CN1127793A - High-efficiency deleading method and liquid deleading agent for fire refining of antimony - Google Patents

High-efficiency deleading method and liquid deleading agent for fire refining of antimony Download PDF

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Publication number
CN1127793A
CN1127793A CN 95110632 CN95110632A CN1127793A CN 1127793 A CN1127793 A CN 1127793A CN 95110632 CN95110632 CN 95110632 CN 95110632 A CN95110632 A CN 95110632A CN 1127793 A CN1127793 A CN 1127793A
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deleading
antimony
liquid
acid
agent
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CN1047407C (en
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刘伯龙
李俊明
李蓉晖
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  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The fire process for refining Sb while effectively removing Pb features that after atomized by nitrogen, liquid lead remover containing oxacid of phosphorus and sulfuric acid is directly sprayed into molten Sb. Its advantages are high refining speed, lead-removing effect and direct yield.

Description

Efficient deleading method of fire refining of antimony and liquid deleading agent thereof
The present invention relates to a kind of method for removing lead and deleading agent thereof that needle antimony is carried out pyrorefining.
In the pyrorefining antimony process, its associated metallic lead major part enters in the needle antimony, and the finished product star metal or stibium trioxide have certain requirement to the content of lead, star metal requires lead tolerance 0.1-0.2%, stibium trioxide requires lead tolerance less than 0.1%, to reach such standard undoubtedly, must carry out the refining lead-removing operation needle antimony.Existing method for removing lead has vacuum distillation method, chlorination process and liquation process.The vacuum distillation method deleading is effective, but the equipment complexity; The chlorination process direct yield is low, and environmental pollution is serious; Liquation process throughput is little, only the production of suitable high purity antimony.
Weak points such as 94113150.5 number patent application has proposed " a kind of ammonium salt deleading method that is used for fire refining of antimony ", its ammonium salt deleading agent prepares easily, application apparatus is simple, deleading is effective, but exists smog big, and refining time is long.
The purpose of this invention is to provide a kind of efficient deleading method and liquid deleading agent thereof that is used for fire refining of antimony, accomplish to improve refining speed, deleading effect and direct yield.
The present invention seeks to realize like this: at first oxygen acid, sulfuric acid and the stablizer with phosphorus is mixed with liquid deleading agent, directly spray in the high temperature antimony melt after then liquid deleading agent being atomized with nitrogen, plumbous in deleading agent and the melt fully contact fast, and generation is taken off lead more completely and is reacted.
The preparation method of liquid deleading agent is as follows: earlier that oxygen acid, the sulfuric acid of phosphorus is mixed by a certain percentage, carry out processed, and add 15% stablizer then and carry out stabilization treatment, obtain liquid finished product.Stablizer is any one in ammonium chloride, bicarbonate of ammonia, Vanadium Pentoxide in FLAKES, the phosphamide.The oxygen acid of phosphorus includes ortho-phosphoric acid, metaphosphoric acid, tetra-sodium, peroxophosphoric acid, polymer phosphate.
The weight percent of liquid each component of deleading agent is the oxygen acid 80-0% of phosphorus, sulfuric acid 0-85%, stablizer 15%.
Fig. 1 is a reverberatory furnace deleading equipment connection diagram.
Fig. 2 is an electric furnace deleading equipment connection diagram.
Be described in detail algorithm of the present invention and method below in conjunction with drawings and Examples.
Embodiment one, the efficient deleading method of reverberatory furnace.
At first the needle antimony of adding leaded 0.82% in reverberatory furnace 5 is 12 tons, in storage tank 2, add 250 kilograms of liquid deleading agents, start nitrogen machine 1 and volume pump 3 then, respectively nitrogen and liquid deleading agent are sent into nozzle 4, the deleading agent after nitrogen and the atomizing will directly be sprayed in the antimony melt by nozzle 4.Nitrogen plays the atomizing deleading agent and stirs antimony melt dual function.Temperature of reaction is 700-1100 ℃, and the time is 20 minutes, and the lead compound scum silica frost that generates in the reaction process should constantly claw, and can obtain lead tolerance at last and be 0.12% star metal more than 11.5 tons.
Embodiment two, electric furnace highly effective deleading method.
As shown in Figure 2, nitrogengas cylinder 6 is communicated with vial 8 tops by tensimeter 7, and vial 8 bottoms are communicated with crucible 9 middle parts, and crucible 9 is contained in the electric furnace 10.
At first in crucible 9, add leaded 0.52% needle antimony 3000 grams, in vial, add liquid deleading agent 40 grams, be warmed to 850-900 ℃ then, open and to get more than leaded 0.069% star metal 2900 grams.
Compared with the prior art, characteristics of the present invention are the atomizings of deleading agent process, Deleading agent after the atomizing can be sent out with the lead in the antimony melt under the stirring of nitrogen Give birth to i.e. fast again fully reaction, so refining speed is fast, deleading is effective, The direct yield height.

Claims (5)

1, the efficient deleading method of a kind of fire refining of antimony, temperature of reaction is 700---1900 ℃, it is characterized in that directly spraying in the high temperature antimony melt after the liquid deleading agent that will mainly be made up of oxygen acid, the sulfuric acid of phosphorus atomizes with nitrogen.
2, the efficient deleading method of fire refining of antimony according to claim 1 is characterized in that nitrogen machine (1) and volume pump (3) send into nitrogen and liquid deleading agent atomizing in the nozzle (4) respectively.
3, a kind of liquid deleading agent that is used for fire refining of antimony, the weight percent that it is characterized in that each component are oxygen acid 85-0%, sulfuric acid 0-80%, the stablizers 15% of phosphorus.
4, liquid deleading agent according to claim 3 is characterized in that stablizer is any one in ammonium chloride, bicarbonate of ammonia, Vanadium Pentoxide in FLAKES, the ammonium phosphate.
5, liquid deleading agent according to claim 3 is characterized in that the oxygen acid of phosphorus includes ortho-phosphoric acid, metaphosphoric acid, tetra-sodium, peroxophosphoric acid, polymer phosphate.
CN95110632A 1995-01-25 1995-01-25 High-efficiency deleading method and liquid deleading agent for fire refining of antimony Expired - Fee Related CN1047407C (en)

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CN95110632A CN1047407C (en) 1995-01-25 1995-01-25 High-efficiency deleading method and liquid deleading agent for fire refining of antimony

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Application Number Priority Date Filing Date Title
CN95110632A CN1047407C (en) 1995-01-25 1995-01-25 High-efficiency deleading method and liquid deleading agent for fire refining of antimony

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CN1127793A true CN1127793A (en) 1996-07-31
CN1047407C CN1047407C (en) 1999-12-15

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101928842A (en) * 2010-09-27 2010-12-29 娄底市兴华有色金属有限公司 Lead removing agent for use in stibium pyrorefining and lead removing method thereof
CN102041399A (en) * 2010-12-06 2011-05-04 益阳市华昌锑业有限公司 Antimony fire refining lead-removal agent and application thereof
CN102296185A (en) * 2011-09-30 2011-12-28 锡矿山闪星锑业有限责任公司 High-efficiency multifunctional impurity remover and application thereof to antimony fire refining method
CN102517459A (en) * 2012-01-11 2012-06-27 湖南娄底华星锑业有限公司 Method for removing cadmium and ferrum from crude antimony by using metaphosphoric acid
CN102634681A (en) * 2012-05-15 2012-08-15 谈应顺 Deleading agent and deleading method for fire refining of bismuth
CN104046789A (en) * 2014-07-11 2014-09-17 湖南娄底华星锑业有限公司 Compound deleading agent for crude antimony refining and preparation method thereof
CN104073659A (en) * 2014-07-11 2014-10-01 湖南娄底华星锑业有限公司 Method for removing lead, cadmium and iron in crude antimony refining process
CN105970005A (en) * 2016-06-08 2016-09-28 锡矿山闪星锑业有限责任公司 Method for separating lead from antimony with pyrogenic process for high-lead antimony
CN107723473A (en) * 2017-08-18 2018-02-23 西北矿冶研究院 Comprehensive utilization method of high-arsenic-content polymetallic gold ore
EA029375B1 (en) * 2016-10-11 2018-03-30 Республиканское Государственное Предприятие На Праве Хозяйственного Ведения "Национальный Центр По Комплексной Переработке Минерального Сырья Республики Казахстан" Комитета Индустриального Развития И Промышленной Безопасности Министерства По Инвестициям И Развитию Республики Казахстан Reagent for antimony refining to remove lead and tin
CN109371261A (en) * 2018-12-18 2019-02-22 锡矿山闪星锑业有限责任公司 A kind of device that needle antimony quickly refines

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1042653C (en) * 1994-08-19 1999-03-24 锡矿山矿务局 Stibium fire refining deleading agent, its preparation and application
CN1123335A (en) * 1994-11-25 1996-05-29 刘伯龙 Lead-removing method for ammonium salt refined by antimony affination process

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101928842A (en) * 2010-09-27 2010-12-29 娄底市兴华有色金属有限公司 Lead removing agent for use in stibium pyrorefining and lead removing method thereof
CN102041399A (en) * 2010-12-06 2011-05-04 益阳市华昌锑业有限公司 Antimony fire refining lead-removal agent and application thereof
CN102296185A (en) * 2011-09-30 2011-12-28 锡矿山闪星锑业有限责任公司 High-efficiency multifunctional impurity remover and application thereof to antimony fire refining method
CN102517459A (en) * 2012-01-11 2012-06-27 湖南娄底华星锑业有限公司 Method for removing cadmium and ferrum from crude antimony by using metaphosphoric acid
CN102634681A (en) * 2012-05-15 2012-08-15 谈应顺 Deleading agent and deleading method for fire refining of bismuth
CN104073659A (en) * 2014-07-11 2014-10-01 湖南娄底华星锑业有限公司 Method for removing lead, cadmium and iron in crude antimony refining process
CN104046789A (en) * 2014-07-11 2014-09-17 湖南娄底华星锑业有限公司 Compound deleading agent for crude antimony refining and preparation method thereof
CN104073659B (en) * 2014-07-11 2016-02-17 湖南娄底华星锑业有限公司 The method of lead, cadmium, iron is removed in a kind of coarse antimony refining
CN105970005A (en) * 2016-06-08 2016-09-28 锡矿山闪星锑业有限责任公司 Method for separating lead from antimony with pyrogenic process for high-lead antimony
CN105970005B (en) * 2016-06-08 2018-07-06 锡矿山闪星锑业有限责任公司 A kind of high lead-antimony pyrogenic process antimony lead separation method
EA029375B1 (en) * 2016-10-11 2018-03-30 Республиканское Государственное Предприятие На Праве Хозяйственного Ведения "Национальный Центр По Комплексной Переработке Минерального Сырья Республики Казахстан" Комитета Индустриального Развития И Промышленной Безопасности Министерства По Инвестициям И Развитию Республики Казахстан Reagent for antimony refining to remove lead and tin
CN107723473A (en) * 2017-08-18 2018-02-23 西北矿冶研究院 Comprehensive utilization method of high-arsenic-content polymetallic gold ore
CN109371261A (en) * 2018-12-18 2019-02-22 锡矿山闪星锑业有限责任公司 A kind of device that needle antimony quickly refines

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