CN103602834B - Selective oxidation-reduction method for recycling arsenic and antimony from arsenic-antimony smoke - Google Patents
Selective oxidation-reduction method for recycling arsenic and antimony from arsenic-antimony smoke Download PDFInfo
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- CN103602834B CN103602834B CN201310545140.2A CN201310545140A CN103602834B CN 103602834 B CN103602834 B CN 103602834B CN 201310545140 A CN201310545140 A CN 201310545140A CN 103602834 B CN103602834 B CN 103602834B
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- Prior art keywords
- antimony
- arsenic
- selective oxidation
- flue dust
- reduction method
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Links
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 61
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 50
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 38
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 230000033116 oxidation-reduction process Effects 0.000 title claims abstract description 11
- DLISVFCFLGSHAB-UHFFFAOYSA-N antimony arsenic Chemical compound [As].[Sb] DLISVFCFLGSHAB-UHFFFAOYSA-N 0.000 title abstract description 10
- 239000000779 smoke Substances 0.000 title abstract 5
- 238000004064 recycling Methods 0.000 title abstract 4
- 239000000463 material Substances 0.000 claims abstract description 17
- 230000001590 oxidative effect Effects 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000003500 flue dust Substances 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 230000002829 reductive effect Effects 0.000 claims description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 10
- 239000003546 flue gas Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 10
- IHBMMJGTJFPEQY-UHFFFAOYSA-N sulfanylidene(sulfanylidenestibanylsulfanyl)stibane Chemical compound S=[Sb]S[Sb]=S IHBMMJGTJFPEQY-UHFFFAOYSA-N 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000003245 coal Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 2
- GOLCXWYRSKYTSP-UHFFFAOYSA-N Arsenious Acid Chemical compound O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 abstract description 6
- AHBGXHAWSHTPOM-UHFFFAOYSA-N 1,3,2$l^{4},4$l^{4}-dioxadistibetane 2,4-dioxide Chemical compound O=[Sb]O[Sb](=O)=O AHBGXHAWSHTPOM-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000411 antimony tetroxide Inorganic materials 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract description 2
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 abstract 1
- 238000003723 Smelting Methods 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000002386 leaching Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 229960002594 arsenic trioxide Drugs 0.000 description 3
- KTTMEOWBIWLMSE-UHFFFAOYSA-N diarsenic trioxide Chemical compound O1[As](O2)O[As]3O[As]1O[As]2O3 KTTMEOWBIWLMSE-UHFFFAOYSA-N 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- DJHGAFSJWGLOIV-UHFFFAOYSA-N Arsenic acid Chemical compound O[As](O)(O)=O DJHGAFSJWGLOIV-UHFFFAOYSA-N 0.000 description 1
- RMBBSOLAGVEUSI-UHFFFAOYSA-H Calcium arsenate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-][As]([O-])([O-])=O.[O-][As]([O-])([O-])=O RMBBSOLAGVEUSI-UHFFFAOYSA-H 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 229940000488 arsenic acid Drugs 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- ZODDGFAZWTZOSI-UHFFFAOYSA-N nitric acid;sulfuric acid Chemical compound O[N+]([O-])=O.OS(O)(=O)=O ZODDGFAZWTZOSI-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
Classifications
-
- 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
Abstract
The invention relates to a selective oxidation-reduction method for recycling arsenic and antimony from arsenic-antimony smoke, belonging to the field of nonferrous metallurgy technologies. The method comprises steps of firstly, selectively oxidizing and recycling arsenic: introducing oxidizing gas into arsenic-antimony smoke, reacting for 20-90 minutes at 400-800 DEG C, collecting the As2O3 volatile smoke in reaction; after reaction is completed, obtaining a secondary material containing antimony; then reducing and recycling antimony: adding a reducing agent into the secondary material containing antimony (obtained in the former step), reacting for 30-180 minutes at 800-1000 DEG C, thus obtaining crude antimony. Based on the characteristics that arsenic trioxide is easy to volatilize and antimony tetroxide is difficult to volatilize at a low temperature, the selective oxidation-reduction method has the beneficial effects that selective oxidization is carried out on the arsenic-antimony smoke, arsenic is volatilized, separated and removed, and finally reduction smelting is carried out so as to obtain the crude antimony; therefore, the method is simple and has good industrial application prospect.
Description
Technical field
The present invention relates to the method that a kind of selective oxidation-reduction method reclaims arsenic, antimony in As and Sb flue dust, belong to technical field of non-ferrous metallurgy.
Background technology
Smelt and reclaim in precious metal process at heavy metal, often contain higher arsenic antimony in the flue dust of generation, this is valuable secondary resource.In order to fully utilize valuable metal, reduce environmental pollution, strengthen the research of arsenic antimony isolation technique is significant.
The method separating about arsenic antimony at present has two kinds of pyrogenic process and wet methods.During pyrogenic process separates, the most frequently used is vacuum distillation method, utilizes the difference of its boiling point character and arsenic antimony is separated, though this method separates arsenic, antimony efficiently, vacuum distillation technique conditional request is high and security of enviromental protection measure is required tight, and Financial cost is also higher.The wet separation of arsenic antimony is divided into two kinds of acid system and alkaline process.Acid system is taking sulfuric acid-nitric acid mixing solutions as leaching agent, even if nitric acid leaching agent is wherein again the oxygenant of arsenic.Spray into milk of lime, arsenic acid is precipitated as to Tricalcium arsenate and removes.Alkaline process-electrochemical lixiviation process is in alkaline leaching groove, to pack anode, negative electrode into, and passes to direct current, the leaching of strengthening arsenic.
In high-arsenic dust electric heating rotary kiln roasting method dearsenicating technology, its process characteristic is to have utilized the volatile character of white arsenic under low temperature, makes As with As
2o
3form volatilization remove, As
2o
3in the time of 120 DEG C, start distillation, just volatilization strongly during to 500 DEG C, and antimony is through being oxidized to Sb
2o
4after be but difficult to volatilization.As under differing temps
2o
3vapour pressure as following table 1.
Table 1As
2o
3vapour pressure and the relation of temperature
The oxidising process of arsenic and antimony is carried out step by step, and its reaction is as follows:
2As+3/2O
2=2As
2O
3 (1)
As
2O
3+O
2=As
2O
5 (2)
2Sb+3/2O
2=2Sb
2O
3 (3)
Sb
2O
3+1/2O
2=Sb
2O
4 (4)
Adopt HSC software for calculation known, the oxygen gesture lgP of reaction (1) ~ (4)
o2the following Fig. 1 of temperature variant relation.
As shown in Figure 1, in temperature higher than 673K, lgP
o2in the time of-4.87 ~ 5.87Pa, can realize and make antimonous oxide be oxidized to Sb
2o
4, and As
2o
3not oxidized, can not be further oxidized to As
2o
5.Under these conditions, arsenic is oxidized to As
2o
3and volatilization removes, antimony is oxidized to the Sb that is difficult to volatilization
2o
4thereby, arsenic antimony is separated.
Summary of the invention
For problem and the deficiency of above-mentioned prior art existence, the invention provides the method for arsenic, antimony in a kind of selective oxidation-reduction method recovery As and Sb flue dust.The present invention makes full use of under low temperature that white arsenic is volatile, the not volatile feature of antimony tetroxide, As and Sb flue dust is carried out to selective oxidation, and the separation removal arsenic that volatilizees, carry out again retailoring and obtain needle antimony, technique is simple, have good prospects for commercial application, the present invention is achieved through the following technical solutions.
Selective oxidation-reduction method reclaims a method for arsenic, antimony in As and Sb flue dust, and its concrete steps are as follows:
(1) selective oxidation reclaim arsenic: in As and Sb flue dust, pass into the oxidizing gas that flow is 0.01～0.5L/min, temperature be 400～800 DEG C reaction 20～90min, in this process to As
2o
3volatilization flue gas is collected, and has reacted rear acquisition secondary antimong-containing material;
(2) antimony is reclaimed in reduction: the secondary antimong-containing material obtaining to step (1) is 10:(1～3 according to the mass ratio of secondary antimong-containing material and reductive agent) add reductive agent, be to react 30～180min under 800～1000 DEG C of conditions in temperature, can obtain needle antimony.
Described As and Sb flue dust comprises the component of following mass percent: arsenic content is 5～20%, and antimony content is 30～60%.
Described oxidizing gas is air, oxygen-rich air or oxygen.
In described step (1) to As
2o
3the collection of volatilization flue gas adopts bag collection.
Described reductive agent is one or more the arbitrary proportion mixtures in fine coal, oil, coke powder.
The invention has the beneficial effects as follows: present method makes full use of under low temperature that white arsenic is volatile, the not volatile feature of antimony tetroxide, As and Sb flue dust is carried out to selective oxidation, and the separation removal arsenic that volatilizees, carry out again retailoring and obtain needle antimony, technique is simple, has good prospects for commercial application.
Brief description of the drawings
Fig. 1 is the temperature variant graph of a relation of oxygen gesture of arsenic sb oxide of the present invention;
Fig. 2 is process flow sheet of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
As shown in Figure 2, this selective oxidation-reduction method reclaims the method for arsenic, antimony in As and Sb flue dust, and its concrete steps are as follows:
(1) selective oxidation reclaims arsenic: to As and Sb flue dust, (As and Sb flue dust comprises the component of following mass percent: arsenic content is 5%, antimony content is 30%) in pass into the oxidizing gas that flow is 0.01L/min, temperature be 400 DEG C reaction 20min, in this process to As
2o
3volatilization flue gas is collected, and has reacted rear acquisition secondary antimong-containing material, and wherein oxidizing gas is air, As
2o
3the collection of volatilization flue gas adopts bag collection;
(2) antimony is reclaimed in reduction: in the secondary antimong-containing material obtaining to step (1), being that 10:1 adds reductive agent according to the mass ratio of secondary antimong-containing material and reductive agent, is to react 30min under 800 DEG C of conditions in temperature, can obtain needle antimony, and wherein reductive agent is fine coal.
Detect and know through sampling, in needle antimony, containing antimony 91.4%, containing arsenic 0.39%, the rate of recovery of antimony is 86.5%.
Embodiment 2
As shown in Figure 2, this selective oxidation-reduction method reclaims the method for arsenic, antimony in As and Sb flue dust, and its concrete steps are as follows:
(1) selective oxidation reclaims arsenic: to As and Sb flue dust, (As and Sb flue dust comprises the component of following mass percent: arsenic content is 20%, antimony content is 60%) in pass into the oxidizing gas that flow is 0.5L/min, temperature be 800 DEG C reaction 90min, in this process to As
2o
3volatilization flue gas is collected, and has reacted rear acquisition secondary antimong-containing material, and wherein oxidizing gas is oxygen-rich air, to As
2o
3the collection of volatilization flue gas adopts bag collection;
(2) antimony is reclaimed in reduction: in the secondary antimong-containing material obtaining to step (1), be that 10:3 adds reductive agent according to the mass ratio of secondary antimong-containing material and reductive agent, be to react 180min under 1000 DEG C of conditions in temperature, can obtain needle antimony, wherein reductive agent is fine coal, oil and the coke powder mixture of quality 1:1:1.
Detect and know through sampling, in needle antimony, containing antimony 90.2%, containing arsenic 0.35%, the rate of recovery of antimony is 88.2%.
Embodiment 3
As shown in Figure 2, this selective oxidation-reduction method reclaims the method for arsenic, antimony in As and Sb flue dust, and its concrete steps are as follows:
(1) selective oxidation reclaims arsenic: to As and Sb flue dust, (As and Sb flue dust comprises the component of following mass percent: arsenic content is 15%, antimony content is 40%) in pass into the oxidizing gas that flow is 0.4L/min, temperature be 600 DEG C reaction 70min, in this process to As
2o
3volatilization flue gas is collected, and has reacted rear acquisition secondary antimong-containing material, and wherein oxidizing gas is oxygen, to As
2o
3the collection of volatilization flue gas adopts bag collection;
(2) antimony is reclaimed in reduction: in the secondary antimong-containing material obtaining to step (1), be that 10:2 adds reductive agent according to the mass ratio of secondary antimong-containing material and reductive agent, be to react 120min under 900 DEG C of conditions in temperature, can obtain needle antimony, wherein reductive agent is fine coal and the coke powder mixture of mass ratio 1:1.
Detect and know through sampling, in needle antimony, containing antimony 93.5%, containing arsenic 0.31%, the rate of recovery of antimony is 89.6%.
Claims (4)
1. selective oxidation-reduction method reclaims a method for arsenic, antimony in As and Sb flue dust, it is characterized in that concrete steps are as follows:
(1) selective oxidation reclaim arsenic: in As and Sb flue dust, pass into the oxidizing gas that flow is 0.01～0.5L/min, temperature be 400～800 DEG C reaction 20～90min, in this process to As
2o
3volatilization flue gas is collected, and has reacted rear acquisition secondary antimong-containing material;
(2) antimony is reclaimed in reduction: in the secondary antimong-containing material obtaining to step (1), be 10:(1～3 according to the mass ratio of secondary antimong-containing material and reductive agent) add reductive agent, be to react 30～180min under 800～1000 DEG C of conditions in temperature, can obtain needle antimony, described reductive agent is one or more the arbitrary proportion mixtures in fine coal, oil, coke powder.
2. selective oxidation according to claim 1-reduction method reclaims the method for arsenic, antimony in As and Sb flue dust, it is characterized in that: described As and Sb flue dust comprises the component of following mass percent: arsenic content is 5～20%, and antimony content is 30～60%.
3. selective oxidation according to claim 1 and 2-reduction method reclaims the method for arsenic, antimony in As and Sb flue dust, it is characterized in that: described oxidizing gas is air, oxygen-rich air or oxygen.
4. selective oxidation according to claim 1 and 2-reduction method reclaims the method for arsenic, antimony in As and Sb flue dust, it is characterized in that: in described step (1) to As
2o
3the collection of volatilization flue gas adopts bag collection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310545140.2A CN103602834B (en) | 2013-11-07 | 2013-11-07 | Selective oxidation-reduction method for recycling arsenic and antimony from arsenic-antimony smoke |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310545140.2A CN103602834B (en) | 2013-11-07 | 2013-11-07 | Selective oxidation-reduction method for recycling arsenic and antimony from arsenic-antimony smoke |
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| Publication Number | Publication Date |
|---|---|
| CN103602834A CN103602834A (en) | 2014-02-26 |
| CN103602834B true CN103602834B (en) | 2014-09-03 |
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Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104294053B (en) * | 2014-11-01 | 2016-05-11 | 中南大学 | A kind of method that separates arsenic from arsenic-containing smoke dust reduction volatilization |
| CN104451171B (en) * | 2014-12-18 | 2016-08-17 | 中南大学 | A kind of method of arsenic-containing smoke dust fluidization dearsenization |
| CN104789786B (en) * | 2015-04-01 | 2017-03-15 | 郴州雄风环保科技有限公司 | A kind of harmlessness disposing arsenic-containing waste residue and the method for synthetical recovery wherein valuable metal |
| CN105695742B (en) * | 2016-02-24 | 2017-11-10 | 锡矿山闪星锑业有限责任公司 | A kind of smelting process of antimony oxygen low-temperature reduction antimony |
| CN106381396B (en) * | 2016-09-13 | 2018-08-10 | 昆明理工大学 | A kind of method that solid oxidizer roasting high-arsenic antimony flue dust detaches arsenic, antimony and recycling wherein antimony |
| CN106702170B (en) * | 2016-12-16 | 2019-02-19 | 昆明理工大学 | A kind of method that high-arsenic antimony soot oxidation-fixation separates arsenic and recycles arsenic, antimony |
| CN107058746B (en) * | 2017-04-27 | 2018-12-07 | 郴州市金贵银业股份有限公司 | A method of separating antimony from silver-colored smelting ash |
| CN107130115B (en) * | 2017-04-27 | 2018-12-07 | 郴州市金贵银业股份有限公司 | A method of separating arsenic, antimony from silver-colored smelting ash |
| CN107828967B (en) * | 2017-10-20 | 2019-12-03 | 昆明理工大学 | A kind of method that copper anode mud reduction-organic sulfide method separates arsenic and recycles antimony, tin |
| CN109628761B (en) * | 2018-12-29 | 2021-06-11 | 焱鑫环保科技有限公司 | Method for producing antimony white by using high-antimony secondary smoke dust to remove arsenic |
| CN109762996A (en) * | 2019-03-07 | 2019-05-17 | 昆明理工大学 | A kind of method that high-antimony low arsenic soot oxidation-vulcanization fixation separates arsenic and recycles antimony |
| CN110398403B (en) * | 2019-07-29 | 2022-05-17 | 华北电力大学（保定） | Preparation method and device of stable arsenic trioxide standard gas |
| CN113955799A (en) * | 2021-10-20 | 2022-01-21 | 山东恒邦冶炼股份有限公司 | Method for purifying antimony-containing arsenic trioxide |
| CN114086002A (en) * | 2021-11-24 | 2022-02-25 | 云南锡业研究院有限公司 | Method for efficiently separating arsenic and antimony from high-arsenic smoke dust |
| CN117025979A (en) * | 2023-08-01 | 2023-11-10 | 昆明理工大学 | Method for efficiently enriching antimonous oxide in vacuum by using crude antimonous oxide |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4244734A (en) * | 1979-07-19 | 1981-01-13 | Hazen Research, Inc. | Process for recovering metal values from materials containing arsenic |
| CN101412538B (en) * | 2008-11-10 | 2010-08-11 | 江苏康洁环境工程有限公司 | Method for extracting arsenic trioxide from roasting dust of arsenic-containing gold concentrate powder |
| CN101654744A (en) * | 2009-09-10 | 2010-02-24 | 东营方圆有色金属有限公司 | Reverberatory furnace pyrorefining method of crude copper with high arsenic and antimony |
| CN102286665B (en) * | 2011-09-05 | 2012-10-31 | 耒阳市焱鑫有色金属有限公司 | Comprehensive recovery method for complicated materials containing arsenic and valuable metal slag dust |
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