RU2213698C2 - Method of preparing solution for lead salt production - Google Patents
Method of preparing solution for lead salt production Download PDFInfo
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- RU2213698C2 RU2213698C2 RU2001132522/12A RU2001132522A RU2213698C2 RU 2213698 C2 RU2213698 C2 RU 2213698C2 RU 2001132522/12 A RU2001132522/12 A RU 2001132522/12A RU 2001132522 A RU2001132522 A RU 2001132522A RU 2213698 C2 RU2213698 C2 RU 2213698C2
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- lead
- solution
- salt
- production
- salts
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- 150000003839 salts Chemical class 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000012141 concentrate Substances 0.000 claims abstract description 6
- 238000003763 carbonization Methods 0.000 claims abstract description 4
- MFEVGQHCNVXMER-UHFFFAOYSA-L 1,3,2$l^{2}-dioxaplumbetan-4-one Chemical compound [Pb+2].[O-]C([O-])=O MFEVGQHCNVXMER-UHFFFAOYSA-L 0.000 claims abstract 3
- 229910000003 Lead carbonate Inorganic materials 0.000 claims abstract 3
- 239000003049 inorganic solvent Substances 0.000 claims abstract 2
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 claims abstract 2
- 239000003960 organic solvent Substances 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 239000002244 precipitate Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 2
- 230000000694 effects Effects 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000005530 etching Methods 0.000 abstract 1
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 6
- 230000008021 deposition Effects 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 229910001245 Sb alloy Inorganic materials 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000002140 antimony alloy Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910000978 Pb alloy Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- QQHJESKHUUVSIC-UHFFFAOYSA-N antimony lead Chemical compound [Sb].[Pb] QQHJESKHUUVSIC-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000009851 ferrous metallurgy Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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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
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
Изобретение относится к цветной металлургии и может быть использовано в технологии синтеза свинцовых солей. The invention relates to ferrous metallurgy and can be used in the technology of the synthesis of lead salts.
Известен способ получения раствора свинцовой соли для производства свинцовых крон и других химических соединений (Карякин Ю.В., Ангелов И.И. Чистые химические вещества. - М. : Химия, 1974, с. 315-325). Недостатком способа является длительность процесса, значительные потери свинца, большие эксплуатационные затраты. Для получения раствора свинцовой соли используют чистый металлический свинец. Последний производят пирометаллургическими способами из сульфидных или сульфидно-окисленных свинцовых концентратов по многоступенчатым технологическим схемам. A known method of producing a solution of lead salt for the production of lead crowns and other chemical compounds (Karyakin Yu.V., Angelov II. Pure chemicals. - M.: Chemistry, 1974, S. 315-325). The disadvantage of this method is the duration of the process, significant losses of lead, high operating costs. Pure metallic lead is used to produce a solution of lead salt. The latter is produced by pyrometallurgical methods from sulfide or sulfide-oxidized lead concentrates according to multistage technological schemes.
Наиболее близким способом является способ для производства раствора свинцовой соли с использованием свинцово-сурьмяного сплава (патент-заявка 96112494/25, С 01 G 21/18, С 09 С 1/20, БИ 27, 1998, с. 100. Способ получения раствора свинцовой соли, используемой при производстве свинцовых кронов). The closest method is a method for producing a solution of lead salt using a lead-antimony alloy (patent application 96112494/25, C 01 G 21/18, C 09 C 1/20, BI 27, 1998, p. 100. The method of obtaining the solution lead salt used in the production of lead crowns).
Сурьмяно-свинцовый сплав также получают пирометаллургическим способом из чернового свинца от переработки свинцово-сурьмяного концентрата. Пирометаллургические способы производства свинца или свинцово-сурьмяного сплава экологически опасны (выброс газов SO2-SO3, свинецсодержащих пылей, возгонов свинца, цинка, мышьяка и прочих ядовитых веществ) с потерями свинца более 6,2-8,9%. В целом технологическое производство получения растворов свинцовой соли состоит из двух технологических схем: технологии производства чистого свинца и технологии получения раствора свинцовой соли (см. чертеж).Antimony-lead alloy is also obtained by the pyrometallurgical method from crude lead from the processing of lead-antimony concentrate. Pyrometallurgical methods for the production of lead or lead-antimony alloy are environmentally hazardous (emission of SO 2 -SO 3 gases, lead dust, sublimates of lead, zinc, arsenic and other toxic substances) with lead losses of more than 6.2-8.9%. In general, the technological production of obtaining solutions of lead salt consists of two technological schemes: the technology for the production of pure lead and the technology for producing a solution of lead salt (see drawing).
Разработанный способ исключает необходимость производства чистого металлического свинца из сульфидного концентрата (см. чертеж). Способ осуществляется следующим образом. Свинец из свинцового концентрата растворяют в растворе азотной кислоты при температуре 65-75oС с получением азотнокислого раствора свинца состава: Pb=91; Zn=0,9; Fe=50 г/л; Со=2,3; Ni=17,2; Ca=22,5; Mn=190; Mg=1,6 мг/л, рН 2,1-0,5.The developed method eliminates the need for the production of pure metallic lead from sulfide concentrate (see drawing). The method is as follows. Lead from a lead concentrate is dissolved in a solution of nitric acid at a temperature of 65-75 o With obtaining nitric acid solution of lead composition: Pb = 91; Zn = 0.9; Fe = 50 g / l; Co = 2.3; Ni = 17.2; Ca = 22.5; Mn = 190; Mg = 1.6 mg / L, pH 2.1-0.5.
Методом селективного осаждения PbSO4 (введением Н2SO4-Na2SO4) проводится отделение свинца от примесей. Полученная чистая соль PbSO4 является исходным продуктом для синтеза других солей свинца. Из соли PbSO4 методом карбонизации составом [Na2СО3-Н2О-СО2] синтезируется соль РbСО3.The method of selective deposition of PbSO 4 (the introduction of H 2 SO 4 -Na 2 SO 4 ) is the separation of lead from impurities. The resulting pure salt of PbSO 4 is the starting material for the synthesis of other lead salts. The PbCO 3 salt is synthesized from the PbSO 4 salt by carbonation with the composition [Na 2 CO 3 -H 2 O-CO 2 ].
Пример 1. Example 1
Степень очистки раствора свинца от примесей в процессе осаждения PbSO4 зависит от рН суспензии (табл.1). Присутствующие в азотнокислом растворе примеси с различной степенью осаждаются в области рН 2,2 и менее (рН 2,1÷0,5). Оптимальными условиями разделения свинца и примесей установлено: при рН менее 1,5, при осаждении соли PbSO4 не осаждаются элементы примеси; с переходом в область рН>1,5 протекает осаждение примесей. Другие условия осаждения PbSO4 (время, температура процесса, перемешивание) не изменяют значения рН осаждения PbSO4.The degree of purification of the solution of lead from impurities during the deposition of PbSO 4 depends on the pH of the suspension (table 1). Impurities present in a nitric acid solution with various degrees of precipitation in the range of pH 2.2 and less (pH 2.1 ÷ 0.5). The optimal conditions for the separation of lead and impurities have been established: at pH less than 1.5, impurity elements do not precipitate during the precipitation of the PbSO 4 salt; with the transition to a pH range> 1.5, the deposition of impurities proceeds. Other conditions for the deposition of PbSO 4 (time, process temperature, stirring) do not change the pH of the deposition of PbSO 4 .
Пример 2. Example 2
Полученная соль PbSO4 является основой для синтеза РbСО3. Состав соли РbСО3 зависит от температуры, смеси подаваемого реагента для карбонизации PbSO4. Процесс проводится в суспензии (т:ж=1:1) введением смеси раствора Nа2СО3 100-200 г/л + CO2] или [Н2СО3 100-200 г/л + СO2] при температуре суспензии на уровне 50-60oС (оптимальный уровень) (табл.2). Полученный осадок после карбонизации представляет монофазу РbСО3 (отсутствуют другие соли).The resulting salt of PbSO 4 is the basis for the synthesis of PbCO 3 . The composition of the salt of PbCO 3 depends on temperature, the mixture of the supplied reagent for the carbonization of PbSO 4 . The process is carried out in suspension (t: W = 1: 1) by introducing a mixture of a solution of Na 2 CO 3 100-200 g / l + CO 2 ] or [H 2 CO 3 100-200 g / l + CO 2 ] at a temperature of the suspension level of 50-60 o C (optimal level) (table 2). The resulting precipitate after carbonization is a monophase of PbCO 3 (no other salts are present).
Пример 3. Example 3
Соль РbСО3 является исходным продуктом для синтеза других солей свинца. Соль РbСО3 растворяют в растворе азотной кислоты с получением раствора соли свинца Рb(NО3)3.Salt PbCO 3 is the starting material for the synthesis of other salts of lead. The PbCO 3 salt is dissolved in a solution of nitric acid to obtain a solution of the lead salt Pb (NO 3 ) 3 .
Оксидные соединения получены термообработкой:
Свинец (II) уксуснокислый синтезировали растворением:
РbО+2СН3СООН-->Рb(СН3СОО)2+Н2О
и последующей упаркой
Соль хромовокислого свинца приготовлена осаждением:
Oxide compounds obtained by heat treatment:
Lead (II) acetic acid was synthesized by dissolving:
PbO + 2CH 3 COOH -> Pb (CH 3 COO) 2 + H 2 O
and subsequent evaporation
Lead chromate is prepared by precipitation:
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103374657A (en) * | 2012-04-24 | 2013-10-30 | 湖北金洋冶金股份有限公司 | Ultrafine lead oxide prepared by using waste lead plaster and preparation method thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB404007A (en) * | 1932-07-01 | 1934-01-01 | Stuart Sidney Webb Bowen | Improvements in and relating to methods and apparatus for the production of lead pigments |
RU2039707C1 (en) * | 1992-03-18 | 1995-07-20 | Лермонтовское производственное объединение "Алмаз" | Method for production of lead nitrate solution |
RU96112494A (en) * | 1996-06-19 | 1998-09-27 | Акционерное общество открытого типа "Полиэкс" | METHOD FOR PRODUCING A LEAD SALT SOLUTION USED IN THE PRODUCTION OF LEAD CROWNS |
-
2001
- 2001-11-30 RU RU2001132522/12A patent/RU2213698C2/en not_active IP Right Cessation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB404007A (en) * | 1932-07-01 | 1934-01-01 | Stuart Sidney Webb Bowen | Improvements in and relating to methods and apparatus for the production of lead pigments |
RU2039707C1 (en) * | 1992-03-18 | 1995-07-20 | Лермонтовское производственное объединение "Алмаз" | Method for production of lead nitrate solution |
RU96112494A (en) * | 1996-06-19 | 1998-09-27 | Акционерное общество открытого типа "Полиэкс" | METHOD FOR PRODUCING A LEAD SALT SOLUTION USED IN THE PRODUCTION OF LEAD CROWNS |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103374657A (en) * | 2012-04-24 | 2013-10-30 | 湖北金洋冶金股份有限公司 | Ultrafine lead oxide prepared by using waste lead plaster and preparation method thereof |
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