CN109371250A - A kind of preparation process extracting metallic sodium from sodium slag by melting displacement method - Google Patents
A kind of preparation process extracting metallic sodium from sodium slag by melting displacement method Download PDFInfo
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- CN109371250A CN109371250A CN201811568220.9A CN201811568220A CN109371250A CN 109371250 A CN109371250 A CN 109371250A CN 201811568220 A CN201811568220 A CN 201811568220A CN 109371250 A CN109371250 A CN 109371250A
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- Prior art keywords
- sodium
- slag
- metallic
- metallic sodium
- calcium
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- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
-
- 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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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- 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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
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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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- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The present invention provides a kind of preparation process for extracting metallic sodium from sodium slag by melting displacement method, and steps are as follows: 1) sodium slag being placed in sodium slag melting tank, heating obtains molten sodium slag under the protection of nitrogen；2) molten sodium slag is incorporated in reaction kettle, while sodium chloride is added carries out displacement reaction and forming metallic sodium and calcium chloride and calcium oxide, obtains the metallic sodium that purity is 96-98%；3) it enters back into treater, is handled through cooling-sedimentation, obtain 99.7% metallic sodium, be transferred to smart sodium storage tank；The residue that cooling-sedimentation generates in treater is added in sodium slag melting tank, is resent to reaction kettle and displacement reaction occurs again；4) 99.7% metallic sodium obtained obtains sodium ingot through casting sodium machine.Production process of the present invention is simple and continuous, production scale is mating and invests that small, risk is small and highly reliable, industrialization easy to accomplish；There is no waste to generate non-environmental-pollution in production process；The high income of metallic sodium is extracted from sodium slag.
Description
Technical field
The invention belongs to metal sodium production fields, and in particular to one kind extracts metallic sodium from sodium slag by melting displacement method
Preparation process.
Background technique
Currently, domestic metal sodium production scale has broken through 100,000 tons/year, main production is sodium chloride, calcium chloride, chlorine
Change barium and is mixed to form electrolytically generated metallic sodium and chlorine after low melting point ternary electrolyte in proportion.From the metallic sodium of electrolytic cell output
In the impurity such as some sodium oxide molybdenas for being formed containing some calcium metals and the air oxidation of metallic sodium contact position, by cooling-sedimentation method
Calcium metal and sodium oxide molybdena therein are isolated from metallic sodium is referred to as sodium slag (sodium content 70-75%, calcium content 20-22%, oxidation
Sodium content 5-8%).The sodium quantity of slag accounts for the 3-4% of electrolytic cell yield, and national metal sodium production device generates 3000 tons or more of sodium every year
Slag but also without the industrial chain of reliable a sodium slag recovery technology and digestibility and utilization sodium slag, this has fully demonstrated current gold
Belong to the imperfection of sodium electrolysis production technique.
However, the production technology of metallic sodium is completely continuously extracted in metal sodium production field from sodium slag not yet.It
Preceding a certain metal sodium production enterprise attempted the production separated using the boiling-point difference of metallic sodium and calcium metal in sodium slag.
Controlling is poor in this method production process, and mainly the generation of metal Sodium vapour and cooling procedure are bad controls, in production process
It is larger also to generate metal Sodium vapour risk, without continuity；Bottom residual metals calcium and sodium oxide molybdena after separation continue to stay
Because the fusing point of calcium metal and sodium oxide molybdena is higher in distillation still, the running temperature of process units is above so solid oxidation
Sodium and calcium metal are bonded on the wall of distillation still, and the normal operation and cleaning tape to distillation still carry out huge difficulty, serious to restrict
The normal operation of process units.And the attribute of the residue mix products is not identified explicitly, it temporarily can only be according to danger
The requirement of waste is handled and is stored.So the distillation subtraction unit of the enterprise belongs to run-stopping status at present.
Summary of the invention
Aiming at the deficiencies in the prior art, the present invention provides one kind and extracts metal from sodium slag by melting displacement method
The preparation process of sodium.
In order to achieve the above object, technical solution of the present invention is as follows:
A kind of preparation process extracting metallic sodium from sodium slag by melting displacement method, includes the following steps:
1) the sodium slag that amount containing sodium is no less than 70% is placed in sodium slag melting tank, 120 DEG C or more is heated under the protection of nitrogen, is obtained
Obtain molten sodium slag；
2) molten sodium slag is incorporated in reaction kettle, while sodium chloride is added, and displacement reaction is carried out at 630-650 DEG C and forms metal
Sodium and calcium chloride and calcium oxide obtain the metallic sodium that purity is 96-98%；
3) metallic sodium of the 96-98% obtained in step 2 enters in treater, handles 0.3-0.5 hours through cooling-sedimentation, obtains
99.7% metallic sodium is transferred to smart sodium storage tank；The residue that cooling-sedimentation generates in treater is added in sodium slag melting tank,
It is resent to reaction kettle and displacement reaction occurs again；Wherein, cooling temperature and sedimentation time of the metallic sodium in treater depend on
The calcium content size in metallic sodium；
4) 99.7% metallic sodium obtained in step 3) obtains sodium ingot through casting sodium machine；
5) reaction generates calcium chloride and micro-oxidation calcium in reaction kettle, into electrolytic cell, uses as electrolysis raw material.
In step 1), in the no less than 70% sodium slag, sodium content 70-75%, calcium content 20-22% by weight,
Calcium oxide content 5-8%.
In step 1), the proportionate relationship of the dosage of time and sodium slag that temperature is kept at 120 DEG C or more are as follows: every 80-
100kg sodium slag heats 2-3 hours.
In step 2), reaction equation is replaced are as follows: Na2O+Ca=2Na+CaO；Ca+2NaCl= CaCl2+2Na.
The utility model has the advantages that (1) production process of the present invention is simple and continuous, production scale is mating and it is small to invest, risk is small and
It is highly reliable, industrialization easy to accomplish；There is no waste to generate non-environmental-pollution in production process；Metallic sodium is extracted from sodium slag
High income can extract 953kg metallic sodium in sodium slag per ton, and metallic sodium yield reaches 95.3%；Reaction product fully recovering to gold
Belonging in natrium electrolytic cell reduces metal sodium production consumption of raw materials as raw material use, and sodium slag utilization rate reaches 100%.
(2) physics and chemistry of raw material needed for activity function and metal natrium electrolytic cell of the present invention using substance every in sodium slag
Can, the calcium metal in sodium slag carries out displacement with sodium oxide molybdena and melting sodium chloride in a kettle and reacts to form metallic sodium and calcium chloride
And calcium oxide.It reacts the metallic sodium generated and passes through cooling down in collector arrangement tedge after collection device is collected,
The separation for the first time of calcium metal and metallic sodium is carried out, the calcium metal separated is fallen into reaction kettle, and the metallic sodium after separation enters
Cooling-sedimentation purity is carried out in treater can reach 99.7% or more, can cast the form export trade of sodium ingot or liquid metal.Treater
The sodium slag reuse that the sodium content of middle generation is 75% is recycled into frit reaction kettle；React the fused calcium chloride and oxygen generated
Change calcium and the ternary electrolysis for adjusting electrolytic cell is added in metal natrium electrolytic cell after natural cooling solidifies after extruding in reaction kettle
Matter ratio.
The present invention is superior to the current sodium slag way of distillation, and the secondary dirt such as hazardous waste will not be generated in entire production process
Easy continuous, sodium slag the utilization rate of dye object, production process reaches 100%, has been fully immersed into existing metallic sodium electrolysis production work
Skill.
Detailed description of the invention
Fig. 1 is preparation process flow block diagram of the invention.
Specific embodiment
The present invention is described below with reference to specific embodiments.It will be appreciated by those skilled in the art that these embodiments are only
For illustrating the present invention, do not limit the scope of the invention in any way.
A kind of preparation process extracting metallic sodium from sodium slag by melting displacement method, as shown in Figure 1, including following step
It is rapid:
1) the sodium slag of amount containing sodium 70% is placed in sodium slag melting tank, 120 DEG C or more is heated under the protection of nitrogen, every 80-
100kg sodium slag heats 2-3 hours, obtains molten sodium slag；
2) molten sodium slag is placed in reaction kettle through supercooling, while sodium chloride is added, and is carried out displacement reaction and is formed metallic sodium and chlorination
Calcium obtains the metallic sodium that purity is 96-98%；Wherein, displacement reaction equation is Ca+2NaCl=CaCl2+2Na；Na2O+ Ca=
2Na+ CaO；
3) metallic sodium of the 96-98% obtained in step 2 enters in treater, handles 0.3-0.5 hours through cooling-sedimentation, obtains
99.7% metallic sodium is transferred to smart sodium storage tank；The residue that cooling-sedimentation generates in treater is recycled, and sodium slag is added to
In melting tank, it is resent to reaction kettle and displacement reaction occurs again, generate metallic sodium and calcium chloride；
4) 99.7% metallic sodium is obtained into sodium ingot through casting sodium machine；
5) calcium chloride and micro-oxidation calcium of generation are reacted in a kettle, are used as metal natrium electrolytic cell raw material.
Claims (3)
1. a kind of preparation process for extracting metallic sodium from sodium slag by melting displacement method, characterized by the following steps:
1) the sodium slag that amount containing sodium is no less than 70% is placed in sodium slag melting tank, 120 DEG C or more is heated under the protection of nitrogen, is obtained
Obtain molten sodium slag；
2) molten sodium slag is incorporated in reaction kettle, while sodium chloride is added, and displacement reaction is carried out at 630-650 DEG C and forms metal
Sodium and calcium chloride and calcium oxide obtain the metallic sodium that purity is 96-98%；
3) metallic sodium of the 96-98% obtained in step 2 enters in treater, handles 0.3-0.5 hours through cooling-sedimentation, obtains
99.7% metallic sodium is transferred to smart sodium storage tank；The residue that cooling-sedimentation generates in treater is added in sodium slag melting tank,
It is resent to reaction kettle and displacement reaction occurs again；Wherein, cooling temperature and sedimentation time of the metallic sodium in treater depend on
The calcium content size in metallic sodium；
4) 99.7% metallic sodium obtained in step 3) obtains sodium ingot through casting sodium machine；
5) reaction generates calcium chloride and micro-oxidation calcium in reaction kettle, into electrolytic cell, uses as electrolysis raw material.
2. the preparation process as described in claim 1 for extracting metallic sodium from sodium slag by melting displacement method, it is characterised in that:
In step 1), in the no less than 70% sodium slag, sodium content 70-75%, calcium content 20-22%, calcium oxide contain by weight
Measure 5-8%.
3. the preparation process as described in claim 1 for extracting metallic sodium from sodium slag by melting displacement method, it is characterised in that:
In step 1), the proportionate relationship of the dosage of time and sodium slag that temperature is kept at 120 DEG C or more are as follows: every 80-100kg sodium slag adds
It is 2-3 hours hot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811568220.9A CN109371250A (en) | 2018-12-21 | 2018-12-21 | A kind of preparation process extracting metallic sodium from sodium slag by melting displacement method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811568220.9A CN109371250A (en) | 2018-12-21 | 2018-12-21 | A kind of preparation process extracting metallic sodium from sodium slag by melting displacement method |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07242956A (en) * | 1994-03-01 | 1995-09-19 | Nippon Kinzoku Kagaku Kk | Treatment of molten alloy and flux holding tool for treatment |
| CN2846436Y (en) * | 2005-08-03 | 2006-12-13 | 宁夏北方巨源液压工贸有限公司 | Metal sodium slag recovery and treating system |
| CN103667708A (en) * | 2013-12-06 | 2014-03-26 | 内蒙古兰太实业股份有限公司 | Process and device for recovering solid sodium metal waste residues |
| CN104294054A (en) * | 2014-01-24 | 2015-01-21 | 内蒙古工业大学 | Method and apparatus for recycling metal sodium and calcium from sodium slag or calcium slag |
| CN105821217A (en) * | 2016-05-13 | 2016-08-03 | 山东默锐科技有限公司 | Separation and purification method for metallic sodium |
| CN107574318A (en) * | 2017-08-08 | 2018-01-12 | 山东默锐科技有限公司 | A kind of sodium slag method for purifying and separating and its equipment for purifying used |
-
2018
- 2018-12-21 CN CN201811568220.9A patent/CN109371250A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07242956A (en) * | 1994-03-01 | 1995-09-19 | Nippon Kinzoku Kagaku Kk | Treatment of molten alloy and flux holding tool for treatment |
| CN2846436Y (en) * | 2005-08-03 | 2006-12-13 | 宁夏北方巨源液压工贸有限公司 | Metal sodium slag recovery and treating system |
| CN103667708A (en) * | 2013-12-06 | 2014-03-26 | 内蒙古兰太实业股份有限公司 | Process and device for recovering solid sodium metal waste residues |
| CN104294054A (en) * | 2014-01-24 | 2015-01-21 | 内蒙古工业大学 | Method and apparatus for recycling metal sodium and calcium from sodium slag or calcium slag |
| CN105821217A (en) * | 2016-05-13 | 2016-08-03 | 山东默锐科技有限公司 | Separation and purification method for metallic sodium |
| CN107574318A (en) * | 2017-08-08 | 2018-01-12 | 山东默锐科技有限公司 | A kind of sodium slag method for purifying and separating and its equipment for purifying used |
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Effective date of registration: 20190930 Address after: Room 309, Lantai dormitory, sandaocandaoxi sanjiefang, Wuda District, wuhilan City, Inner Mongolia 016000 Applicant after: Hai Quan Address before: 221137 Houshizhuang, Qingshan Spring Town, Jiawang District, Xuzhou City, Jiangsu Province Applicant before: Zhao Ying Applicant before: Hai Quan |
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Application publication date: 20190222 |