JPH05314791A (en) 1992-05-12 1993-11-26 Fujitsu Ltd Performance test method for semiconductor device with redundant circuit and semiconductor device with redundant circuit
WO1995011197A1 (en) 1993-10-21 1995-04-27 Laporte Industries Limited Flocculants

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU450780A1 (en) 1971-02-19 1974-11-25 Кали-Хеми Аг (Фирма) The method of obtaining basic aluminum chlorides
JPH052645A (en) 1991-06-26 1993-01-08 Kawasaki Steel Corp Ordered filtering method
JPH05314791A (en) 1992-05-12 1993-11-26 Fujitsu Ltd Performance test method for semiconductor device with redundant circuit and semiconductor device with redundant circuit
WO1995011197A1 (en) 1993-10-21 1995-04-27 Laporte Industries Limited Flocculants

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