WO1980000852A1 - Methode de recuperation du plomb a partir d'un materiau brut de chlorure de plomb - Google Patents

Methode de recuperation du plomb a partir d'un materiau brut de chlorure de plomb Download PDF

Info

Publication number
WO1980000852A1
WO1980000852A1 PCT/SE1979/000199 SE7900199W WO8000852A1 WO 1980000852 A1 WO1980000852 A1 WO 1980000852A1 SE 7900199 W SE7900199 W SE 7900199W WO 8000852 A1 WO8000852 A1 WO 8000852A1
Authority
WO
WIPO (PCT)
Prior art keywords
lead
lead chloride
chloride
column reactor
temperature
Prior art date
Application number
PCT/SE1979/000199
Other languages
English (en)
Inventor
E Baeck
Original Assignee
Boliden Ab
E Baeck
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Boliden Ab, E Baeck filed Critical Boliden Ab
Publication of WO1980000852A1 publication Critical patent/WO1980000852A1/fr
Priority to DK248980A priority Critical patent/DK248980A/da

Links

Classifications

    • 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
    • C22B13/00—Obtaining lead
    • C22B13/02—Obtaining lead by dry processes

Definitions

  • the proposed processes include the leaching of lead sulphides in a chloride environment during simultaneous oxidation. Subsequent to the solution being purified from contaminants, it contains lead chloride in a dissolved form.
  • the lead chloride can be reduced to metal form directly, by electrolysis, although the lead thus obtained is porous and does not adhere satisfactory to the surface of the cathode, and hence there is obtained a lead-metal product which is difficult to remove from the electrolysis cell.
  • Another proposed method of reduction is one which is based on the concept of crystallizing lead chloride from the purified solution, whereafter said lead chloride is subjected to a smelt-electrolysis process, lead metal and chlorine gas being formed. Up to the present day, however, this method has not been shown to be sufficiently economical .
  • the process is based on the concept of bringing liquid lead chloride in a column reactor into contact, in counterflow, with a stream of reducing gas; and recirculating the non-reduced lead chloride, optionally subsequent to adjusting the temperature.
  • the lead reduced in the process is separated in a bottom container and removed.
  • the temperature of the lead chloride is maintained within a range of between 900 and 970°C, the lower temperature limit being determined by the fact that beneath this temperature, the equilibrium of the reaction for forming metallic lead from lead chloride at normal process pressures is displaced to the left, and hence the reaction yield of the lead chloride is very low and, as a result thereof, the major part of the reaction product must be recirculated.
  • temperatures exceeding about 900°C the reaction equilibrium is displaced to the right and considerably higher reaction yields can be achieved; the higher the temperature selected the greater the yield of the reaction.
  • Optimation of the temperature within the preferred range, and also in special circumstances outside said range, is determined by the specific conditions prevailing in the choosen plant. If an elevated pressure is applied, an elevated temperature can thus be choosen, therewith to influence the reaction yield positively, without any appreciable vaporization of lead chloride and losses to the residual gases. On the other hand, it may be advantageous in certain cases to use a low process pressure, thereby enabling low reaction temperatures to be used, primarily with respect to the construction of the apparatus used.
  • the reduction gases used may be reducing gases, such as hydrogen, gaseous carbon compounds, such as hydrocarbons, carbon monoxide and the like, and ammonia or mixtures thereof. Among those reduction gases which can conceivably be used, ammonia and hydrogen are preferred. The use of hydrogen, however, is particularly preferred.
  • the process particularly relates to a reduction process in a column reactor provided with packings or intermediate bottoms, in which reactor hydrogen or some other reducing gas is contacted with liquid lead chloride in counterflow.
  • the temperature in the bottom container is maintained at a level above the melting point of lead chloride, 501°C, and suitably beneath its boiling point, 954°C.
  • Lead melts at 327.5°C and boils at a temperature immediately above 1700°C.
  • the process is carried out continuously, by continuously conveying molten lead chloride up to the upper part of the column . reactor, suitable means being provided for heating the lead chloride melt to a temperature above 900°C during the continuous trans- port of said melt.
  • the heated chloride is then caused to pass downwardly through the reactor and is contacted with and reacts with hydrogen, or some other reducing gas, in counterflow, said gas being supplied continuously to the lower part of the reactor.
  • the metallic lead formed by the reaction is collected in the lower part of the reactor, from where the lead is tapped-off continuously, or at suitable intervals, while non-reduced lead chloride is re circulated in the process and returned to the upper part of the column reactor.
  • Raw material in the form of molten lead chloride is also supplied continuously during the process, or at uniform intervals of time.
  • the process can also be carried out in a line of column reactors coupled in series, in which molten lead chloride is transferred from the bottom container of the first column reactor to the upper part of a second column reactor, where said molten lead chloride is treated with reducing gas at elevated temperature.
  • the lead chloride can then be transferred, at further elevated temperature, to a third column reactor, and to further reactors, and from there returned to the upper stage of the first column reactor.
  • the reaction temperatures in the latter stages can be choosen so as to obtain a high reaction yield, without the corresponding risk of losses of lead chloride in vapour form.
  • This first stage in the line of series-coupled reactors is preferably effected at a temperature which provides an acceptable low loss of lead chloride to the process gas.
  • the following formulae are indicating the reac tions between lead chloride and hydrogen, used as the reducing gas, in the column reactor:
  • Lead chloride melts at a temperature of about 500°C, and has a boiling point at atmospheric pressure of about 954°C. Thermodynamic ally, the conditions of equilibrium for the reactions can be seen from Figure 1, where ⁇ G in kcal/mole are given for the reduction of solid, liquid and gaseous lead chloride with hydrogen.
  • Figure 1 illustrates the thermodynamic conditions for said process when reducing lead chloride with hydrogen
  • Figure 2 illustrates an apparatus for reducing lead chloride:- in accordance with the invention, said apparatus including a column reactor
  • Figure 3 illustrates an arrangement according to the invention comprising three column reactors in series.
  • FIG. 2 there is illustrated a column reactor 1 provided with a column part 2 having packings 3 arranged therein, and a bottom container 4 in which, in continuous operation, there is located a lower lead-layer 5 and an upper layer 6 of non-reduced, liquid lead chloride.
  • a liquid lead chloride distributing means 7 Arranged above the column is a liquid lead chloride distributing means 7. Lead chloride is supplied from the bottom container 4 to a pump 9, via a line 8, said lead chloride being conveyed from the pump 9 to the distributing means 7 via a line 10.
  • Arranged in the line 10 is a means 11 for heating the lead chloride with a heating coil 12 and a supply line 13 for raw material, viz. liquid lead chloride.
  • the bottom container may also be provided with a heating means 14, and a device for tapping-off reduced lead 15.
  • Reduction gas is supplied to the column reactor through a line 16, and departs from said reactor with reaction gases, through a line 17.
  • the reaction gases are cooled in a cooler 18 in a manner such as to condense the gaseous lead chloride entrained with said gases, whereafter the reaction gases, which comprise hydrogen chloride and nonreacted reduction gas, depart through a line 19.
  • the reaction gases are recirculated, suitably totally or partially and optionally after absorbing hydrogen chloride therefrom by washing said gases in aqueous solution and returned, to said column via a feed-back line (not shown) to said line 16.
  • the cooler is provided with cooling coils 20 and a line 21 through which condensed lead chloride is returned to the reactor.
  • Figure 3 illustrates an embodiment of the invention comprising three column reactors coupled in series, liquid lead chloride, having a temperature of between 900 - 970°C, being supplied to a first reactor 22 through a line 23.
  • Lead and lead chloride are separated into two separate layers in a bottom container 24 of the column reactor 22.
  • Lead chloride is passed through a line 25 to a second column reactor 26, subsequent to having passed a heating means 27.
  • Liquid lead and lead chloride are separated in a bottom container 28 of the second reactor 26.
  • Lead chloride is introduced to a third column reactor 30 through a line 29 which incorporates a heating means 31.
  • Lead and lead chloride are separated from one another in a bottom container 32 of the third column reactor 30, said lead chloride being returned to the upper part of the first column reactor 22 through a line 33 having a heating means 34 incorporated therein.
  • Lead is taken from the column reactors 22, 26 and 30 through lines 35, 36 and 37 respectively.
  • Reaction gas is supplied to the bottom container 32 of the third column reactor 30 through a line 38, and passes from the upper part of said reactor to the bottom container 28 of the second reactor 26 through a line 39, from where it is passed from the upper part of said second column reactor 26 to the bottom container 24 of said first column reactor 22 through a line 40.
  • Reaction gases are removed from the reactor through a line 41, incorporating a cooling means 42, and a line 43, said cooling gases being recirculated, suitably subsequent to washing said gases to absorb hydrogen chloride contained therein, to the bottom container 32 of the column reactor 30, through a line 38, to form part of the reduction gas.
  • Lead chloride condensed in the cooler means 42 is returned to the first column reactor 22 via a line 44.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

Un procede de recuperation du plomb a partir de materiaux bruts de chlorure de plomb obtenus particulierement par hydrometallurgie consiste a reduire lesdits materiaux bruts avec un gaz de reduction. Le procede est conduit de maniere appropriee avec de l'hydrogene ou de l'ammoniac dans un reacteur a colonnes (1) a contre-courant, le chlorure de plomb liquide etant en contact avec le gaz de reduction, a une temperature appropriee situee entre 900 et 970 C. Le reacteur a colonnes (1) peut comprendre une pluralite de reacteurs (22, 26, 30) couples en serie. Le plomb metal forme (5) sort par le fond (15, 35, 36, 37) en coulant des colonnes respectives. Le chlorure de plomb qui n'a pas reagit (6) et, si desire les gaz de procede peuvent etre recircules (8, 9, 10, 7 et 19, 16 respectivement).
PCT/SE1979/000199 1978-10-12 1979-10-04 Methode de recuperation du plomb a partir d'un materiau brut de chlorure de plomb WO1980000852A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DK248980A DK248980A (da) 1978-10-12 1980-06-10 Fremgangsmaade til udvinding af bly fra et blychloridraamateriale

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE7810670 1978-10-12
SE7810670A SE7810670L (sv) 1978-10-12 1978-10-12 Forfarande for utvinning av bly ur en blykloridravara

Publications (1)

Publication Number Publication Date
WO1980000852A1 true WO1980000852A1 (fr) 1980-05-01

Family

ID=20336081

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/SE1979/000199 WO1980000852A1 (fr) 1978-10-12 1979-10-04 Methode de recuperation du plomb a partir d'un materiau brut de chlorure de plomb

Country Status (5)

Country Link
EP (1) EP0020429A1 (fr)
JP (1) JPS55500787A (fr)
DK (1) DK248980A (fr)
SE (1) SE7810670L (fr)
WO (1) WO1980000852A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0117855A1 (fr) * 1983-02-02 1984-09-05 Boliden Aktiebolag Procédé de production du plomb à partir de matières contenant des chlorides de plomb
CN110791661A (zh) * 2019-09-18 2020-02-14 超威电源集团有限公司 一种废铅膏回收处理方法
CN118028610A (zh) * 2024-03-28 2024-05-14 中国恩菲工程技术有限公司 一种含铅氧化渣氨气还原方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2365636A2 (fr) * 1976-09-24 1978-04-21 Penarroya Miniere Metall Recuperation du plomb a partir de solutions de lixiviation selective

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2365636A2 (fr) * 1976-09-24 1978-04-21 Penarroya Miniere Metall Recuperation du plomb a partir de solutions de lixiviation selective

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Gmelins Handbuch der anorganischen Chemie 47:C:1, Verlag Chemie GmbH, Weinheim/Bergstr 1969, p 307. *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0117855A1 (fr) * 1983-02-02 1984-09-05 Boliden Aktiebolag Procédé de production du plomb à partir de matières contenant des chlorides de plomb
US4512803A (en) * 1983-02-02 1985-04-23 Boliden Aktiebolag Process for recovering lead from lead chloride containing raw material
CN110791661A (zh) * 2019-09-18 2020-02-14 超威电源集团有限公司 一种废铅膏回收处理方法
CN118028610A (zh) * 2024-03-28 2024-05-14 中国恩菲工程技术有限公司 一种含铅氧化渣氨气还原方法

Also Published As

Publication number Publication date
JPS55500787A (fr) 1980-10-16
SE7810670L (sv) 1980-04-13
EP0020429A1 (fr) 1981-01-07
DK248980A (da) 1980-06-10

Similar Documents

Publication Publication Date Title
KR100472913B1 (ko) 고압,비촉매방법에의해생성된순도가개선된멜라민
US3816599A (en) Hydrogen chloride recovery
CA1115492A (fr) Production du chlore
US3839550A (en) Closed-cycle thermochemical process for the decomposition of water
SE521482C2 (sv) Sätt att öka lakutbytet av guld vid cyonidbehandling
US4045541A (en) Carbonylation process
US2778726A (en) Purification of refractory metals
US3002816A (en) Method of effecting exothermic catalytic reactions
CA1165780A (fr) Recuperation de produits chlores dans un procede integre pour l'oxychloration et la combustion d'hydrocarbures chlores
WO1980000852A1 (fr) Methode de recuperation du plomb a partir d'un materiau brut de chlorure de plomb
US3688474A (en) Collection of metal carbonyls
IL23892A (en) Process for producing iodine pentafluoride
US2212847A (en) Process for the recovery anb keuti-
US4036776A (en) Recovery of chlorine values from a melt oxidation gas
JPH03103311A (ja) 硫化水素の製造方法およびその製造装置
US4512803A (en) Process for recovering lead from lead chloride containing raw material
US4346069A (en) Recovery of chlorine values in integrated process for oxychlorination and combustion of chlorinated hydrocarbons
US2928731A (en) Continuous process for purifying gallium
US4125590A (en) Method for manufacturing boron trichloride
JPS60208970A (ja) 尿素からメラミンを製造するためのプラントシステム
JPH0633156A (ja) 硫化原料からの亜鉛、鉛、カドミウム等の揮発容易性金属の製法
US2945897A (en) Recovery of 1, 1-dichloroethane
US4028427A (en) Aqueous stream treatment in chlorinated hydrocarbon production
JP2679557B2 (ja) メチルイソシアネートの連続的製造法
US4113786A (en) Hydrogen chloride recovery

Legal Events

Date Code Title Description
AK Designated states

Designated state(s): BR DK JP RO SU US

AL Designated countries for regional patents

Designated state(s): AT CH DE FR GB LU NL