CN106564916A - Preparation method for preparing high-quality chromium slag filler and recovering sodium carbonate by using chromium slag - Google Patents
Preparation method for preparing high-quality chromium slag filler and recovering sodium carbonate by using chromium slag Download PDFInfo
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- CN106564916A CN106564916A CN201611023887.1A CN201611023887A CN106564916A CN 106564916 A CN106564916 A CN 106564916A CN 201611023887 A CN201611023887 A CN 201611023887A CN 106564916 A CN106564916 A CN 106564916A
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- chromium slag
- sodium carbonate
- filler
- chromium
- quality
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0045—Mixed oxides or hydroxides containing aluminium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The invention discloses a preparation method for preparing high-quality chromium slag filler and recovering sodium carbonate by using chromium slag. The method comprises the steps: carrying out ball-milling on dried calcium-free chromium slag, and then, carrying out screening until the grain size is 150 to 200 meshes; adding deionized water and the calcium-free chromium slag into a hydrothermal autoclave according to the liquid-to-solid ratio of (3: 1) to (5: 1), introducing gas CO2 into the hydrothermal autoclave, and carrying out a reaction for 12 to 24 hours; stopping introducing the gas CO2 after the reaction ends, carrying out pressure relief, then, subjecting the material to filtrating and washing, and collecting filtrated residues and filtrate; heating the temperature of the filtrate to 90 DEG C to 100 DEG C, carrying out evaporative crystallization, cooling the temperature of the solution to 30 DEG C to 40 DEG C when the concentration of Na<+> in the solution is higher than 190g/L, and baking white solids, which are obtained through filtration, at the temperature of 150 DEG C, thereby obtaining sodium carbonate solid; and baking the filtrated residue in a slag dryer, thereby obtaining the high-melting-point spinel chromium slag filler. According to the method, phases such as sodium-aluminum silicate and sodium-aluminum-containing low-melting-point amorphous sticking substances in the chromium slag can be dissociated, and elemental sodium is recovered in the form of sodium carbonate; and attachments are removed from chromium slag granules, so that the obtaining of the high-quality filler through sorting coarse chromium slag granules is facilitated.
Description
Technical field
The invention belongs to the cycling and reutilization technical field of the cleaning treatment of chromium slag and resource, and in particular to one kind utilizes chromium
Slag prepares high-quality chromium slag filler and reclaims the preparation method of sodium carbonate.
Background technology
Chromium and chromium compound are important Inorganic Chemicals, in plating, tanning, printing and dyeing, medicine, pigment, catalyst, oxidation
The aspect such as agent and metal inhibitor has a wide range of applications, and is related to the range of goods of national economy 15%.
The current main production process of chromic salts is chromite calcium-free roasting method, often produces one ton of chromic salts product and produces 0.6～08
The chromium slag of ton, has chromium content height (Cr in non-calcium chromium slags2O3, 8～18%) the characteristics of, in order to avoid chromium slag contaminated (Cr6+It is acute
Poison) and improve resource utilization, chromium slag it is general it is sorted after obtain thick slag and return roasting as filler being extracted again, but
Because chromium slag backfills the accumulation of the element such as Na, Al, Si in roasting repeatedly, formed some sodium aluminum silicates and the eutectic containing sodium aluminium without
Amorphous substance, these things not only easily form segregation liquid phase when roasting is returned and cause to tie kiln, and the spinel particle in slag
Between bond, it is impossible to the Spinel in slag is mutually efficiently separated with sodium aluminum silicate when chromium slag is sorted, reduce chromium slag filler
Quality, be unfavorable for stove direct motion.
The content of the invention
In view of this, present invention is primarily targeted at provide one kind prepares high-quality chromium slag filler and recovery using chromium slag
The preparation method of sodium carbonate.
To reach above-mentioned purpose, the technical scheme is that what is be achieved in that：
Embodiment of the present invention people provides a kind of utilization chromium slag and prepares high-quality chromium slag filler and reclaim the preparation side of sodium carbonate
Method, the method is realized by following steps：
Step 1：Ball milling is sieved：Dry non-calcium chromium slags are put in ball grinder, ball milling, ball milling are carried out by planetary ball mill
After the completion of be sized to 150～200 mesh；
Step 2：Carburizing reagent：With liquid-solid ratio 3:1～5:1 adds the non-calcium chromium slags after deionized water and step 1 ball milling
To in hydro-thermal autoclave, into the hydro-thermal autoclave CO is passed through2Gas, 12～24h of reaction time；
Step 3：It is separated by filtration：After reaction terminates, stopping is passed through CO2Gas, after the hydro-thermal autoclave release, will be described
Material in hydro-thermal autoclave is filtered, washed, while collecting filter residue and filtrate；
Step 4：Evaporative crystallization：Step 3 gained filtrate is heated to into 90～100 DEG C and is evaporated crystallization, treat Na in solution+
When concentration is more than 190g/L, solution is cooled to into 30～40 DEG C, is filtered, the white solid being filtrated to get at 150 DEG C
Carry out drying sodium carbonate solid；
Step 5：Filter residue is dried：Step 3 gained filter residue is put in slag drying machine and is dried, Gao Rong is obtained final product after drying
Point spinelle chromium slag filler.
In such scheme, in the step 2, ratio of grinding media to material 6 is chosen:1～9:1, the rotating speed of ball mill is 300～400r/
min。
In such scheme, in the step 3, CO is passed through2The pressure of gas is 0.2～1MPa, the hydro-thermal autoclave
Temperature is 100～150 DEG C, and mixing speed is 200～500r/min.
In such scheme, the step 5 also includes：The trickle powder of chromium slag is collected by drying machine bagroom.
In such scheme, also include before the step 1：The chromium slag for weighing is dried into 10-14h at 100～120 DEG C,
Obtain dry non-calcium chromium slags.
Compared with prior art, beneficial effects of the present invention：
The present invention can be in chromium slag sodium aluminum silicate and the amorphous adhesive of the eutectic containing sodium aluminium dissociated, sodium element
Reclaimed in the form of sodium carbonate, while the attachment on principal phase spinelle surface is removed, beneficial to the coarse grained sorting of chromium slag,
Obtain high-quality filler.
Description of the drawings
Fig. 1 provides the preparation that a kind of utilization chromium slag prepares high-quality chromium slag filler and recovery sodium carbonate for the embodiment of the present invention
The flow chart of method；
Fig. 2 is that the embodiment of the present invention 1 provides the system that a kind of utilization chromium slag prepares high-quality chromium slag filler and recovery sodium carbonate
Preparation Method chromium slag XRD thing phasors.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and
It is not used in the restriction present invention.
The embodiment of the present invention provides a kind of utilization chromium slag and prepares high-quality chromium slag filler and reclaim the preparation method of sodium carbonate,
As shown in figure 1, the method is realized by following steps：
Step 1：Ball milling is sieved：Dry non-calcium chromium slags are put in ball grinder, ball milling, ball milling are carried out by planetary ball mill
After the completion of be sized to 150～200 mesh；
Specifically, also include before the step 1：The chromium slag for weighing is dried into 10-14h at 100～120 DEG C, is obtained
Dry non-calcium chromium slags.
Step 2：Carburizing reagent：With liquid-solid ratio 3:1～5:1 adds the non-calcium chromium slags after deionized water and step 1 ball milling
To in hydro-thermal autoclave, into the hydro-thermal autoclave CO is passed through2Gas, 12～24h of reaction time；
Specifically, in the step 2, ratio of grinding media to material 6 is chosen:1～9:1, the rotating speed of ball mill is 300～400r/min.
Step 3：It is separated by filtration：After reaction terminates, stopping is passed through CO2Gas, after the hydro-thermal autoclave release, will be described
Material in hydro-thermal autoclave is filtered, washed, while collecting filter residue and filtrate；
Specifically, in the step 3, it is passed through CO2The pressure of gas be 0.2～1MPa, the temperature of the hydro-thermal autoclave
For 100～150 DEG C, mixing speed is 200～500r/min.
Step 4：Evaporative crystallization：Step 3 gained filtrate is heated to into 90～100 DEG C and is evaporated crystallization, treat Na in solution+
When concentration is more than 190g/L (when more white precipitate occurs in ie in solution), solution is cooled to into 30～40 DEG C, is filtered,
The white solid being filtrated to get carries out drying sodium carbonate solid at 150 DEG C；
Step 5：Filter residue is dried：Step 3 gained filter residue is put in slag drying machine and is dried, Gao Rong is obtained final product after drying
Point spinelle chromium slag filler.
Specifically, the step 5 also includes：The trickle powder of chromium slag is collected by drying machine bagroom, so as to
Separately recycle.
Embodiment 1：
The embodiment of the present invention provides a kind of utilization chromium slag and prepares high-quality chromium slag filler and reclaim the preparation method of sodium carbonate,
The method is：The chromium slag 300g that certain chromium salt factory calcium-free roasting method is produced is taken, the 12h test compositions such as institute of table 1 is dried at 110 DEG C
Show.Dry chromium slag is put in ball milling jar, ratio of grinding media to material 6 is chosen:1 carries out ball milling, the rotating speed of ball mill with planetary ball mill
300r/min, ball milling is selected to complete, the sub-sieve for crossing 150 mesh is standby；Chromium slag and 450ml water after 150g screenings is taken, is added together
To in the hydro-thermal autoclave of 2L, the kettle cover of hydro-thermal autoclave is sealed up, toward in hydro-thermal autoclave CO is passed through2Gas, pressure 1MPa, water
The temperature of thermal high kettle is 120 DEG C, stirs 300r/min, reaction time 12h；Kettle is torn in release after the completion of reaction open, takes out reactant
In material beaker, when feed liquid is also in muddiness, at once the liquid phase suspension containing subparticle is poured out filtration, obtain filter residue
1, now the settled coarse granule of beaker bottom individually filter, obtain filter residue 2, filter residue 1 and filter residue 2 collect respectively drying after survey
Composition as shown in table 2 and table 3.The filtrate collected is carried out concentration and evaporation, works as Na+(have a large amount of when concentration is more than 190g/L
When white solid occurs) crystallisation by cooling is carried out, white sodium carbonate solid is obtained after filtering drying.Be dried original chromium slag specimen product and
Coarse granule filter residue 2 carries out XRD material phase analysis, as a result as shown in Fig. 2 in figure a be chromium slag raw sample, b be the siccative of coarse granule filter residue 2
Sample；As seen from Figure 2, after carbonization, large or fine granule sorting, gained filter residue 2 is more pure Mg (Fe, Cr, Al)2O4Spinel, be high-melting-point, high-quality roasting filler.
Table 1 is dry original chromium slag specimen product component table (XRF)
Table 2 is the trickle component table of powder filter residue 1 (XRF)
Table 3 is the component table of coarse granule filter residue 2 (XRF)
The present invention can be processed being cleaned of chromium slag filler for returning, and while reclaiming sodium carbonate in slag, obtain Gao Rong
Point filler containing picotite, contributes to the further extraction and stove direct motion of chromium in chromium slag；By carburizing reagent, during chromium slag can be made
Most of sodium in the eutectics such as the phase of thing containing sodium, amorphous substance is converted into sodium carbonate and enters solution, while principal phase point containing chromium is brilliant
The parafacies such as stone and sodium aluminum silicate is peeled off, and the sodium carbonate crystallization in solution is reclaimed；Filter residue is dried and cloth bag by hot-blast stove
Gather dust, equivalent to the sorting for carrying out large or fine granule, can very well except parafacies such as the alumino-silicates dechromised in slag, it is to avoid when returning roasting
Eutectic phase is re-formed with sodium；
The CO that equipment is simple, flow process is short, used of the present invention2Ingredient requirement is not strict, is retrieved from the stove tail gas of factory,
Realize waste gas resource higher value application.
Embodiment 2：
The embodiment of the present invention provides a kind of utilization chromium slag and prepares high-quality chromium slag filler and reclaim the preparation method of sodium carbonate,
The method is：The chromium slag 400g that certain chromium salt factory calcium-free roasting method is produced is taken, at 120 DEG C 14h is dried.Dry chromium slag is put into
In ball milling jar, ratio of grinding media to material 6 is chosen:1 carries out ball milling with planetary ball mill, and the selection of speed 350r/min of ball mill, ball milling is complete
Into the sub-sieve for crossing 170 mesh is standby；Chromium slag and 800ml water after 200g screenings is taken, during the hydro-thermal autoclave of 2L is added to together,
The kettle cover of hydro-thermal autoclave is sealed up, toward in hydro-thermal autoclave CO is passed through2Gas, pressure 0.5MPa, the temperature of hydro-thermal autoclave is
120 DEG C, stir 350r/min, reaction time 12h；Kettle is torn in release after the completion of reaction open, in taking out reaction mass beaker, when feed liquid also
In muddiness when, at once the liquid phase suspension containing subparticle is poured out filtration, obtained filter residue 1, now beaker bottom has been
The coarse granule of precipitation is individually filtered, and obtains filter residue 2.The filtrate collected is carried out concentration and evaporation, works as Na+When concentration is more than 190g/L
Crystallisation by cooling is carried out (when there are a large amount of white solids to occur), white sodium carbonate solid is obtained after filtering drying.Through being carbonized,
After large or fine granule sorting, gained filter residue 2 is more pure Mg (Fe, Cr, Al)2O4Spinel, be high-melting-point, high-quality
Roasting filler.
Embodiment 3：
The embodiment of the present invention provides a kind of utilization chromium slag and prepares high-quality chromium slag filler and reclaim the preparation method of sodium carbonate,
The method is：The chromium slag 200g that certain chromium salt factory calcium-free roasting method is produced is taken, at 110 DEG C 10h is dried.Dry chromium slag is put into
In ball milling jar, ratio of grinding media to material 9 is chosen:1 carries out ball milling with planetary ball mill, and the selection of speed 400r/min of ball mill, ball milling is complete
Into the sub-sieve for crossing 200 mesh is standby；Chromium slag and 500ml water after 100g screenings is taken, during the hydro-thermal autoclave of 2L is added to together,
The kettle cover of hydro-thermal autoclave is sealed up, toward in hydro-thermal autoclave CO is passed through2Gas, pressure 1MPa, the temperature of hydro-thermal autoclave is 150
DEG C, stir 500r/min, reaction time 12h；Kettle is torn in release after the completion of reaction open, in taking out reaction mass beaker, when feed liquid is also located
When muddiness, at once the liquid phase suspension containing subparticle is poured out filtration, obtained filter residue 1, now beaker bottom is sunk
The coarse granule in shallow lake is individually filtered, and obtains filter residue 2.The filtrate collected is carried out concentration and evaporation, works as Na+When concentration is more than 190g/L
(when having a large amount of white solids to occur) carries out crystallisation by cooling, and white sodium carbonate solid is obtained after filtering drying.Through carbonization, slightly
After fine grained sorting, gained filter residue 2 is more pure Mg (Fe, Cr, Al)2O4Spinel, be high-melting-point, high-quality
Roasting filler.
The above, only presently preferred embodiments of the present invention is not intended to limit protection scope of the present invention.
Claims (5)
1. a kind of utilization chromium slag prepares high-quality chromium slag filler and reclaims the preparation method of sodium carbonate, it is characterised in that the method
Realized by following steps：
Step 1：Ball milling is sieved：Dry non-calcium chromium slags are put in ball grinder, ball milling is carried out by planetary ball mill, ball milling is completed
After be sized to 150～200 mesh；
Step 2：Carburizing reagent：With liquid-solid ratio 3:1～5:Non-calcium chromium slags after deionized water and step 1 ball milling are added to water by 1
In thermal high kettle, into the hydro-thermal autoclave CO is passed through2Gas, 12～24h of reaction time；
Step 3：It is separated by filtration：After reaction terminates, stopping is passed through CO2Gas, after the hydro-thermal autoclave release, by the hydro-thermal
Material in autoclave is filtered, washed, while collecting filter residue and filtrate；
Step 4：Evaporative crystallization：Step 3 gained filtrate is heated to into 90～100 DEG C and is evaporated crystallization, treat Na in solution+Concentration
During more than 190g/L, solution is cooled to into 30～40 DEG C, is filtered, the white solid being filtrated to get is carried out at 150 DEG C
Drying sodium carbonate solid；
Step 5：Filter residue is dried：Step 3 gained filter residue is put in slag drying machine and is dried, high-melting-point point is obtained final product after drying
Spar chromium slag filler.
2. utilization chromium slag according to claim 1 prepares high-quality chromium slag filler and reclaims the preparation method of sodium carbonate, its
It is characterised by, in the step 2, chooses ratio of grinding media to material 6:1～9:1, the rotating speed of ball mill is 300～400r/min.
3. utilization chromium slag according to claim 1 and 2 prepares high-quality chromium slag filler and reclaims the preparation method of sodium carbonate,
Characterized in that, in the step 3, being passed through CO2The pressure of gas is 0.2～1MPa, and the temperature of the hydro-thermal autoclave is 100
～150 DEG C, mixing speed is 200～500r/min.
4. utilization chromium slag according to claim 3 prepares high-quality chromium slag filler and reclaims the preparation method of sodium carbonate, its
It is characterised by, the step 5 also includes：The trickle powder of chromium slag is collected by drying machine bagroom.
5. utilization chromium slag according to claim 4 prepares high-quality chromium slag filler and reclaims the preparation method of sodium carbonate, its
It is characterised by, also includes before the step 1：The chromium slag for weighing is dried into 10-14h at 100～120 DEG C, drying is obtained
Non-calcium chromium slags.
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| CN201611023887.1A CN106564916B (en) | 2016-11-14 | 2016-11-14 | High quality chromium slag filler is prepared using chromium slag and reclaims the preparation method of sodium carbonate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107803063A (en) * | 2017-11-01 | 2018-03-16 | 武汉钢铁有限公司 | A kind of slag filter material for sponge urban construction and preparation method thereof |
| CN108585439A (en) * | 2018-03-13 | 2018-09-28 | 山东科技大学 | A method of detaching metallic particles from cupric zinc organic sludge |
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| US7128886B2 (en) * | 1999-01-08 | 2006-10-31 | Solvay Chemicals, Inc. | Sodium carbonate and sodium bicarbonate production from nahcolitic oil shale |
| CN101767825A (en) * | 2009-11-23 | 2010-07-07 | 中国科学院过程工程研究所 | Method for preparing chromium hemitrioxide by red-soil nickel ore |
| CN101824530A (en) * | 2010-04-08 | 2010-09-08 | 白向南 | Process for roasting chromite resources in ring kiln through pure oxygen by using low-temperature method and harmlessly and deeply utilizing chromium residue |
| CN102191374A (en) * | 2010-03-10 | 2011-09-21 | 中国科学院过程工程研究所 | Method for recycling traditional chromium residue |
| CN104762637A (en) * | 2015-02-13 | 2015-07-08 | 于志远 | Comprehensive utilization method and device for acid dissolution extraction of valuable element chromium silicon iron magnesium aluminum nickel from chromite |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7128886B2 (en) * | 1999-01-08 | 2006-10-31 | Solvay Chemicals, Inc. | Sodium carbonate and sodium bicarbonate production from nahcolitic oil shale |
| CN101767825A (en) * | 2009-11-23 | 2010-07-07 | 中国科学院过程工程研究所 | Method for preparing chromium hemitrioxide by red-soil nickel ore |
| CN102191374A (en) * | 2010-03-10 | 2011-09-21 | 中国科学院过程工程研究所 | Method for recycling traditional chromium residue |
| CN101824530A (en) * | 2010-04-08 | 2010-09-08 | 白向南 | Process for roasting chromite resources in ring kiln through pure oxygen by using low-temperature method and harmlessly and deeply utilizing chromium residue |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107803063A (en) * | 2017-11-01 | 2018-03-16 | 武汉钢铁有限公司 | A kind of slag filter material for sponge urban construction and preparation method thereof |
| CN107803063B (en) * | 2017-11-01 | 2020-01-14 | 武汉钢铁有限公司 | Steel slag filter material for sponge city construction and preparation method thereof |
| CN108585439A (en) * | 2018-03-13 | 2018-09-28 | 山东科技大学 | A method of detaching metallic particles from cupric zinc organic sludge |
| CN108585439B (en) * | 2018-03-13 | 2019-07-19 | 山东科技大学 | A method of separating metallic particles from cupric zinc organic sludge |
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| CN106564916B (en) | 2018-02-13 |
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