CN108408747A - A kind of calcination method puies forward the processing method of magnesium slag obtained by lithium - Google Patents
A kind of calcination method puies forward the processing method of magnesium slag obtained by lithium Download PDFInfo
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- CN108408747A CN108408747A CN201810408050.1A CN201810408050A CN108408747A CN 108408747 A CN108408747 A CN 108408747A CN 201810408050 A CN201810408050 A CN 201810408050A CN 108408747 A CN108408747 A CN 108408747A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1045—Oxyacids
- C01B35/1054—Orthoboric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/24—Magnesium carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention discloses the processing method that a kind of calcination method carries magnesium slag obtained by lithium, includes the following steps：(1) magnesium slag is formulated as slurry, and be passed through containing CO2Process gas carry out carburizing reagent, reaction after the completion of be separated by solid-liquid separation, obtain filter residue and heavy magnesium water；(2) heavy magnesium water is pyrolyzed, obtains magnesium carbonate slurry；The first filter cake and filtrate are obtained after filtering, first filter cake is through calcining up to light magnesium oxide；(3) inorganic acid, adjustment pH value to 12 is added in the filtrate after evaporation and concentration, you can boric acid precipitation is precipitated.The processing method provided by the present invention not only solve at present due to do not have rational method disposition caused by " magnesium slag " huddle the problem of putting, also create certain economic benefit, entire technological process is easy to operate, low energy consumption, and boron magnesium separation degree is high, low for equipment requirements, invest small, income height.
Description
Technical field
The present invention relates to chemical industry and environmental technology fields, and in particular to a kind of calcination method carries the processing side of magnesium slag obtained by lithium
Method.
Background technology
Contain the elements such as abundant potassium, lithium, boron, magnesium in China western part salt lake.Wherein lithium is high in the modern times as strategic resources
It is widely used in sci-tech product, price and demand also rapid growth.However, there are Mg/Li ratio height, companions in China western part salt lake
Raw complicated feature carries adjoint after lithium and produces raw a large amount of " waste residue ".Calcination method is wherein used to carry the waste residue of lithium technique generation
The mainly magnesium hydroxide containing boron, referred to as magnesium slag, this magnesium slag are influenced by boron, and use scope is very limited.At present due to
The such magnesium slag effect of prior art processing is bad or cost is too high, therefore manufacturer's only live heap how without any processing
It puts, not only results in waste of resources, but also influence environment.
Invention content
It is an object of the invention to overcome defect described in the prior art, magnesium obtained by lithium is carried to provide a kind of calcination method
The processing method of slag, the processing method not only solve at present that " magnesium slag " is huddled and put caused by not having rational method disposition
Problem also creates certain economic benefit, and entire technological process is easy to operate, and low energy consumption, and boron magnesium separation degree is high, is wanted to equipment
Ask low, investment is small, and income is high.
To achieve the goals above, the present invention provides the following technical solutions as follows：
A kind of calcination method puies forward the processing method of magnesium slag obtained by lithium, includes the following steps：
(1) magnesium slag is formulated as slurry, and be passed through containing CO2Process gas carry out carburizing reagent, reaction complete it is laggard
Row is separated by solid-liquid separation, and obtains filter residue and heavy magnesium water；
(2) heavy magnesium water is pyrolyzed, obtains magnesium carbonate slurry；After filtering the first filter cake and filtrate, described first
Filter cake is through calcining up to light magnesium oxide；
(3) inorganic acid, adjustment pH value to 1-2 is added in the filtrate after evaporation and concentration, you can boric acid precipitation is precipitated.
The equation of step (1) described carburizing reagent is in the present invention：
Mg(OH)2+CO2=MgCO33H2O↓
CaO+2CO2+H2O=Ca (HCO3)2
B2O3+3H2O=2H3BO3
Preferably：The content of magnesium hydroxide is 2wt%-10wt% in step (1) described slurry, in the process gas
CO2Volume content 3%-30%.
Further：The temperature of carburizing reagent described in step (1) is 35 DEG C -90 DEG C, reaction time 5h-10h.
Further：The temperature calcined described in step (2) is 880 DEG C -950 DEG C.
Preferably：First filter cake described in step (2) can obtain basic magnesium carbonate with drying, and the temperature of the drying is
250 DEG C -300 DEG C, the time of the drying is 0.8-1.2h.
Preferably：Filtrate portion described in step (3) is used to prepare slurry with step (1) the magnesium slag, and remainder is used
In continuing to be concentrated by evaporation.
Further：The content of boron, works as B in periodic analysis step (3) described filtrate2O3Content reach 3.5g.L-1-
35g.L-1When, the 5%-30% for taking out filtrate gross mass is evaporated concentration, obtains concentrate.
Further：As B in the concentrate2O3Content reach 42g.L-1-110g.L-1When, inorganic acid tune is added
Whole pH value is heated to 65 DEG C -100 DEG C to 1-2, and boric acid is precipitated.
Preferably：Step (3) adjusts pH value using hydrochloric acid or sulfuric acid.
Compared with prior art, preparation method provided by the invention has the advantages that：
(1) present invention realizes the utilization of waste first, by what is stacked due to the higher separating difficulty of presence throughout the year
Boracic magnesium slag has carried out reasonable processing, reduces the generation of solid waste；Meanwhile using this method can obtain two or more purity compared with
High industrial products improve the economic benefit of product；In addition to this, method provided by the present invention, simple for process, operation is held
Easily, and relatively low to equipment requirement, it is only necessary to (to be both needed to have high voltage performance, highly-acidproof without complete outfit using conventional equipment
Can be equal) separation of boron magnesium in boracic magnesium slag can be realized；
(2) carburizing reagent is the process of boron magnesium separation, and the quality of carburizing reagent will directly affect the purity of magnesium oxide product
With the rate of recovery of magnesia in raw material, the content of the magnesium hydroxide in slurry is adjusted to 1wt%-2wt% by the present invention first, so
It is passed through the CO of middle volume content >=30% afterwards2, at 15 DEG C -35 DEG C, apply the pressure of 0.08Mpa-0.55Mpa, make magnesium slag with
CO21.5h-3h is reacted, to efficiently separate out magnesium ion, also makes carbonizatin method in terms of the raw material for producing magnesium carbonate, magnesia
Further expansion is done.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
The process flow diagram that Fig. 1 is provided by the embodiment of the present invention.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
The every other embodiment that personnel are obtained without making creative work, shall fall within the protection scope of the present invention.
In addition, technical characteristic involved in invention described below different embodiments is as long as they do not conflict with each other
It can be combined with each other.
It should be noted that：Magnesium slag used in the following embodiments of the present invention is limited by the lithium industry development of Qinghai CITIC Guoan
Company carries generated filter residue after lithium technique using calcination method, and ingredient lists are as follows：
Embodiment 1
As shown in Figure 1, the present invention provides the processing method that a kind of calcination method carries magnesium slag obtained by lithium, include the following steps：
(1) filtrate obtained by 3000 kilograms of 1 steps of water embodiment (2) is added in material-compound tank, it is public to be then added 220
Jin magnesium slag, after stirring evenly, the content for obtaining magnesium hydroxide is the slurry of 2wt%；Then enter dioxide containing gas into slurry
Under normal pressure, carburizing reagent 9h under conditions of 15 DEG C, the wherein process gas come from combustion of fossil fuel to the process gas of body
Gas it is purified after gained, the volume content of carbon dioxide is 10%；Calcium oxide and boron oxide respectively by carburizing reagent with
Carbon dioxide knot is combined into solution, after reaction, is filtered and is washed with centrifuge, is separated by solid-liquid separation while being removed to carry out
It is attached to the sulfate radical and chloride ion impurities of carbonic acid magnesium surface, obtains filter residue and heavy magnesium water；
(2) heavy magnesium water is pyrolyzed, obtains magnesium carbonate slurry, the first filter cake and filtrate are obtained after filtering, the first filter cake is in temperature
To get magnesia, analysis show that magnesia purity is 96.5% to Calcination: Calcination, and accumulation is close within 3 hours in the rotary kiln that degree is 950 DEG C
Degree is 0.20g.ml-1, reach II class high-class product standard of technical grade light magnesium oxide；
(3) obtained by periodic analysis step (2) in filtrate boron content, work as B2O3Content reach 3.5g.L-1When, take out filter
The 5% of liquid gross mass is evaporated concentration, obtains concentrate, as B in the concentrate2O3Content reach 52g.L-1When, it is added
Sulfuric acid adjusts pH value to 2, is then aged 1 hour and is filtered, and the solid of filtering gained is dried at a temperature of 80 DEG C, is obtained
White boric acid powder analyzes to obtain boric acid content 99.5%, reaches technical grade boric acid Grade A standard.
Embodiment 2
As shown in Figure 1, the present invention provides the processing method that a kind of calcination method carries magnesium slag obtained by lithium, include the following steps：
(1) filtrate in 2840 kilograms of embodiments 1 obtained by step (2) is added in material-compound tank, 160 kilograms of magnesium are then added
In addition slag supplies 3000 kilograms, after stirring evenly with a water, the content for obtaining magnesium hydroxide is the slurry of 6wt%；Then to
Enter the process gas of carbon dioxide containing gas in slurry under normal pressure, carburizing reagent 10h under conditions of 20 DEG C, the wherein process gas
Body comes from the gas obtained by the first filter cake of calcining of embodiment 1, and the volume content of carbon dioxide is 3%；Calcium oxide and boron oxide
Be combined into solution by carburizing reagent and carbon dioxide knot respectively, after reaction, filtered and washed with centrifuge, with into
Row is separated by solid-liquid separation while removing the sulfate radical and chloride ion impurities that are attached to carbonic acid magnesium surface, obtains filter residue and heavy magnesium water；
(2) heavy magnesium water is pyrolyzed, obtains magnesium carbonate slurry, the first filter cake and filtrate are obtained after filtering, the first filter cake is in temperature
To get magnesia, analysis show that magnesia purity is 96.9% to the tunnel oven Calcination: Calcination that degree is 880 DEG C, bulk density within 5 hours
For 0.19g.ml-1, reach II class high-class product standard of technical grade light magnesium oxide.
(3) obtained by periodic analysis step (2) in filtrate boron content, work as B2O3Content reach 5.2g.L-1When, take out filter
The 18% of liquid gross mass is evaporated concentration, obtains concentrate, as B in the concentrate2O3Content reach 62g.L-1When, it is added
Sulfuric acid adjusts pH value to 1, is then aged 1 hour and is filtered, and the solid of filtering gained is dried at a temperature of 100 DEG C, is obtained
To white boric acid powder, boric acid content 99.6% is analyzed to obtain, reaches technical grade boric acid Grade A standard.
Embodiment 3
As shown in Figure 1, the present invention provides the processing method that a kind of calcination method carries magnesium slag obtained by lithium, include the following steps：
(1) filtrate obtained by 2820 kilograms of 2 steps of embodiment (2) is added in material-compound tank, 180 kilograms of magnesium slags are added, so
Material is supplied 3000 kilograms, after stirring evenly with a water again afterwards, the content for obtaining magnesium hydroxide is the slurry of 10wt%；To
Enter the process gas of carbon dioxide containing gas in slurry under normal pressure, carburizing reagent 5h under conditions of 20 DEG C, the wherein process gas
Body comes from the purified rear gained of gas of combustion of fossil fuel, and the volume content of carbon dioxide is 30%；Calcium oxide and oxidation
Boron is combined by carburizing reagent and carbon dioxide knot in solution respectively, after reaction, is filtered and is washed with centrifuge, with
It carries out being separated by solid-liquid separation while removing the sulfate radical and chloride ion impurities that are attached to carbonic acid magnesium surface, obtains filter residue and heavy magnesium water；
(2) heavy magnesium water is pyrolyzed, obtains magnesium carbonate slurry, the first filter cake and filtrate are obtained after filtering, the first filter cake is in temperature
To get magnesia, analysis show that magnesia purity is 95.8% to Calcination: Calcination, and accumulation is close within 3 hours in the shuttle kiln that degree is 950 DEG C
Degree is 0.22g.ml-1, reach II class high-class product standard of technical grade light magnesium oxide；
(3) obtained by periodic analysis step (2) in filtrate boron content, work as B2O3Content reach 9.1g.L-1When, take out filter
The 30% of liquid gross mass is evaporated concentration, obtains concentrate, as B in the concentrate2O3Content reach 92g.L-1When, it is added
Hydrochloric acid adjusts pH value to 1.4, is then aged 1 hour and is filtered, and the solid of filtering gained is dried at a temperature of 100 DEG C,
White boric acid powder is obtained, boric acid content 99.5% is analyzed to obtain, reaches technical grade boric acid Grade A standard.
Embodiment 4
As shown in Figure 1, the present invention provides the processing method that a kind of calcination method carries magnesium slag obtained by lithium, include the following steps：
(1) water is added in material-compound tank, magnesium slag is then added, after stirring evenly, the content for obtaining magnesium hydroxide is
The slurry of 2wt%；Then the process gas for entering carbon dioxide containing gas into slurry under normal pressure, is carbonized instead under conditions of 15 DEG C
5h, the wherein process gas is answered to come from the purified rear gained of gas of combustion of fossil fuel, the volume content of carbon dioxide is
3%；Calcium oxide and boron oxide are combined by carburizing reagent and carbon dioxide knot in solution respectively, after reaction, with from
Scheming is filtered and is washed, and is attached to the sulfate radical and chloride ion impurities of carbonic acid magnesium surface be separated by solid-liquid separation while remove, is obtained
Filter residue and heavy magnesium water；
(2) heavy magnesium water is pyrolyzed, obtains magnesium carbonate slurry, the first filter cake and filtrate are obtained after filtering, the first filter cake is in temperature
Degree obtains basic magnesium carbonate to dry 0.8h in 250 DEG C of static drying chamber.
(3) obtained by periodic analysis step (2) in filtrate boron content, work as B2O3Content reach 14g.L-1When, take out filter
The 5% of liquid gross mass is evaporated concentration, obtains concentrate, as B in the concentrate2O3Content reach 42g.L-1When, it is added
Sulfuric acid adjusts pH value to 1, is then aged 1 hour and is filtered, and the solid of filtering gained is dried at a temperature of 65 DEG C, is obtained
White boric acid powder analyzes to obtain boric acid content 99.3%, reaches technical grade boric acid Grade A standard.
Embodiment 5
As shown in Figure 1, the present invention provides the processing method that a kind of calcination method carries magnesium slag obtained by lithium, include the following steps：
(1) filtrate obtained by 4 step of embodiment (2) is added in material-compound tank, magnesium slag is then added, after stirring evenly, obtains
The slurry that content to magnesium hydroxide is 10wt%；Then enter the process gas of carbon dioxide containing gas into slurry in normal pressure
Under, carburizing reagent 10h under conditions of 35 DEG C, the wherein process gas come from the purified rear institute of gas of combustion of fossil fuel
, the volume content of carbon dioxide is 30%；Calcium oxide and boron oxide are combined by carburizing reagent with carbon dioxide respectively goes forward side by side
Enter in solution, after reaction, filtered and washed with centrifuge, carbonic acid magnesium surface is attached to be separated by solid-liquid separation while remove
Sulfate radical and chloride ion impurities, obtain filter residue and heavy magnesium water；
(2) heavy magnesium water is pyrolyzed, obtains magnesium carbonate slurry, the first filter cake and filtrate are obtained after filtering, the first filter cake is in temperature
Degree obtains basic magnesium carbonate to dry 1.2h in 300 DEG C of flash dryer；
(3) obtained by periodic analysis step (2) in filtrate boron content, work as B2O3Content reach 35g.L-1When, take out filter
The 30% of liquid gross mass is evaporated concentration, obtains concentrate, as B in the concentrate2O3Content reach 110g.L-1When, add
Enter hydrochloric acid and adjust pH value to 2, is then aged 1 hour and is filtered, the solid of filtering gained is dried at a temperature of 70 DEG C, is obtained
To white boric acid powder, boric acid content 99.6% is analyzed to obtain, reaches technical grade boric acid Grade A standard.
The foregoing is merely the specific implementation modes of the present invention, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, all answer by the change or replacement that can be readily occurred in
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be with the scope of the claims
It is accurate.
Claims (9)
1. a kind of calcination method puies forward the processing method of magnesium slag obtained by lithium, which is characterized in that include the following steps：
(1) magnesium slag is formulated as slurry, and be passed through containing CO2Process gas carry out carburizing reagent, reaction after the completion of carry out solid-liquid
Separation, obtains filter residue and heavy magnesium water；
(2) heavy magnesium water is pyrolyzed, obtains magnesium carbonate slurry；The first filter cake and filtrate, first filter cake are obtained after filtering
Through calcining up to light magnesium oxide；
(3) inorganic acid, adjustment pH value to 1-2 is added in the filtrate after evaporation and concentration, you can boric acid precipitation is precipitated.
2. processing method according to claim 1, which is characterized in that the content of magnesium hydroxide in step (1) described slurry
For 2wt%-10wt%, CO in the process gas2Volume content 3%-30%.
3. processing method according to claim 2, which is characterized in that the temperature of carburizing reagent described in step (1) is 35
DEG C -90 DEG C, reaction time 5h-10h.
4. processing method according to claim 1, which is characterized in that the temperature calcined described in step (2) be 880 DEG C-
950℃。
5. processing method according to claim 1, which is characterized in that the first filter cake described in step (2) can also be through drying
Basic magnesium carbonate is done to obtain, the temperature of the drying is 250 DEG C -300 DEG C, and the time of the drying is 0.8-1.2h.
6. processing method according to claim 1, which is characterized in that filtrate portion described in step (3) is used for and step
(1) the magnesium slag prepares slurry, and remainder is for continuing to be concentrated by evaporation.
7. processing method according to claim 6, which is characterized in that boron contains in periodic analysis step (3) described filtrate
Amount, works as B2O3Content reach 3.5g.L-1-35g.L-1When, the 5%-30% for taking out filtrate gross mass is evaporated concentration, obtains dense
Contracting liquid.
8. processing method according to claim 7, which is characterized in that as B in the concentrate2O3Content reach
42g.L-1-110g.L-1When, inorganic acid is added and adjusts pH value to 1-2, and is heated to 65 DEG C -100 DEG C, boric acid is precipitated.
9. processing method according to claim 1, which is characterized in that step (3) adjusts pH value using hydrochloric acid or sulfuric acid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112645368A (en) * | 2020-12-25 | 2021-04-13 | 河北工程大学 | Resource utilization method of waste magnesium oxide catalyst |
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|---|---|---|---|---|
| CN102491379A (en) * | 2011-12-10 | 2012-06-13 | 中南大学 | Method for preparing high-purity magnesium oxide with high boron salt lake brine |
| CN103754902A (en) * | 2013-12-30 | 2014-04-30 | 辽宁首钢硼铁有限责任公司 | Method for preparing light magnesium carbonate and coproducing borax or boric acid by using low-grade magnesium-boron-containing concentrate |
| CN105883864A (en) * | 2014-09-16 | 2016-08-24 | 常德云港生物科技有限公司 | Method for producing basic magnesium carbonate from boron mud waste material |
| CN106477593A (en) * | 2016-10-12 | 2017-03-08 | 泰誉威（天津）新材料科技有限公司 | A kind of method that boric acid is prepared as raw material with raphite ore deposit |
-
2018
- 2018-05-02 CN CN201810408050.1A patent/CN108408747A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491379A (en) * | 2011-12-10 | 2012-06-13 | 中南大学 | Method for preparing high-purity magnesium oxide with high boron salt lake brine |
| CN103754902A (en) * | 2013-12-30 | 2014-04-30 | 辽宁首钢硼铁有限责任公司 | Method for preparing light magnesium carbonate and coproducing borax or boric acid by using low-grade magnesium-boron-containing concentrate |
| CN105883864A (en) * | 2014-09-16 | 2016-08-24 | 常德云港生物科技有限公司 | Method for producing basic magnesium carbonate from boron mud waste material |
| CN106477593A (en) * | 2016-10-12 | 2017-03-08 | 泰誉威（天津）新材料科技有限公司 | A kind of method that boric acid is prepared as raw material with raphite ore deposit |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112645368A (en) * | 2020-12-25 | 2021-04-13 | 河北工程大学 | Resource utilization method of waste magnesium oxide catalyst |
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