CN109735701A - A kind of method that microwave decomposition sulfide prepares metal and sulphur - Google Patents
A kind of method that microwave decomposition sulfide prepares metal and sulphur Download PDFInfo
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- CN109735701A CN109735701A CN201910093011.1A CN201910093011A CN109735701A CN 109735701 A CN109735701 A CN 109735701A CN 201910093011 A CN201910093011 A CN 201910093011A CN 109735701 A CN109735701 A CN 109735701A
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Abstract
The present invention relates to a kind of methods that microwave decomposition sulfide prepares metal and sulphur, belong to metal metallurgy smelting and field of material preparation.The method utilizes microwave decomposition technology, it is optimized by the technological parameter to load microwave, it decomposes sulfide sufficiently during with microwave interactive, to obtain the metal simple-substance and sulphur of higher degree, and avoids the generation of pernicious gas in decomposable process.The method of the invention has many advantages, such as simple process, high production efficiency, environmentally protective and at low cost, has broad application prospects in metal metallurgy smelting field.
Description
Technical field
The present invention relates to metal metallurgy smelting and field of material preparation, and in particular to a kind of to prepare sulphur using microwave decomposition sulfide
The method of sulphur and non-ferrous metal.
Background technique
With the development of metallurgical technology, metal (Mo, In, Ga, Pb, Mn, Zn, Ag, Ni, Pt, Fe in sulphide ore are extracted at present
Deng) main technique be pyrogenic process roast and Wet Decomposition.Both methods converts metal oxide (MeS for sulphide ore firstx
+O2→MeOx+SO2), recycle intermediate products further purify be metal or metallic compound.It is inevitable in pyrogenic process roasting
The sulfur dioxide gas for generating pollution environment, with the continuous improvement of environmental requirement, although sulphur dioxide flue gas acid preparing gradually at
For the main source of sulfuric acid, but the high investment and low price of sulfuric acid preparation, drastically influence the economic effect of non-ferrous metallurgical enterprise
Benefit；Soda acid and ammonia etc. can be generally used in hydrometallurgy overshoot, and therefore forms the secondary pollutions such as waste water, waste residue, exhaust gas.
Therefore, under the pressure of under the dual-pressure of environmental requirement and economic benefit, novel green metallurgical technique starts by numerous researchers
Concern.
The interaction of High-Power Microwave and material have fast heating speed, homogeneous heating, be conducive to decompose the steam generated it is fast
It the features such as speed diffusion, has been developed that and applies in fields such as industrial production, scientific research, biomedicines.But it is with High-Power Microwave
Heat source directly decomposes sulfide there is no relevant report to obtain the research of sulphur and metal simple-substance at present.
Summary of the invention
For deficiency present in existing sulfide conventional metallurgical technique and technology, the purpose of the present invention is to provide one kind
The method that microwave decomposition sulfide prepares metal and sulphur, this method is with energy-efficient, environmentally protective, process is short, at low cost
The advantages that, and prepared sulphur and metal purity is high, has broad application prospects.
A kind of method that microwave decomposition sulfide prepares metal and sulphur, the method comprises the following steps:
Step 1. is evenly laid out in crucible by sulfide powders, and the thickness that tiles is not less than 5mm, then places crucible
In microwave oven, the air inlet of microwave oven and the gas source of protective gas are connected, the gas outlet of microwave oven and gas
The connection of body collection device；
Step 2. set microwave oven load microwave microwave power as 1000W~1600W and heating temperature be 500
DEG C~1100 DEG C, and being filled with flow to microwave heating furnace interior is the protective gas that 2L/min~20L/min is not involved in reaction；So
After start to load microwave, reach heat preservation after heating temperature and be no less than 10min, then stop heating and furnace cooling, finally stop logical
Enter protective gas, the decomposition product in crucible is the mixture of metal and sulphur, and the product collected in gas collector is sulphur
Sulphur.
Further, the crucible preferably uses mullite crucible.
Further, 20 μm of the purity > 80% of the sulfide, diameter of particle <；The preferred MoS of sulfide2、In2S3、
Ga2S3、PbS、MnS、ZnS、Ag2S、NiS、PtS2Or FeS2。
Further, the protective gas is nitrogen or inert gas.
Further, after the heating temperature for reaching setting, the preferred 10min~30min of soaking time.
Further, the preferred 915MHz~5800MHz of the frequency of the microwave oven.
The utility model has the advantages that
The method of the invention utilizes microwave decomposition technology, by the process parameter optimizing to load microwave, makes sulfide
It is sufficiently decomposed during with microwave interactive, and avoids the generation of pernicious gas.Using the method for the invention preparation
Sulphur and metal purity are high, and the mixture of the two is easily isolated.The method has simple process, high production efficiency, green
The advantages that colour circle is protected and is at low cost, has broad application prospects in metal metallurgy smelting field.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of molybdenum prepared in embodiment 1.
Fig. 2 is the energy spectrum analysis figure of Fig. 1.
Specific embodiment
The invention will be further elaborated combined with specific embodiments below.
See Table 1 for details for reagent used in following embodiment and instrument.
Table 1
The frequency of microwave oven used is 2450MHz in following embodiment.
Embodiment 1
(1) the molybdenum disulfide powder that 5g average grain diameter is 10 μm is equably laid in mullite crucible, the thickness of tiling
Degree is about 5mm；Then, mullite crucible is placed in the burner hearth middle position of microwave oven, the air inlet of microwave oven with
The connection of Ar gas source, the gas outlet of microwave oven is connect with gas collector；
(2) set microwave oven load microwave microwave power as 1000W and heating temperature be 500 DEG C, close it is micro-
The fire door of Wave heating furnace is simultaneously filled with the Ar progress atmosphere protection that flow is 2L/min to microwave heating furnace interior；Then start to load
Microwave keeps the temperature 15min after reaching heating temperature, then stops heating and furnace cooling, stops being passed through Ar after cooling again, in crucible
Decomposition product be sulphur and molybdenum mixture, also collection part sulphur in gas collector.
It is clear that the sulphur simple substance of yellow from the decomposition product of crucible, exists simultaneously with glossiness molybdenum gold
Belong to, this absolutely proves the decomposition that can be realized sulfide using microwave decomposition technology, reaches desulfurization effect, realizes green metallurgical.
From figure 1 it appears that the institutional framework of prepared molybdenum is in lath-shaped；By carrying out power spectrum point to Fig. 1
Analysis is it is found that remaining is Mo element (as shown in Figure 2), and S element is not detected other than detecting micro impurity element.
Therefore, molybdenum disulfide can decompose to obtain purity higher Mo metal simple-substance under the conditions of microwave action.
Embodiment 2
(1) zinc sulphide powder that 5g average grain diameter is 15 μm is equably laid in mullite crucible, the thickness of tiling
About 6mm；Then, mullite crucible is placed in the burner hearth middle position of microwave oven, the air inlet and Ar of microwave oven
Gas source connection, the gas outlet of microwave oven is connect with gas collector；
(2) set microwave oven load microwave microwave power as 1600W and heating temperature be 1100 DEG C, close it is micro-
The fire door of Wave heating furnace is simultaneously filled with the Ar progress atmosphere protection that flow is 20L/min to microwave heating furnace interior；Then start to add
Microwave is carried, keeps the temperature 15min after reaching heating temperature, then stops heating and furnace cooling, stops being passed through Ar, crucible again after cooling
Interior decomposition product is the mixture of sulphur and zinc metal, also being capable of collection part sulphur in gas collector.
Energy spectrum analysis is carried out to prepared zinc metal, other than detecting micro impurity element, remaining is Zn member
Element, and S element is not detected, this, which is absolutely proved, can be realized the decomposition of zinc sulphide using microwave decomposition technology and is obtaining
The higher Zn metal simple-substance of purity.
Embodiment 3
(1) the vulcanization aluminium powder that 5g average grain diameter is 15 μm is equably laid in mullite crucible, the thickness of tiling
About 5mm；Then, mullite crucible is placed in the burner hearth middle position of microwave oven, the air inlet and Ar of microwave oven
Gas source connection, the gas outlet of microwave oven is connect with gas collector；
(2) set microwave oven load microwave microwave power as 1200W and heating temperature be 700 DEG C, close it is micro-
The fire door of Wave heating furnace is simultaneously filled with the Ar progress atmosphere protection that flow is 10L/min to microwave heating furnace interior；Then start to add
Microwave is carried, keeps the temperature 25min after reaching heating temperature, then stops heating and furnace cooling, stops being passed through Ar, crucible again after cooling
Interior decomposition product is the mixture of sulphur and silver metal, also being capable of collection part sulphur in gas collector.
Energy spectrum analysis is carried out to prepared silver metal, other than detecting micro impurity element, remaining is Ag member
Element, and S element is not detected, this, which is absolutely proved, can be realized the decomposition of silver sulfide using microwave decomposition technology and is obtaining
The higher Ag metal simple-substance of purity.
Embodiment 4
(1) the manganese sulfide powder that 5g average grain diameter is 20 μm is equably laid in mullite crucible, the thickness of tiling
About 7mm；Then, mullite crucible is placed in the burner hearth middle position of microwave oven, the air inlet and Ar of microwave oven
Gas source connection, the gas outlet of microwave oven is connect with gas collector；
(2) set microwave oven load microwave microwave power as 1400W and heating temperature be 900 DEG C, close it is micro-
The fire door of Wave heating furnace is simultaneously filled with the Ar progress atmosphere protection that flow is 15L/min to microwave heating furnace interior；Then start to add
Microwave is carried, keeps the temperature 20min after reaching heating temperature, then stops heating and furnace cooling, stops being passed through Ar, crucible again after cooling
Interior decomposition product is the mixture of sulphur and manganese Metal, also being capable of collection part sulphur in gas collector.
Energy spectrum analysis is carried out to prepared manganese Metal, other than detecting micro impurity element, remaining is Mn member
Element, and S element is not detected, this, which is absolutely proved, can be realized the decomposition of manganese sulfide using microwave decomposition technology and is obtaining
The higher Mn metal simple-substance of purity.
The present invention includes but is not limited to above embodiments, it is all carried out under the spirit and principles in the present invention it is any etc.
With replacement or local improvement, all will be regarded as within protection scope of the present invention.
Claims (7)
1. a kind of method that microwave decomposition sulfide prepares metal and sulphur, it is characterised in that: steps are as follows for the method,
Step 1. is evenly laid out in crucible by sulfide powders, and the thickness that tiles is not less than 5mm, is then placed on crucible micro-
In Wave heating furnace, the air inlet of microwave oven and the gas source of protective gas are connected, and the gas outlet of microwave oven and gas are received
Acquisition means connection；
Step 2. set the microwave power of microwave oven load microwave as 1000W~1600W and heating temperature be 500 DEG C~
1100 DEG C, and being filled with flow to microwave heating furnace interior is the protective gas that 2L/min~20L/min is not involved in reaction；Then it opens
Begin load microwave, and heat preservation is no less than 10min after reaching heating temperature, then stops heating and furnace cooling, finally stops being passed through guarantor
Gas is protected, the decomposition product in crucible is the mixture of metal and sulphur, and the product collected in gas collector is sulphur.
2. the method that microwave decomposition sulfide according to claim 1 prepares metal and sulphur, it is characterised in that: the sulphur
Compound is MoS2、In2S3、Ga2S3、PbS、MnS、ZnS、Ag2S、NiS、PtS2Or FeS2。
3. the method that microwave decomposition sulfide according to claim 1 or 2 prepares metal and sulphur, it is characterised in that: institute
State the purity > 80% of sulfide, 20 μm of diameter of particle <.
4. the method that microwave decomposition sulfide according to claim 1 or 2 prepares metal and sulphur, it is characterised in that: institute
Crucible is stated using mullite crucible.
5. the method that microwave decomposition sulfide according to claim 1 or 2 prepares metal and sulphur, it is characterised in that: reach
To after the heating temperature of setting, soaking time is 10min~30min.
6. the method that microwave decomposition sulfide according to claim 1 or 2 prepares metal and sulphur, it is characterised in that: institute
Stating protective gas is nitrogen or inert gas.
7. the method that microwave decomposition sulfide according to claim 1 or 2 prepares metal and sulphur, it is characterised in that: institute
The frequency for stating microwave oven is 915MHz~5800MHz.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041224A (en) * | 2019-12-03 | 2020-04-21 | 中南大学 | Method for directly preparing metallic lead by galena |
| CN112427648A (en) * | 2020-11-30 | 2021-03-02 | 长安大学 | Preparation method and preparation device of metal molybdenum powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202347065U (en) * | 2011-11-01 | 2012-07-25 | 长沙隆泰微波热工有限公司 | Molybdenum disulfide microwave desulfuration device |
| CN103657370A (en) * | 2012-09-07 | 2014-03-26 | 韩国能量技术研究院 | Device and method for removing hydrogen sulphide and carbonyl sulphide by virtue of microwave plasmas |
| CN104524934A (en) * | 2014-12-29 | 2015-04-22 | 湘潭大学 | Method for producing hydrogen and sulfur by using microwave catalytic decomposition of hydrogen sulfide |
| CN105463184A (en) * | 2015-12-09 | 2016-04-06 | 西安建筑科技大学 | Mining pretreatment equipment |
| 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 |
-
2019
- 2019-01-30 CN CN201910093011.1A patent/CN109735701A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202347065U (en) * | 2011-11-01 | 2012-07-25 | 长沙隆泰微波热工有限公司 | Molybdenum disulfide microwave desulfuration device |
| CN103657370A (en) * | 2012-09-07 | 2014-03-26 | 韩国能量技术研究院 | Device and method for removing hydrogen sulphide and carbonyl sulphide by virtue of microwave plasmas |
| CN104524934A (en) * | 2014-12-29 | 2015-04-22 | 湘潭大学 | Method for producing hydrogen and sulfur by using microwave catalytic decomposition of hydrogen sulfide |
| CN105463184A (en) * | 2015-12-09 | 2016-04-06 | 西安建筑科技大学 | Mining pretreatment equipment |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041224A (en) * | 2019-12-03 | 2020-04-21 | 中南大学 | Method for directly preparing metallic lead by galena |
| CN112427648A (en) * | 2020-11-30 | 2021-03-02 | 长安大学 | Preparation method and preparation device of metal molybdenum powder |
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