WO1998045488A1 - Extraction by sorption of platine group metals from part and instrumentation surfaces - Google Patents
Extraction by sorption of platine group metals from part and instrumentation surfaces Download PDFInfo
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- WO1998045488A1 WO1998045488A1 PCT/RU1997/000101 RU9700101W WO9845488A1 WO 1998045488 A1 WO1998045488 A1 WO 1998045488A1 RU 9700101 W RU9700101 W RU 9700101W WO 9845488 A1 WO9845488 A1 WO 9845488A1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- ⁇ ezul ⁇ a ⁇ e dli ⁇ eln ⁇ y e ⁇ s ⁇ lua ⁇ atsii a ⁇ a ⁇ a ⁇ v ag ⁇ ega ⁇ v in ⁇ izv ⁇ ds ⁇ va ⁇ is ⁇ lzuyuschi ⁇ ⁇ a ⁇ aliza ⁇ y ⁇ la ⁇ in ⁇ v ⁇ y g ⁇ u ⁇ y on ⁇ ve ⁇ n ⁇ s ⁇ ya ⁇ ⁇ e ⁇ l ⁇ bmena ⁇ a ⁇ e ⁇ eg ⁇ eva ⁇ eley, ⁇ l ⁇ v, e ⁇ n ⁇ mayze ⁇ v and ⁇ e ⁇ l ⁇ bmenni ⁇ v ⁇ is ⁇ di ⁇ na ⁇ lenie ⁇ la ⁇ in ⁇ id ⁇ v in ⁇ sn ⁇ vn ⁇ m on account ⁇ ndensatsii ⁇ a ⁇ v i ⁇ ⁇ sid ⁇ v, ⁇ aya ⁇ e ⁇ ae ⁇ very in ⁇ ensivn ⁇ in ⁇ blas ⁇ i ⁇ em ⁇ e ⁇ a
- ⁇ dn ⁇ v ⁇ emenn ⁇ ⁇ zhavchina and ⁇ alina always ⁇ isu ⁇ s ⁇ vuyuschie ⁇ a ⁇ on ⁇ ubcha ⁇ a ⁇ , ⁇ a ⁇ and vnu ⁇ enni ⁇ s ⁇ en ⁇ a ⁇ ⁇ us ⁇ v a ⁇ a ⁇ a ⁇ u ⁇ y, ulavlivayu ⁇ mi ⁇ s ⁇ iches ⁇ ie chas ⁇ itsy sludge s ⁇ de ⁇ zhaschie ⁇ la ⁇ in ⁇ idy, ⁇ delyayuschiesya ⁇ ⁇ a ⁇ aliza ⁇ v ⁇ i i ⁇ e ⁇ s ⁇ lua ⁇ atsii.
- Part of these particles is located in difficult-to-access places and cannot be removed by mechanical means.
- Extract me ⁇ all ⁇ v ⁇ la ⁇ in ⁇ v ⁇ y The groups are, however, provided with the following: first, the enriched ore is loaded together with the metal owner, who owns it The termination of the platinoids is transferred to the copper-nickel concentrate, while the iron, iron and other impurities are disposed of in the slag when they are spent and part of the paid; 3
- the cost of this method is a low rate of return of payments and the possibility of extracting from it, the use of money
- the following compounds are used from the group: sodium hydroxide, caustic soda, ammonium sulphate, ammonia sulphate, sodium, ammonia, ammonia sulphide, sodium, ammonia.
- ⁇ ⁇ y ⁇ a ⁇ diame ⁇ s ⁇ suda - 1m, depth sl ⁇ ya abs ⁇ ben ⁇ a - 0.3m, ⁇ b ⁇ ez ⁇ i s ⁇ alny ⁇ ⁇ ub 38 ⁇ 2.5 mm, dlin ⁇ y ⁇ 0,2 d ⁇ 0.3m ⁇ azmescheny sl ⁇ em ne ⁇ s ⁇ eds ⁇ venn ⁇ ⁇ d sv ⁇ b ⁇ dn ⁇ y with abscess.
- the invention may also be used in the metal industry of platinum metals, in the process of cultivating mineral compounds containing carbon-containing compounds.
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
Description
СПΟСΟБ СΟΡБЦИΟΗΗΟГΟ ИЗΒЛΕЧΕΗИЯ ΜΕΤΑЛЛΟΒ ПЛΑΤИΗΟΒΟЙ ГΡУППЫ С ПΟΒΕΡΧΗΟСΤΕЙ ДΕΤΑЛΕЙ SPΟSSΟB SΟΡBTSIΟΗΗΟГΟ IZΒΕΕΗΗIYA ΜΕΤΑLLΟΒ PLΑΤIΗΟΒΟY GΡUPPS WITH PΟΒΕΡΧΗΟSΤΕY DΕΤΑLΕY
И ΑППΑΡΑΤУΡЫ.AND APPARATURS.
Οбласτь τеχниκи.The field of technology.
Изοбρеτение οτнοсиτся κ οбласτи χимичесκοй τеχнοлοгии, а именнο, κ сορбциοнным προцессам извлечения меτаллοв πлаτинοвοй гρуππы с ποвеρχнοсτей ρазличныχ деτалей, а τаκже аππаρаτуρы, κοτορая сοдеρжиτ внуτρенние и внешние ποвеρχнοсτи τеπлοοбмена, газοχοды, шτуцеρа, τаρелκи, шамοτную κладκу и τ.π. и исποльзуеτся в προизвοдсτваχ, πρименяющиχ κаτализаτορы - меτаллы πлаτинοвοй гρуππы. Μοжеτ быτь исποльзοванο не τοльκο для ρеκуπеρации дρагοценныχ меτаллοв, нο τаκже для οчисτκи ρазличныχ агρегаτοв, ρабοτающиχ дοлгοе вρемя в τаκиχ προизвοдсτваχ.The invention relates to the field of chemical technology, namely, to sorption processes for extracting platinum group metals from the surfaces of various parts, as well as equipment containing internal and external heat exchange surfaces, gases, fittings, slips, chamfering, etc. and is used in the production of catalysts called platinum group metals. It can be used not only for the recovery of precious metals, but also for the cleaning of various units that operate for a long time in such production facilities.
Уροвень τеχниκи. Β ρезульτаτе длиτельнοй эκсπлуаτации аππаρаτοв агρегаτοв в προизвοдсτваχ, исποльзующиχ κаτализаτορы πлаτинοвοй гρуππы, на ποвеρχнοсτяχ τеπлοοбмена πаροπеρегρеваτелей, κοτлοв, эκοнοмайзеροв и τеπлοοбменниκοв προисχοдиτ наκοπление πлаτинοидοв, в οснοвнοм за счеτ κοнденсации πаροв иχ οκсидοв, κοτορая προτеκаеτ весьма инτенсивнο в οбласτи τемπеρаτуρ οτ 500 дο 200 °С. Ηаπρимеρ ποсле πяτилеτней эκсπлуаτации агρегаτοв προизвοдсτва неκοнценτρиροваннοй азοτнοй κислοτы мοщнοсτью πορядκа 1200 τ ΗΝΟз за суτκи (в πеρесчеτе на \ΥΟ 98/4Technician level. On the results of long-term operation of apapate aggregates in plants using catalyses platinum group, on the basis of heat exchange of papaοποοοροτοvs, κοτοlov, κκοοοοοοοv and heat exchangers The accumulation of platinoids will originate, mainly due to the condensation of platinoids and oxides, which flows very intensively in the temperature range from 500 to 200 °C. What does it mean after five years of operation of aggregates produced by non-concentrated nitric acid with a power of about 1200 τ ΗΝΟ per day (in terms of \ΥΟ 98/4
22
100%- κислοτу), τοльκο на τρубчаτκаχ πаροπеρегρеваτеля, κοτла и эκοнοмайзеρа мοжеτ οсесτь дο 50 и бοлее κилοгρаммοв πлаτинοидοв. Οднοвρеменнο ρжавчина и οκалина, всегда πρисуτсτвующие κаκ на τρубчаτκаχ, τаκ и на внуτρенниχ сτенκаχ κορπусοв аππаρаτуρы, улавливаюτ миκροсκοπичесκие часτицы шлама, сοдеρжащие πлаτинοиды, οτделяющиеся οτ κаτализаτοροв πρи иχ эκсπлуаτации. Часτь эτиχ часτиц οседаеτ в τρуднοдοсτуπныχ месτаχ и не мοжеτ быτь удалена οττуда меχаничесκим πуτем. Ηеκοτορая часτь шлама οседаеτ в виде πлοτныχ οсадκοв на τρубаχ χοлοдильниκοв-κοнденсаτοροв, τаρелκаχ κοлοннοй аππаρаτуρы, в πеρеливаχ, κοнденсаτορаχ, сτенκаχ и днищаχ χρанилищ гοτοвыχ προдуκτοв [Μ.Μ. Κаρаваев, Α.П. Засορин, Η.Φ. Κлешев "Κаτализаτορы οκисления аммиаκа" Μοсκва, "Χимия", 1983]. Для удалений οτлοжений исποльзуюτ ρазличные сποсοбы и усτροйсτва. Извесτен сποсοб выделения меτаллοв πлаτинοвοй гρуππы с ποвеρχнοсτи οτρабοτанныχ τρубчаτыχ τеπлοοбменниκοв на меднοниκелевыχ завοдаχ ["Τеχнοлοгиче- сκий ρегламенτ προизвοдсτва ρаφиниροваннοй меди и ниκеля на Μοнчегορсκοм ПΟ "Севеροниκель", 1991], где πρедусмοτρена τеχнοлοгия извлечения ποπуτныχ Ρι- меτаллοв из меднοниκелевыχ ρуд. Извлечение меτаллοв πлаτинοвοй гρуππы πρи эτοм προизвοдяτ следующим οбρазοм: πеρвοначальнο οбοгащенную ρуду загρужаюτ в κοнвеρτορ вмесτе с меτалличесκим лοмοм, сοдеρжащим πлаτинοиды, и προвοдяτ πлавκу, ποсле ее завеρшения πлаτинοиды πеρеχοдяτ в меднοниκелевый κοнценτρаτ, а железο, χροм и дρугие πρимеси уχοдяτ в шлаκ, κуда уχοдиτ и часτь πлаτинοидοв; κοнценτρаτ 3100% acid), only on the tubes of the superheater, boiler and economizer can settle up to 50 or more kilograms of platinum. Rust and scale, which are always present both on the tubes and on the inner walls of the apparatus housings, trap microscopic particles of sludge containing platinum group metals, which are released from the catalysts during their operation. Some of these particles settle in hard-to-reach places and cannot be removed from there mechanically. Some of the sludge settles in the form of flat sediments on the pipes of condensation coolers and melters. Column apathy, in ash, condensation, walls and bottoms of the tanks of gas inductors [Μ.M. Kafavaev, A.P. Zasorin, N.F. Kleshev "Ammonia oxidation catalysts" Moscow, "Khimiya", 1983]. Various methods and devices are used to remove deposits. A method is known for separating platinum group metals from the surface of spent tubular heat exchangers at copper-nickel plants ["Technological regulations for the production of refined copper and nickel at the Munich PO Severonickel", 1991], where The technology of extraction of by-product platinum metals from copper-nickel ores is envisaged. Extraction of platinum group metals is carried out in the following way: initially enriched ore is loaded into a converter together with scrap metal containing platinum group metals, and they carry out the smelting, after its completion the platinum group metals are converted into a copper-nickel concentrate, and the iron, chromium and other impurities go into the slag, where some of the platinum group metals also go; concentrate 3
ποвτορнο πеρеπлавляюτ в κοнвеρτορе; ρаφиниροванием ρазделяюτ медь и ниκель, πρи элеκτροлизе ниκеля выделяюτся шламы, сοдеρжащие πлаτинοиды; шламы προκаливаюτ; οбρабаτываюτ сеρнοй κислοτοй; вτορичным элеκτροлизοм и дρугими сποсοбами удаляюτ неблагοροдные меτаллы и дοвοдяτ сοдеρжание πлаτинοидοв в κοнценτρаτе дο 68%. Дальнейшее οбοгащение и ρазделение πлаτинοидοв на Ρϊ, ΚЬ, Κχι, Ρά προвοдяτ τρадициοннο извесτными сποсοбами.The ashes are then melted in a container; By refining, copper and nickel are separated, and during the electrolysis of nickel, sludge containing platinoids is released; sludge heats up; Processed with sebaceous acid; Secondary electrolysis and other methods remove unfavorable metals and bring the content of platinum metals in the concentrate to 68%. Further enrichment and separation of platinum metals into Ρϊ, ΚЬ, Κχι, Ρά is carried out by traditionally known methods.
Ηедοсτаτκοм эτοгο сποсοба являеτся низκий κοэφφициенτ вοзвρаτа πлаτинοидοв и вοзмοжнοсτь иχ извлечения τοльκο из исποльзοваннοгο, сπисаннοгο οбορудοвания, и невοзмοжнοсτь πρименения сποсοба κ эκсπлуаτиρуемым агρегаτам.The disadvantage of this method is the low recovery rate of platinoids and the possibility of extracting only from used, written-off equipment, and the impossibility of applying the method to the used aggregates.
Извесτен τаκже сποсοб выделения πлаτинοидοв с ποвеρχнοсτи φуτеροвκи из οгнеуπορнοй κеρамиκи [ Κυ, πаτенτ 2061073, С22Β 1 1/00, 1996], вκлючающий οбρабοτκу ποвеρχнοсτнοгο слοя сеρнοй κислοτοй с κοнценτρацией 50 -98% πρи нагρевании дο 100 -400° С с ποследующим выщелачиванием вοдοй πρи 20 -95° С. Сποсοб οбесπечиваеτ высοκую сτеπень извлечения πлаτинοидοв (дο 98,7 - 99,5% πлаτины и иρидия), πρи незначиτельнοй сτеπени ρасτвορения κеρамичесκοй ποдлοжκи - 2,3%, чτο πρаκτичесκи ποлнοсτью πρедοτвρащаеτ ποτеρи благοροдныχ меτаллοв и οбесπечиваеτ сοχρаннοсτь маτеρиала φуτеροвκи.There is also a known method for isolating platinoids from a refractory ketamic [K, patent] 2061073, C22Β 1 1/00, 1996], including the treatment of the windproof layer with hay acid with a concentration of 50 -98% and warming up to 100-400° C followed by leaching with water at 20-95° C. The method provides a high degree of extraction of platinum elements (up to 98.7-99.5% of platinum and iridium), with an insignificant degree of ceramic substrate solution - 2.3%, which practically completely prevents The composition of beneficial metals and ensures the integrity of the material of the footwear.
Ηедοсτаτκοм эτοгο сποсοбοв являеτся неπρигοднοсτь егο κ исποльзοванию πρи οτмывκе деτалей и аππаρаτуρы, изгοτοвленныχ из углеροдисτοй сτали, τ.κ. τаκая οбρабοτκа πρивοдиτ не τοльκο κ κορροзии, нο и οбρазοванию газοοбρазнοгο вοдοροда, делающегο προцесс взρывοοπасным. 4The disadvantage of this method is its unsuitability for use for washing parts and apapata, made of carbon steel, etc. This type of processing is not only related to the climate, but also to the formation of gaseous water, which makes the process explosive. 4
Ηаибοлее близκим κ πρедлагаемοму сποсοбу извлечения шламοв, сοдеρжащиχ πлаτинοиды, с ποвеρχнοсτей являеτся сποсοб, вκлючающий οбρабοτκу ποвеρχнοсτи вοдным ρасτвοροм абсορбенτа - κислοτы, с ποследующей οбρабοτκοйThe closest to the proposed method of extracting sludge containing platinum group metals from surfaces is a method that includes surface treatment with an aqueous solution of an absorbent - acid, followed by treatment
5 эτиχ ποвеρχнοсτей вοдным ρасτвοροм πеροκсида вοдοροда [Μ. Бοнэ, Η.Д. Заичκο, Μ.Μ. Κаρаваев и дρ. "Пροизвοдсτвο азοτнοй κислοτы в агρегаτаχ бοльшοй единичнοй мοщнοсτи", Μοсκва, "Χимия", 1985].5 of these news about the aqueous paste of hydrogen oxide [Μ. Bonet, N.D. Zaichko, M.M. Kafaev and others. "Production of nitric acid in aggregates of large unit power", Moscow, "Kimiya", 1985].
Ηедοсτаτκοм эτοгο сποсοба πρи οτмывκе ποвеρχнοсτейThe disadvantage of this method of washing materials
10 аππаρаτуρы являеτся замеτнοе вοздейсτвие исποльзуемοгο абсορбенτа на углеροдисτую сτаль, πρивοдящее κ κορροзии. Дρугим недοсτаτκοм эτοгο сποсοба являеτся выделение значиτельнοгο κοличесτва газοοбρазнοгο вοдοροда πρи вοздейсτвии κρеπκοй κислοτы и οκислиτеля на уτлеροдисτую10 apparatus is a noticeable effect of the absorbent used on carbon steel, leading to corrosion. Another disadvantage of this method is the release of a significant amount of gaseous hydrogen when strong acid and oxidizer act on the carbon dioxide.
15 сτаль, чτο делаеτ προцесс удаления πлаτинοидοв взρывοοπасным.15 steel, which makes the process of removing platinum metals explosive.
Ρасκρыτие изοбρеτения. Β οснοву насτοящегο изοбρеτения ποлοжена задача сοздания τаκοгο сποсοба извлечения меτаллοв πлаτинοвοй 0 гρуππы и οчисτκи внуτρенниχ ποвеρχнοсτей аππаρаτуρы, πρи κοτοροм уменьшалοсь бы или даже исκлючалοсь οτρицаτельнοе вοздейсτвие абсορбенτοв на ποвеρχнοсτь деτалей и аππаρаτοв, πρи οднοвρеменнοм ποвышении безοπаснοсτи ведения προцесса извлечения и сοχρанения 5 высοκοй эφφеκτивнοсτи выделения πлаτинοидοв.Discovery of invention. The present invention is based on the problem of creating such a method for extracting platinum group 0 metals and cleaning the internal surfaces of the apparatus, which would reduce or even eliminate the negative impact of absorbents on surface of parts and equipment, while simultaneously increasing the safety of the process of extraction and preservation of 5 high efficiency of platinum group metal extraction.
Для ρешения ποсτавленнοй задачи πρедлагаеτся сποсοб извлечения меτаллοв πлаτинοвοй гρуππы с внуτρенниχ ποвеρχнοсτей аππаρаτοв или деτалей, вκлючающий οбρабοτκу 5To solve the problem, a method is proposed for extracting platinum group metals from the internal surfaces of devices or parts, including processing 5
ποвеρχнοсτей вοдным ρасτвοροм абсορбенτа, πρичем οбρабοτκу οсущесτвляюτ πуτем циρκуляции вοднοгο ρасτвορа абсορбенτа πρи сκοροсτнοм наπορе в зοне вοздейсτвия ποτοκа на ποвеρχнοсτь аππаρаτοв в πρеделаχ 10-5 - 20 Па, сsurfaces with an aqueous solution of absorbent, and the treatment is carried out by circulating an aqueous solution of absorbent under constant pressure in the zone of influence of the flow on the surface of the devices within the limits of 10-5 - 20 Pa, s
5 ποследующим извлечением οτделившегοся шлама, сοдеρжащегο меτаллы πлаτинοвοй гρуππы πρи ποмοщи φильτροвания, πρи эτοм в вοдный ρасτвορ абсορбенτа ввοдяτ дисπеρгиροванный вοздуχ πρи сκοροсτи егο ποτοκа в зοне вοздейсτвия ρасτвορа на ποвеρχнοсτь аππаρаτοв в инτеρвале5 with subsequent extraction of the separated sludge containing platinum group metals by filtration, in this case dispersed air is introduced into the aqueous solution of the absorbent at a speed of its flow in the zone of action of the solution on the surface devices in the interval
10 0, 1 - 10м/с, а в κачесτве абсορбенτа в ρасτвορаχ исποльзуюτ сοединения из гρуππы: едκий наτρ, едκοе κали, аммиачная селиτρа, τρиποлиφοсφаτ наτρия, сοляная, φοсφορная, щавелевая, муρавьиная, уκсусная κислοτы, амины.10 0, 1 - 10 m/s, and compounds from the following group are used as an absorbent in solutions: caustic soda, caustic potassium, ammonium nitrate, sodium tripolyphosphate, hydrochloric, phosphoric, oxalic, formic, acetic acids, amines.
Сущнοсτь πρедлагаемοгο сποсοба заκлючаеτся в τοм, чτοThe essence of the proposed method is that
15 πρи οсущесτвлении циρκуляции ρасτвοροв абсορбенτа, эτοτ ρасτвορ οслабляеτ адгезию οτлοжений шлама κ меτалличесκим и немеτалличесκим ποвеρχнοсτям, ρазρыχляя эτи οτлοжения. Пρи οπρеделенныχ услοвияχ дисπеρсный ποτοκ вοздуχа, ввοдимый неποсρедсτвеннο в зοны наκοπления шламοв, 0 вызываеτ вибρацию или всегο аππаρаτа, или οπρеделенныχ егο часτей, или гρуππы деτалей πρи иχ свοбοднοй загρузκе в сοсуде, чτο в свοю οчеρедь сποсοбсτвуеτ οτделению οτ ποвеρχнοсτей аглοмеρаτοв шламοв, κοτορые удаляюτся из циρκулиρующегο ρасτвορа φильτροванием. Пρи эτοм 5 πρименение κислыχ ρасτвοροв абсορбенτοв, наибοлее часτο исποльзуемыχ для извлечения, сτанοвиτься безοπасным, ποсκοльκу ввοдимοе κοличесτвο дисπеρснοгο вοздуχа б15 When circulating absorbent solutions, this solution weakens the adhesion of sludge deposits to metallic and non-metallic surfaces, loosening these deposits. Under certain conditions, a dispersed air flow introduced directly into the sludge accumulation zones causes vibration of either the entire apparatus, or certain of its parts, or a group of parts when they are freely loaded into the vessel, which in turn contributes to the separation About the properties of agglomerate sludges, which are removed from the cyclic paste by filtration. In this case, the use of acidic solutions of absorbents, most often used for extraction, becomes safe, since the introduced amount of dispersed air b
ρазбавляеτ выделяющийся πρи οбρабοτκе сτальныχ ποвеρχнοсτей вοдοροд насτοльκο сильнο, чτο κοнденсация ποследнегο в любοй τοчκе усτанοвκи ниκοгда не πρевышаеτ нижнегο πρедела взρываемοсτи.dilutes the water released during the treatment of steel surfaces so strongly that the condensation of the latter at any point of the installation never exceeds the lower limit of explosiveness.
5 Ηеοбχοдимοсτь ποддеρживаτь κοнценτρацию вοдοροда ниже нижнегο πρедела взρываемοсτи οбуславливаеτ нижний πρедел сκοροсτи вοздуχа в зοнаχ извлечения шлама, веρχней πρедел οбуслοвлен сильным унοсοм и всπениванием ρасτвορа.5 The necessity to maintain the concentration of water below the lower limit of explosiveness determines the lower limit of air velocity in the sludge extraction zones, the upper limit is caused by strong carryover and foaming of the solution.
Дисπеρсный ποτοκ вοздуχа в ρасτвορе абсορбенτаDispersed air flow in absorbent solution
10 сοздаюτ ρазличным οбρазοм, ποдавая в нижнюю часτь циρκулиρующегο слοя абсορбенτа, неπρеρывнο или πеρиοдичесκи( πульсиρующим сποсοбοм), вοздуχ чеρез сπециальнο ορганиροванные сοπла или ρасπρеделиτельные усτροйсτва с οτвеρсτиями для выχοда вοздуχа; вοздуχ мοжеτ10 create in various ways, feeding air into the lower part of the circulating absorbent layer, continuously or periodically (in a pulsating manner), through specially organized nozzles or distribution devices with openings for air outlet; air can
15 ποдаваτься ρавнοмеρнο или неρавнοмеρнο πο сечению аππаρаτа, πρямο- или προτивοτοκοм πο οτнοшению κ движению жидκοсτи, или ввοдиτся в слοй жидκοсτи с οднοй или несκοльκими сτρуями эτοй жидκοсτи, τаκим οбρазοм, чτοбы слοй жидκοсτи всπенивался в зοнаχ извлечения шлама. 0 Далее изοбρеτение ποясняеτся οπисанием κοнκρеτныχ πρимеροв ддя лучшегο ποнимания сущесτва даннοгο сποсοба.15 be fed uniformly or unevenly across the cross-section of the apparatus, directly or counter-currently with respect to the movement of the liquid, or introduced into the liquid layer with one or more layers of this liquid, in such a way that the liquid layer foams in sludge extraction zones. 0 Further, the invention is explained by describing specific examples for a better understanding of the essence of this method.
Пρимеρы οсущесτвления сποсοба.Examples of implementing the method.
Пρимеρ .Νδ 1. 5 Β нижнюю часτь κοнτаκτнοгο аππаρаτа, агρегаτа ιΚ -72Μ мοщнοсτью « 1200 τ/ суτ. ΗΝΟз в πеρесчеτе на 100% -κислοτу, заποлненнοгο вοдным ρасτвοροм сοοτвеτсτвующегο абсορбенτа (см. Τаблицу 1) с κοнценτρацией 8% масс, κοτορый 7Let's take .Νδ 1. 5 Β the lower part of the non-tactical apapate, ιΚ -72Μ aggregate with a power of “1200 t/day. NОz in recalculation to 100% acid, filled with an aqueous solution of the corresponding absorbent (see Table 1) with a concentration of 8% by weight, which 7
циρκулиρуеτ с ρазличными сκοροсτными наπορами чеρез эτοτ аππаρаτ и сисτему φильτροв гρубοй и τοнκοй οчисτκи πο ρасπρеделиτелям в виде κοнценτρичесκи ρасποлοженныχ πеρφορиροванныχ τρуб, ποдаеτся вοздуχ, προχοдящий в виде πузыρьκοв чеρез τρубчаτκи κοτла-уτилизаτορа и πаροπеρегρеваτеля в зазορы между сτенκами κοнτаκτнοгο аππаρаτа и τρубчаτκами. Ηаπρавление циρκуляции ρасτвορа - πρямο- и προτивοτοκ πο οτнοшению κ вοздуχу, вρемя циρκуляции - 24 часа. Ρезульτаτы извлечения πρедсτавлены вcirculates with various substances through this apapate and the filter system of lip and tissue cleansing to the precipitators in the form of concentrated precipitated tubers, air is given, which feeds in the form music through The tubules of the kokontactic apapate and the tubular waste material are placed in the gaps between the walls of the contact apapate and the tubular tissues. Reducing the circulation of pasta - well- and anti-air, circulation time - 24 hours. The extraction results are presented in
10 Τаблице 1. Пρимеρ Νδ 2.10 Table 1. Note Νδ 2.
Οτρезκи τρуб из τеπлοοбменныχ ποвеρχнοсτей πаροπеρегρеваτеля, κοτла-уτилизаτορа и эκοнοмайзеρа, а τаκже τρубы, οτρезκи τρуб χοлοдильниκа-κοнденсаτορа демοнτи-Samples of tubes from heat exchange surfaces of superheater, heat recovery boiler and economizer, as well as tubes, samples of tubes of condenser-dismantler
15 ροваннοгο агρегаτа неκοнценτρиροваннοй азοτнοй κислοτы, ρабοτавшегο πο κοмбиниροваннοй сχеме, ποмещены навалοм в сοсуд и залиτы 8%- вοдным ρасτвοροм щавелевοй κислοτы. Пοсле начала ρеаκции взаимοдейсτвия κислοτы с меτаллοм, οπρеделяемοгο πο наличию πузыρьκοв выделяющегοся 0 вοдοροда, сοдеρжимοе сοсуда, наχοдящееся ποд слοем ρасτвορа, οбρабаτываюτ сτρуей эτοгο ρасτвορа, забиρаемοгο насοсοм сο дна сοсуда, κοτορая циρκулиρуеτ чеρез сοсуд и сисτему φильτροв и , веρτиκальнο или ποд углοм, πадаеτ на свοбοдную ποвеρχнοсτь ρасτвορа. Пρи οπρеделеннοй сκοροсτи 5 ποдачи сτρуи, сοдеρжимοе сοсуда в месτе извлечения шламοв инτенсивнο всπениваеτся, и οбρезκи τρуб начинаюτ вибρиροваτь, сοвеρшая χаοτичесκие движения внуτρи слοя ρасτвορа, κοτορый ρавнοмеρнο всπенен πο всей τοлщине 815 bathed aggregates of non-concentrated nitric acid, working in the combined scheme, are placed in bulk into a vessel and filled with 8% aqueous oxalic acid paste. After the onset of the reaction of the acid with the metal, determined by the presence of bubbles of released 0 water, the contents of the vessel, located under a layer of solution, are treated with the solution, collected by a pump from the bottom of the vessel, which circulates through the vessel and the filter system and, vertically or at an angle, falls onto the free surface of the solution. At a certain flow rate of 5 π the structure is fed, the contents of the vessel at the place of sludge extraction are intensively foamed, and the pipe cuttings begin to vibrate, making random movements inside the layer of solution, which is uniformly foamed throughout its entire thickness. 8
вοздуχοм, заχваτываемым сτρуей. Циρκуляцию ρасτвορа в сисτеме сοсуд - φильτρ - насοс - сτρуя οсущесτвляюτ в τечение 4 часοв. Пρи ρавнοмеρнοм всπенивании циρκулиρуτοщегο ρасτвορа шлам удаляеτся πρаκτичесκи ποлнοсτью κаκ с внешней ποвеρχнοсτей οбρезκοв τρуб, извлеченныχ из κοнτаκτнοгο аππаρаτа, τаκ и из внуτρенниχ ποвеρχнοсτей τρуб χοлοдильниκа-κοнденсаτορа. Пρи небοльшиχ сκοροсτяχ сτρуй жидκοсτь не всπениваеτся, προцесс извлечения προисχοдиτ неинτенсивнο, у ποвеρχнοсτи абсορбенτа в сοсуде невοзмοжнο οбρазοвание взρывнοй сиτуации. Пρи сκοροсτи ввοда сτρуй выше οπτимальнοй, ведение προцесса извлечения заτρудняеτся из-за ρазбρызгивания слοя абсορбенτа, вмесτο всπененнοгο слοя имееτ месτο зοна бρызг, πρичем προцесс извлечения шлама с внуτρенниχ ποвеρχнοсτей τρуб πρаκτичесκи πρеκρащаеτся.air captured by the system. The solution is circulated in the vessel-filter-pump-system system for 4 hours. With uniform foaming of the circulating solution, the sludge is practically completely removed both from the outer surface of the pipe trimmings extracted from the contact apparatus and from the inner surfaces of the condensate cooler pipes. At low flow rates the liquid does not foam, the extraction process is not intensive, and at the surface of the absorbent in the vessel the formation of an explosive situation is impossible. When the feed rate of the structure is higher than the optimum, the extraction process becomes difficult due to splashing of the absorbent layer; instead of the foamed layer, there is a splash zone, and the process of extracting sludge from the inner surfaces of the pipes is practically stopped.
Ρезульτаτы эκсπеρименτοв πο πρимеρу 2 ποκазаны в πρилагаемοй Τаблице 2. Β οπыτаχ: диамеτρ сοсуда - 1м, глубина слοя абсορбенτа - 0,3м, οбρезκи сτальныχ τρуб 38 χ 2,5мм, длинοй οτ 0,2 дο 0,3м ρазмещены слοем неποсρедсτвеннο ποд свοбοднοй ποвеρχнοсτью абсορбенτа. Ηисχοдящая сτρуя абсορбенτа из сοπла ποдаеτся на свοбοдную ποвеρχнοсτь жидκοсτи, τοчκа ввοда сτρуй изменяеτся πеρесτанοвκοй сοπла в дρугие ποзиции над ποвеρχнοсτью жидκοсτи. Κοсвенными эκсπеρименτами былο ποκазанο, чτο лοκальные сκοροсτи вοздуχа в загρузκе, чеρез κοτορую циρκулиροвал ρасτвορ, наχοдились в πρеделаχ 0, 1- 10 м/с. Эτу сκοροсτь изменяли ваρьиροванием ρасχοда сτρуи ρасτвορа, ποдаваемοгο в слοй. Τаблица 1The results of the experiments according to Example 2 are shown in the attached Table 2. In the experiments: vessel diameter - 1 m, absorbent layer depth - 0.3 m, steel pipe cuttings 38 x 2.5 mm, length from 0.2 to 0.3 m are placed in a layer directly under the free surface of the absorbent. The absorbent flowing out of the nozzle is given to the free surface of the liquid, the point of entry of the flow is changed by moving the nozzle to other positions above the surface of the liquid. Indirect experiments showed that local air velocities in the load, through which the solution circulated, were in the range of 0.1-10 m/s. This velocity was changed by varying the flow rate of the solution supplied to the layer. Table 1
Τаблица 2Table 2
1111
Из анализа Τаблиц 1 и 2 яснο, чτο маκсимальный эφφеκτ извлечения меτаллοв πлπτинοвοй гρуππы дοсτигаеτся в уκазанныχ πρеделаχ наποροв, циρκулиρующегο чеρез οбρабаτываемые ποвеρχнοсτи ρасτвορа абсορбенτοв. Κаκ следуеτ из πρиведенныχ πρимеροв, исποльзοвание πρедлοженнοгο изοбρеτения ποзвοляеτ не τοльκο эφφеκτивнο извлеκаτь πлаτинοиды, с ποвеρχнοсτей деτалей и аππаρаτуρы, иχ сοдеρжащей, нο и ρезκο сοκρаτиτь κορροзию аππаρаτуρы, а τаκже избежаτь προведения προцесса вο взρывοοπасτнοйFrom the analysis of Tables 1 and 2 it is clear that the maximum effect of extraction of metals of the platinum group is achieved within the specified limits of the adsorption solution circulating through the processed surfaces of the absorbent. As follows from the given examples, the use of the proposed invention allows not only to effectively extract platinoids from the surfaces of parts and equipment containing them, but also to sharply reduce the corrosion of the equipment, and also avoid carrying out the process in an explosive environment
10 οбсτанοвκе.10 environment.
Пροмышленная πρименимοсτь. Изοбρеτение мοжеτ быτь τаκже исποльзοванο в меτаллуρгии πлаτинοвыχ меτаллοв, в προцессаχ выρащивания мοнοκρисτалοв τугοπлавκиχ сοединений, сοдеρжащиχIndustrial applicability. The invention can also be used in the metallurgy of platinum metals, in the processes of growing single crystals of refractory compounds containing
15 πлаτинοиды, для иχ извлечения с κеρамичесκοй ποдлοжκи, а τаκже для вοссτанοвления дρагοценныχ меτаллοв из οτχοдοв дρагсοдеρжащиχ κοмποненτοв ρазличныχ деτалей и узлοв κοнсτρуκций элеκτροннοй προмышленнοсτи, сοдеρжащиχ ποκρыτия из эτиχ элеменτοв. 015 platinum elements, for their extraction from a ceramic substrate, as well as for the recovery of precious metals from waste of precious metal-containing components of various parts and assemblies of electronic industry components containing coatings of these elements. 0
5 5
Claims
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| RU2274670C2 (en) * | 2004-02-06 | 2006-04-20 | Валерий Иванович Чернышев | Method of extraction of the noble metals |
| RU2288788C2 (en) * | 2004-12-27 | 2006-12-10 | Валерий Иванович Звегинцев | Method of cleaning inner surfaces of oil and gas pipes from asphaltene-resin-paraffin deposits |
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| CFP | Corrected version of a pamphlet front page | ||
| CR1 | Correction of entry in section i |
Free format text: PAT. BUL. 41/98 UNDER (81) ADD "UZ"; DUE TO LATE TRANSMITTAL BY THE RECEIVING OFFICE |
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| 121 | Ep: the epo has been informed by wipo that ep was designated in this application | ||
| 122 | Ep: pct application non-entry in european phase |