CN110331279A - A kind of microwave calcining stibnite concentrate directly volatilizees the method for recycling antimony oxide - Google Patents
A kind of microwave calcining stibnite concentrate directly volatilizees the method for recycling antimony oxide Download PDFInfo
- Publication number
- CN110331279A CN110331279A CN201910626967.3A CN201910626967A CN110331279A CN 110331279 A CN110331279 A CN 110331279A CN 201910626967 A CN201910626967 A CN 201910626967A CN 110331279 A CN110331279 A CN 110331279A
- Authority
- CN
- China
- Prior art keywords
- microwave
- antimony
- stibnite concentrate
- stibnite
- concentrate
- Prior art date
- Legal status (The legal status 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 status listed.)
- Granted
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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
-
- 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
It directly volatilizees the method for antimony trisulfide the present invention relates to a kind of microwave calcining stibnite concentrate, belongs to antimony metallurgical technology field.In order to solve the problems, such as that long flow path existing for existing stibium fire smelting technique, energy consumption are high, consumption is big, metal antimony recovery is low, at high cost, 1) directly the volatilize method of antimony trisulfide of the microwave calcining stibnite concentrate includes the following steps: using antimony concentrate as raw material；2) stibnite concentrate after crushing grinding is placed in quartz boat, is placed in microwave heating furnace cavity；3) microwave is opened, while blasting oxygen-enriched air, oxidizing roasting generates antimony oxide in the process；4) due to the characteristic that antimony oxide easily distils, generated antimony oxide cigarette vapour is discharged through microwave reactor gas outlet, and flue gas after cooling is collected to obtain the higher antimony oxide of purity by device for recovering powder.The present invention selects microwave as heat source, has many advantages, such as that process flow is short, low energy consumption, heating efficiency is high, simple to operation.
Description
Technical field
It directly volatilizees the method for antimony trisulfide the present invention relates to a kind of microwave calcining stibnite concentrate, belongs to antimony metallurgical technology neck
Domain.
Background technique
There are pyrogenic process and two kinds of wet process applied to the method for antimony regulus at present, but industrially mainly based on antimony pyrometallurgical smelting.Fire
In method, most enterprises use volatilization roasting (melting) -- reduction melting, are mainly characterized by " low column, the thin bed of material, high coke yield ",
This makes the technique, and there are long flow paths, the high and low concentration SO of energy consumption2The drawbacks such as smoke pollution.Wherein most widely used is blast furnace
Volatile smelting technique, this technique is mainly by the Sb in stibnite concentrate2S3It is oxidized to by oxidizing roasting volatile
Sb2O3.The Sb evaporated2O3Into flue gas, pass through the further cooling and available needle antimony oxygen of recovered flue gas.The process work
Skill long flow path, energy consumption is high, and production efficiency is low.
In order to solve the problems, such as that energy consumption height and production efficiency are low, 103173637 B of patent CN discloses a kind of antimony trisulfide essence
Mine oxygen-enriched smelting method and side-blown converter, this method by stibnite concentrate carry out ingredient, granulation then be added side-blown converter in into
Row oxygen-rich oxide.The method achieve the autogenous smeltings of stibnite concentrate, reduce energy consumption.But because wanting first ingredient and granulation,
And process is cumbersome.
107858530 A of patent CN discloses a kind of method of antimony sulfide ore oxygen-enriched air smelting, although the method increase lifes
Efficiency is produced, but needs to carry out antimony sulfide ore broken granulation in fusion process, and also need to preheat oxygen-enriched air.
Cause process flow long, it is inconvenient.
Since above insufficient and disadvantage, the above several method all not can apply in industrial production, China is main at this stage
Stibium smelting technology or blast furnace volatile smelting.Therefore, need to seek that a kind of process flow is short, antimony regulus method of low energy consumption.
Microwave metallurgical as a kind of novel green metallurgical technology, have been applied in ore dressing, ore grinding, drying, roasting, calcining,
In the metallurgical process such as sintering, reduction, oxidation, melting, purification and purification.Compared with traditional heating mode, have the following characteristics that
(1) selectivity heating, the rate of heat addition is fast, and heating efficiency is high；(2) environmentally friendly；(3) low energy consumption.Patent CN 105948123
A discloses a kind of method for preparing low-sulfur molybdenum trioxide, and this method reaches high-efficient roasting brightness molybdenum by using Microwave Pretreatment
Mine.Fully utilize the advantage of microwave heating.
Microwave directly heats object by energy dissipation of the microwave inside material as a kind of green high-efficient heating method
Material, therefore sample is heated by microwave, heat transfer direction is from inside to outside, compared to traditional heating side from outside to inside
Formula, microwave heating are more advantageous to the volatilization of antimony oxide.Furthermore stibnite concentrate is normal in microwave frequency band dielectric with higher
Number (8 ~ 30) and dielectric loss (0.2 ~ 0.8), has stronger response to microwave, and in mineral other compositions dielectric constant (4 ~
12) weaker to responding microwave, it can be very good the characteristics of heating using microwave selective.Therefore stibnite concentrate can preferentially inhale wave
And oxidation reaction occurs, antimony oxide product can be rapidly achieved fusing point (655 DEG C) and be more likely to volatilize.Therefore by microwave applications in roasting
Stibnite concentrate is burnt to be with a wide range of applications come the antimony trisulfide therein that volatilizees.
Summary of the invention
The method flow that the present invention passes through blast furnace volatile smelting for stibnite concentrate is long, energy consumption is high, consumption is big, cost
High, environmental pollution is serious problem proposes a kind of microwave calcining stibnite concentrate and directly volatilizees the process of antimony trisulfide, this hair
It is bright to be achieved through the following technical solutions.
A kind of microwave calcining stibnite concentrate directly volatilizees the method for antimony trisulfide, the specific steps of which are as follows:
(1) select antimony concentrate as starting material, the mass percentage of Sb is 35 ~ 55%, S mass percentage > 20%；
(2) antimony concentrate material selected in step (1) is ground, the stibnite concentrate of 40 ~ 200 mesh is taken to be placed in quartz boat
Middle tiling is to 2.5 ~ 5.0cm, and being placed on microwave power is 0 ~ 20kW, and frequency is 2450Hz ± 50Hz or 915Hz ± 50Hz
Heating furnace chamber body in；
(3) microwave is opened, while with 1.5 ~ 2.0m3The rate of/h blasts air, adjusts microwave output power, will be levigate after sulphur
Change antimony concentrate is from room temperature with the roasting process the first heating stage in the affiliated step of 50 ~ 100/min (3) with 50 ~ 100 DEG C/min temperature rise
Rate is rapidly heated to 200 ~ 300 DEG C, keeps the temperature 30 ~ 60min；Second temperature rise period was warming up to 20 ~ 40 DEG C/min temperature rise rate
Maturing temperature；Rate is rapidly heated to 950 ~ 1050 DEG C, keeps the temperature 1 ~ 2h;
(4) fume recovery, be rapidly heated and roasting process in generated flue gas be discharged through microwave reactor gas outlet,
Flue dust is collected, collected flue dust is the needle antimony oxygen powder of the powder containing antimony oxide, and mass percentage containing antimony is greater than 80%；
(5) after step (2) keep the temperature 1 ~ 2h, microwave is closed, remaining slag is taken out after natural cooling.
Further, the stibnite concentrate in the step (1) includes following mass percent component: antimony 42.444%, sulphur
35.075%, silicon 17.184%, iron 5.026%, arsenic 0.122%, lead 0.090%, zinc, 0.060%；
Further, the antimony trisulfide in stibnite concentrate occurs following to react and enter cigarette during heating in the step (3)
In gas:
Further, it can be used for further restoring by the obtained needle antimony oxygen of fume recovery in the step (3) and obtain metallic antimony.
The beneficial effects of the present invention are:
(1) this method is volatilized antimony trisulfide therein using microwave roasting direct stibnite concentrate, and process flow is short, environmental pollution
Small, operation is easier；
(2) since stibnite concentrate is in microwave frequency band dielectric constant with higher and dielectric loss, there is stronger sound to microwave
It answers and the characteristics of microwave selective heats, material heating efficiency is high, and reaction rate is fast, and products obtained therefrom is high-quality；
(3) due to microwave " body heating " characteristic, make material entirety thermally equivalent, oxidation process does not generate temperature gradient, product at
Point and uniform particle sizes.
[Detailed description of the invention]
Fig. 1 is microwave tube type oven apparatus structure schematic diagram used in the present invention.
In figure: 1- oxygen-enriched air storage tank, 2- flow controller, 3- air inlet, 4- quartz ampoule, 5- silica crucible, 6- number
Word display system, 7- Current Voltage display instrument, 8- microwave power controller, 9- scram button, the gas outlet 10-, the recycling of 11- dust
Device.
Fig. 2 is present invention specific implementation flow chart.
Specific embodiment
Below with reference to specific embodiment, the invention will be further described.
Embodiment 1
Stibnite concentrate is ground into 150 mesh first, the stibnite concentrate 40g after then taking grinding is into quartz boat, and tiling is extremely
With a thickness of 2.5cm, it is placed in Wave heating furnace cavity.
Power supply is opened, while with 1.5cm3The speed of/h blasts air into microwave cavity, passes through the microwave of microwave equipment
Controller adjusting output microwave power is 6kW, output frequency is 2450MHz ± 50Hz.
Observe rate temperature change in real time by device display, the control rate of heat addition is 50 DEG C/min, be rapidly heated to
200 DEG C, keep the temperature 40min and with 20 DEG C/min temperature rise rate be heated to 950 DEG C, in temperature-rise period to flue gas caused by roasting into
Row recycling.Microwave power control heating temperature is adjusted in 950 DEG C of heat preservation 40min.
After roasting, stopping blasts air and simultaneously closes off microwave.Remaining slag is taken out after natural cooling.To cigarette after cooling
Gas carries out recycling analysis.Collected antimony oxygen powder, mass percentage containing antimony are greater than 80%.
Embodiment 2
Stibnite concentrate is ground into 180 mesh first, the stibnite concentrate 60g after then taking grinding is into quartz boat, and tiling is extremely
With a thickness of 3.0cm, it is placed in Wave heating furnace cavity.
Power supply is opened, while with 1.8cm3The speed of/h blasts air into microwave cavity, passes through the microwave of microwave equipment
Controller adjusting output microwave power is 12kW, output frequency is 2450MHz ± 50Hz.
Observe rate temperature change in real time by device display, the control rate of heat addition is 70 DEG C/min, be rapidly heated to
250 DEG C, 40min is kept the temperature with 40 DEG C/min temperature rise rate and is heated to 1000 DEG C, to flue gas caused by roasting in temperature-rise period
It is recycled.Microwave power control heating temperature is adjusted in 1000 DEG C of heat preservation 50min.
After roasting, stopping blasts air and simultaneously closes off microwave.Remaining slag is taken out after natural cooling.To cigarette after cooling
Gas carries out recycling analysis.Collected antimony oxygen powder, mass percentage containing antimony are greater than 80%.
Embodiment 3
Stibnite concentrate is ground into 200 mesh first, the stibnite concentrate 90g after then taking grinding is into quartz boat, and tiling is extremely
With a thickness of 4.0cm, it is placed in Wave heating furnace cavity.
Power supply is opened, while with 1.8cm3The speed of/h blasts air into microwave cavity, passes through the microwave of microwave equipment
Controller adjusting output microwave power is 18kW, output frequency is 2450MHz ± 50Hz.
Observe rate temperature change in real time by device display, the control rate of heat addition is 100 DEG C/min, be rapidly heated to
300 DEG C, 50min is kept the temperature, is heated to 1050 DEG C with 50 DEG C/min temperature rise rate, to flue gas caused by roasting in temperature-rise period
It is recycled.Microwave power control heating temperature is adjusted in 1050 DEG C of heat preservation 60min.
After roasting, stopping blasts air and simultaneously closes off microwave.Remaining slag is taken out after natural cooling.To cigarette after cooling
Gas carries out recycling analysis.Collected antimony oxygen powder, mass percentage containing antimony are greater than 85%.
Claims (7)
- A kind of method of antimony trisulfide 1. microwave calcining antimony trisulfide directly volatilizees, it is characterised in that specific step is as follows:(1) select antimony concentrate as starting material, the mass percentage of Sb is 35 ~ 55%, S mass percentage > 20%；(2) antimony concentrate material selected in step (1) is ground, takes stibnite concentrate (wherein 200 mesh of 40 ~ 200 mesh 80% or more accounting) it is placed in quartz boat, it is placed on the microwave heating furnace cavity that microwave frequency is 2450MHz or 915MHz It is interior；(3) open microwave, while blasting oxygen-enriched air, adjust microwave output power, will be levigate after stibnite concentrate from room temperature It is warming up to 850 ~ 1050 DEG C in two stages, keeps the temperature 0.5 ~ 2h;(4) fume recovery, generated flue gas is discharged through microwave reactor gas outlet in heating and roasting process, collects Flue dust；After step (2) keep the temperature 0.5 ~ 2h, microwave is closed, remaining slag is taken out after natural cooling.
- 2. the method for microwave calcining stibnite concentrate volatilization antimony trisulfide according to claim 1, it is characterised in that: the step Suddenly stibnite concentrate tiles in quartz boat with a thickness of 2.5 ~ 5.0cm in (2).
- 3. the method that microwave calcining stibnite concentrate according to claim 1 directly waves antimony trisulfide, which is characterized in that affiliated The rate that oxygen-enriched air is blasted in step (3) is 1.5 ~ 2.0m3/h。
- 4. the method that microwave calcining stibnite concentrate according to claim 1 directly waves antimony trisulfide, which is characterized in that affiliated Microwave power is 0 ~ 20kW, frequency 2450Hz ± 50Hz or 915Hz ± 50Hz in microwave calcining device in step (3).
- 5. the method that microwave calcining stibnite concentrate according to claim 1 directly waves antimony trisulfide, which is characterized in that affiliated The roasting process the first heating stage is rapidly heated with 50 ~ 100 DEG C/min temperature rise rate to 300 ~ 400 DEG C in step (3), heat preservation 30 ~60min；Second temperature rise period was warming up to maturing temperature with 20 ~ 40/min temperature rise rate.
- 6. the method that microwave calcining stibnite concentrate according to claim 1 directly waves antimony trisulfide, which is characterized in that affiliated Roasting process temperature is 850 ~ 1050 DEG C, preferably 950 ~ 1050 DEG C in step (3).
- 7. the method that microwave calcining stibnite concentrate according to claim 1 directly waves antimony trisulfide, which is characterized in that in step Suddenly in (4), after heating obtained flue dust by gas outlet discharge, flue gas is collected with device for recovering powder or cottrell, Obtained antimonial, which can be used for further restoring, obtains metallic antimony.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910626967.3A CN110331279B (en) | 2019-07-12 | 2019-07-12 | Method for directly volatilizing and recycling antimony oxide by roasting antimony sulfide concentrate with microwaves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910626967.3A CN110331279B (en) | 2019-07-12 | 2019-07-12 | Method for directly volatilizing and recycling antimony oxide by roasting antimony sulfide concentrate with microwaves |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110331279A true CN110331279A (en) | 2019-10-15 |
| CN110331279B CN110331279B (en) | 2023-05-23 |
Family
ID=68146470
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910626967.3A Active CN110331279B (en) | 2019-07-12 | 2019-07-12 | Method for directly volatilizing and recycling antimony oxide by roasting antimony sulfide concentrate with microwaves |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110331279B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114480880A (en) * | 2022-02-09 | 2022-05-13 | 云南民族大学 | Method for preparing metallic antimony by directly reducing antimony oxide powder by microwave |
| CN115259221A (en) * | 2022-08-31 | 2022-11-01 | 云南民族大学 | Method for preparing nano antimony trioxide by oxygen-enriched blowing under microwave field |
| CN116873976A (en) * | 2023-07-20 | 2023-10-13 | 益阳生力材料科技股份有限公司 | Preparation method of antimonous oxide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06322455A (en) * | 1993-05-14 | 1994-11-22 | Sumitomo Metal Mining Co Ltd | Production of metallic antimony |
| US20100071510A1 (en) * | 2006-12-18 | 2010-03-25 | Alexander Beckmann | Method for obtaining copper from cupriferous arsenosulphide and/or antimony sulphide ores or ore concentrates |
| WO2012048474A1 (en) * | 2010-10-12 | 2012-04-19 | 深圳市格林美高新技术股份有限公司 | Method for recycling noble metal from electronic waste material and apparatus thereof |
| CN106319199A (en) * | 2016-10-17 | 2017-01-11 | 北京矿冶研究总院 | Pretreatment method of antimony-and arsenic-containing refractory gold ore |
| CN108048655A (en) * | 2017-11-08 | 2018-05-18 | 江苏省冶金设计院有限公司 | A kind of smelting process of antimony metal |
-
2019
- 2019-07-12 CN CN201910626967.3A patent/CN110331279B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06322455A (en) * | 1993-05-14 | 1994-11-22 | Sumitomo Metal Mining Co Ltd | Production of metallic antimony |
| US20100071510A1 (en) * | 2006-12-18 | 2010-03-25 | Alexander Beckmann | Method for obtaining copper from cupriferous arsenosulphide and/or antimony sulphide ores or ore concentrates |
| WO2012048474A1 (en) * | 2010-10-12 | 2012-04-19 | 深圳市格林美高新技术股份有限公司 | Method for recycling noble metal from electronic waste material and apparatus thereof |
| CN106319199A (en) * | 2016-10-17 | 2017-01-11 | 北京矿冶研究总院 | Pretreatment method of antimony-and arsenic-containing refractory gold ore |
| CN108048655A (en) * | 2017-11-08 | 2018-05-18 | 江苏省冶金设计院有限公司 | A kind of smelting process of antimony metal |
Non-Patent Citations (3)
| Title |
|---|
| "一种含锑、砷难处理金矿的预处理方法", 《有色冶金节能》 * |
| "一种含锑、砷难处理金矿的预处理方法", 有色冶金节能 * |
| 谷晋川: "难选冶金矿石微波预处理研究", 《湿法冶金》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114480880A (en) * | 2022-02-09 | 2022-05-13 | 云南民族大学 | Method for preparing metallic antimony by directly reducing antimony oxide powder by microwave |
| CN115259221A (en) * | 2022-08-31 | 2022-11-01 | 云南民族大学 | Method for preparing nano antimony trioxide by oxygen-enriched blowing under microwave field |
| CN115259221B (en) * | 2022-08-31 | 2023-10-31 | 云南民族大学 | Method for preparing nano antimony trioxide by oxygen-enriched blowing under microwave field |
| CN116873976A (en) * | 2023-07-20 | 2023-10-13 | 益阳生力材料科技股份有限公司 | Preparation method of antimonous oxide |
| CN116873976B (en) * | 2023-07-20 | 2024-04-09 | 益阳生力材料科技股份有限公司 | Preparation method of antimonous oxide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110331279B (en) | 2023-05-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110331279A (en) | A kind of microwave calcining stibnite concentrate directly volatilizees the method for recycling antimony oxide | |
| US4612041A (en) | Process for recovering valuable metals from an iron dust containing a higher content of zinc | |
| CN110065969B (en) | Method for preparing pure molybdenum trioxide by microwave roasting molybdenum concentrate pellets | |
| CN111156820A (en) | Antimony concentrate vacuum smelting device | |
| CN109136576A (en) | A kind of method of arsenic-containing smoke dust removing arsenic | |
| JP3513832B2 (en) | Operating method of movable hearth furnace and movable hearth furnace | |
| CN104451171A (en) | Method for removing arsenic from arsenic containing smoke under fluidization | |
| CN109022791A (en) | A method of directly blown low-grade oxidation lead zine ores with fuming furnace | |
| CN109576507B (en) | Process for continuously separating antimony from gold in antimony-gold concentrate | |
| CN217202884U (en) | Device for recovering antimony oxide from medium-low-grade antimony sulfide in microwave blast combined roasting | |
| CN114480880B (en) | Method for preparing metallic antimony by directly reducing antimony oxide powder by microwave | |
| CN106654248A (en) | Preparation method of high-purity manganese monoxide | |
| CN211575857U (en) | Antimony concentrate vacuum smelting device | |
| CN210711689U (en) | Antimony metal extraction system | |
| JPH05132723A (en) | Method for recovering zinc and lead from steelmaking dust | |
| CN106957958A (en) | A kind of method of the low-grade Oxidation Leaching of calcification containing chromic vanadium-titanium ferroferrite vanadium extraction | |
| CN211057202U (en) | Air-blast type extraction system of antimony metal | |
| CN111500813B (en) | Method for utilizing iron and vanadium resources by melting vanadium-titanium metallized pellets in electric furnace | |
| CN113667829A (en) | Zinc-aluminum-iron alloy dezincification process | |
| JP2003147450A (en) | Method of producing rude zinc oxide powder | |
| CN206986249U (en) | A kind of device that manganese-silicon is prepared using poor ferrous manganese ore | |
| JPH06322455A (en) | Production of metallic antimony | |
| CN206828593U (en) | A kind of system for handling zinc leaching residue | |
| CN109609773A (en) | A kind of method of smelting carrying out reduction dearsenification and arsenic removal of volatilizing to high antimony secondary smoke with multilayer air port, Gao Jiaozhu blast furnace | |
| CN211057203U (en) | Well type extraction system for antimony metal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |