CN109896550A - A kind of method that the utilization of ternary precursor devil liquor recovery prepares iron oxide red - Google Patents
A kind of method that the utilization of ternary precursor devil liquor recovery prepares iron oxide red Download PDFInfo
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- CN109896550A CN109896550A CN201910352120.0A CN201910352120A CN109896550A CN 109896550 A CN109896550 A CN 109896550A CN 201910352120 A CN201910352120 A CN 201910352120A CN 109896550 A CN109896550 A CN 109896550A
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Abstract
The invention belongs to chemical technology fields, the method for preparing iron oxide red is utilized using titanium dioxide byproduct ferrous sulfate and ternary precursor nickle cobalt lithium manganate devil liquor recovery more particularly to a kind of, the following steps are included: 1) ferrous sulfate water-bath is dissolved, sulfide removing heavy metals are added and promote hydrolysis except titanium aluminium obtains solution A；2) hydrogen peroxide and NCM presoma waste liquid are added in solution A using two bursts of cocurrents, mixed liquid B after being aoxidized, and the pH to 3.5~4.5 of mixed liquid B is adjusted using the waste liquid regulator by 10~30% sodium hydroxides and the preparation of NCM presoma waste liquid, generates slurry C；3) slurry C is put into water-bath and is heated; stirring; filtering and washing; drying and calcining obtains iron oxide red, and the present invention, which prepares iron oxide red realization using waste liquid, to turn waste into wealth, and reduces wastewater treatment number; protect environment; also the production cost for preparing iron oxide red with ferrous sulfate, and simple process are greatlyd save, large-scale production is suitble to.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of ternary precursor devil liquor recovery utilization prepares the side of iron oxide red
Method.
Background technique
China is one of the big producer of iron oxide pigment in the world, and yield in recent years accounts for about the 1/3 of the whole world, is only second to titanium
The white second largest inorganic pigment and the first big colored organic pigments.Limitation due to various countries to heavy metallic pigment, iron oxide
Column pigment will have broader application prospect and stronger vitality.Domestic iron oxide red is prepared generally with iron sheet or iron at present
Bits are raw material, are prepared using wet process oxidation technology.The relatively good iron oxide red of pigment performance generally uses ferrous sulfate heptahydrate for original
Material preparation, but need a large amount of sodium hydroxides or ammonium hydroxide to be neutralized with the preparation of this method, valence of the cost often beyond iron oxide red itself
Value, so being difficult to realize extensive industrialization.
In recent years, electric car is commercially available fast development, thus brings the power battery market demand quickly to increase
Long, nickle cobalt lithium manganate (NCM) ternary material lithium battery is big because having many advantages, such as height ratio capacity, good cycle, being readily synthesized
Amount is applied on passenger car.And synthesizing NCM presoma needs could be co-precipitated completely under very strong alkaline condition, after separation of solid and liquid
Contain a large amount of hydroxyls and ammonia in waste liquid, ingredient is mainly Na+、SO4 2-、OH-、NH3·H2O, micro heavy (Ni, Co,
Mn) etc., actually these waste liquids are not used effectively, but directly handle, therefore it is useless to generate tens tons up to a million every year
Liquid, wastewater treatment also want acid adding to neutralize, and result in waste of resources.
CN102583575A discloses a kind of method using titanium dioxide waste residue ferrous sulfate production pigment-level iron oxide red, advanced
The removal of impurities of row ferrous sulfate, then ferrous sulfate solution is aoxidized, iron black precipitating is made, it is red that rear calcining prepares grade ferric oxide.
CN106115793A discloses a kind of ferric oxide red colorant and preparation method thereof, prepares sulfuric acid using the acid waste water of titanium dioxide pigment
Ferrous iron solution dilutes solution, and dispersing agent and liquid alkaline is added, and is passed through maximum air, controls material liquid pH, and it is straight to carry out oxidation reaction
To being in brownish red, iron red crystal seed formation solution is made, then secondary oxidation adds alkali control pH that ferric oxide red colorant is made.
Two above invention prepares iron oxide red with ferrous sulfate, all uses in liquid alkaline or ammonium hydroxide and generate the sediment of iron,
Calcining is dried again and is made iron oxide red, but through experiments, it was found that: to produce the piece alkali that 1 ton of iron oxide red needs nearly 1 ton, alkali at
Originally already exceed the value of general iron oxide red.Institute is difficult on large-scale industrial production at present in this way.The present invention
Contain a large amount of alkali and ammonium hydroxide using the waste liquid after ternary NCM precursor synthesis and titanium dioxide waste residue ferrous sulfate is prepared into pigment and uses
Iron oxide red, solve the problems, such as the cost of alkali very well, NCM presoma waste liquid rationally utilized, reduce wastewater treatment assembly
This, also greatly reduces the cost of production iron oxide red.
Summary of the invention
The present invention prepares pigment using titanium dioxide waste residue ferrous sulfate and ternary precursor precursor of nickel-cobalt-lithium-manganese-oxide waste liquid and uses
Iron oxide red method, which comprises the following steps:
(1) ferrous sulfate edulcoration purification: titanium white by product product ferrous sulfate heptahydrate being dissolved, is put into 30~60 DEG C of water-baths,
65~85g/L of concentration of iron in ferrous iron solution adjusts pH value of solution to 2.5~3.5 with sodium hydroxide solution, it is molten that vulcanized sodium is added
Liquid stirs 30min~2h, solution A is obtained by filtration；
(2) waste liquid pre-processes: filtering out insoluble matter in NCM presoma waste liquid by filter press, obtains clarification waste liquid；
(3) crystal seed is prepared: under room temperature (20~35 DEG C), by 30% hydrogen peroxide and NCM presoma waste liquid peristaltic pump two
Stock cocurrent is added in solution A, after adding, continues 3~12h of stirring, obtains mixed liquid B；
(4) it generates slurry C: mixed liquid B being put into 80~90 DEG C of water-baths and is heated, adjust mixed liquid B with waste liquid regulator
PH, so that pH is maintained at 3.5~4.5, stir 2~10h, generate slurry C；
(5) iron oxide red is made: slurry C is sufficiently washed with pure water, re-dry, roasting obtain iron oxide red.
Preferably, in step (1):
The concentration of sodium hydroxide solution is 10~25%；
Vulcanized sodium additional amount is heavy metal Ni, 1.1~1.3 times of Co, Zn and Mn total mole number in ferrous sulfate；
Preferably, in step (3):
The hydrogen peroxide additional amount is 1.0~1.3 times of the molal quantity of iron in ferrous sulfate solution；
The hydrogen peroxide is pumped into 4~12ml/min of speed；
The precursor of nickel-cobalt-lithium-manganese-oxide waste liquid is filtrate after the separation of solid and liquid of ternary nickle cobalt lithium manganate precursor synthesis, pH
10.5~12；
The precursor of nickel-cobalt-lithium-manganese-oxide waste liquid additional amount is 4~10 times of solution A total volume；
The precursor of nickel-cobalt-lithium-manganese-oxide waste liquid is pumped into 100~160ml/min of speed.
Preferably, in step (4):
The waste liquid regulator is formulated by sodium hydroxide and precursor of nickel-cobalt-lithium-manganese-oxide waste liquid, wherein sodium hydroxide
Account for the 10~30% of waste liquid regulator quality.
Preferably, in step (5):
The drying temperature is 80~120 DEG C；
The maturing temperature is 650~820 DEG C.
The method of the invention solve the problems, such as currently with ferrous sulfate preparation iron oxide red cost it is excessively high, also will be before NCM
Industrial wastes reasonable employment after driving body synthesis, reduces the pollution to environment.
Compared to the prior art, the beneficial effects of the present invention are:
(1) present invention prepares iron oxide red using the waste liquid after ternary precursor of nickel-cobalt-lithium-manganese-oxide precursor synthesis, gives up
Liquid ingredient is mainly Na+、SO4 2-、OH-、NH3·H2O, micro heavy (Ni, Co, Mn) etc., since NCM presoma is needed strong
It could be co-precipitated completely under the conditions of alkali, a large amount of alkali and ammonium hydroxide are added in synthesis process, it is also remaining that waste liquid is separated by solid-liquid separation after synthesis
A large amount of alkali and ammonium hydroxide are used as preparation iron oxide red neutralizer, can effectively reduce the cost of iron oxide red alkali, and be conducive to protection ring
Border；
(2) since synthesis precursor of nickel-cobalt-lithium-manganese-oxide presoma is complete coprecipitation reaction, raw material nickel salt, cobalt salt and manganese
The substantially all precipitating of salt, only micro Ni in waste liquid2+、Co2+And Mn2+, the pH that the present invention prepares iron oxide red is very low, in waste liquid
Only a small part foreign ion enters in iron oxide red, this micro impurity is very little on the performance of pigment and using influencing,
So foreign ion will not pollute iron oxide red in waste liquid；
(3) present invention prepares iron oxide red realization using precursor of nickel-cobalt-lithium-manganese-oxide waste liquid and ferrous sulfate and turns waste into wealth, and reduces
Wastewater treatment number, resource rational utilization are conducive to protect environment, also greatly save and prepare being produced into for iron oxide red with ferrous sulfate
This, and simple process, it is suitble to large-scale production.
Detailed description of the invention
The following further describes the present invention with reference to the drawings.
Fig. 1 is the method for the present invention flow diagram.
Specific embodiment
The present invention will be further described with reference to the examples below.Described embodiment and its result are merely to illustrate
The present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
(1) ferrous sulfate edulcoration purification: 500g titanium white by product product ferrous sulfate heptahydrate is dissolved in pure water to volume 1L,
It is put into 60 DEG C of water-baths, with 10% sodium hydroxide solution adjusting pH value of solution to 3.5,10g sodium sulfide solution is added, stirs 30min,
Solution A is obtained by filtration；
(2) waste liquid pre-processes: filtering out insoluble matter in NCM presoma waste liquid by filter press, obtains clarification waste liquid；
(3) it prepares crystal seed: under 28 DEG C of room temperature, 170 milliliter of 30% hydrogen peroxide and 10 liters of NCM presoma waste liquids being wriggled
It pumps two bursts of cocurrents to be added in solution A, pump speed is respectively 8ml/min and 130ml/min, continues to stir 8h, obtains mixed liquid B；
(4) generate slurry C: mixed liquid B is put into 80 DEG C of water-baths and is heated, with waste liquid regulator (20% sodium hydroxide and
80%NCM presoma waste liquid) pH that adjusts mixed liquid B, so that pH is maintained at 4.5, stir 10h, generates slurry C；
(5) iron oxide red is made: slurry C sufficiently being washed with pure water, 120 DEG C of dryings, 820 DEG C of roastings obtain iron oxide red.
Embodiment 2
(1) ferrous sulfate edulcoration purification: 500g titanium white by product product ferrous sulfate heptahydrate is dissolved in pure water to volume
1.35L is put into 30 DEG C of water-baths, adjusts pH value of solution to 2.5 with 25% sodium hydroxide solution, 10g sodium sulfide solution, stirring is added
Solution A is obtained by filtration in 1h；
(2) waste liquid pre-processes: filtering out insoluble matter in NCM presoma waste liquid by filter press, obtains clarification waste liquid；
(3) crystal seed is prepared: under 20 DEG C of room temperature, by 200 milliliter of 30% hydrogen peroxide and 5.4 liters of NCM presoma waste liquids with compacted
Dynamic two bursts of cocurrents of pump are added in solution A, and pump speed is respectively 4r/min and 100r/min, continue to stir 3h, obtain mixed liquid B；
(4) generate slurry C: mixed liquid B is put into 90 DEG C of water-baths and is heated, with waste liquid regulator (10% sodium hydroxide and
90%NCM presoma waste liquid) pH that adjusts mixed liquid B, so that pH is maintained at 3.5, stir 6h, generates slurry C；
(5) iron oxide red is made: slurry C sufficiently being washed with pure water, 80 DEG C of dryings, 650 DEG C of roastings obtain iron oxide red.
Embodiment 3
(1) ferrous sulfate edulcoration purification: 500g titanium white by product product ferrous sulfate heptahydrate is dissolved in pure water to volume
1.17L is put into 45 DEG C of water-baths, adjusts pH value of solution to 3.0 with 18% sodium hydroxide solution, 10g sodium sulfide solution, stirring is added
Solution A is obtained by filtration in 2h；
(2) waste liquid pre-processes: filtering out insoluble matter in NCM presoma waste liquid by filter press, obtains clarification waste liquid；
(3) it prepares crystal seed: under 35 DEG C of room temperature, 185 milliliter of 30% hydrogen peroxide and 9 liters of NCM presoma waste liquids being wriggled
It pumps two bursts of cocurrents to be added in solution A, pump speed is respectively 12r/min and 160r/min, continues to stir 12h, obtains mixed liquid B；
(4) generate slurry C: mixed liquid B is put into 85 DEG C of water-baths and is heated, with waste liquid regulator (30% sodium hydroxide and
70%NCM presoma waste liquid) pH that adjusts mixed liquid B, so that pH is maintained at 4.0, stir 2h, generates slurry C；
(5) iron oxide red is made: slurry C sufficiently being washed with pure water, 100 DEG C of dryings, 720 DEG C of roastings obtain iron oxide red.
Embodiment 4
(1) ferrous sulfate edulcoration purification: 500g titanium white by product product ferrous sulfate heptahydrate is dissolved in pure water to volume
1.35L is put into 30 DEG C of water-baths, adjusts pH value of solution to 2.5 with 25% sodium hydroxide solution, 10g sodium sulfide solution, stirring is added
Solution A is obtained by filtration in 1h；
(2) waste liquid pre-processes: filtering out insoluble matter in NCM presoma waste liquid by filter press, obtains clarification waste liquid；
(3) it prepares crystal seed: under 20 DEG C of room temperature, 160 milliliter of 30% hydrogen peroxide and 12 liters of NCM presoma waste liquids being wriggled
It pumps two bursts of cocurrents to be added in solution A, pump speed is respectively 4r/min and 100r/min, continues to stir 8h, obtains mixed liquid B；
(4) generate slurry C: mixed liquid B is put into 90 DEG C of water-baths and is heated, with waste liquid regulator (20% sodium hydroxide and
80%NCM presoma waste liquid) pH that adjusts mixed liquid B, so that pH is maintained at 3.5, stir 6h, generates slurry C；
(5) iron oxide red is made: slurry C sufficiently being washed with pure water, 80 DEG C of dryings, 650 DEG C of roastings obtain iron oxide red.
Comparative example 1
(1) ferrous sulfate edulcoration purification: 500g titanium white by product product ferrous sulfate heptahydrate will be dissolved in pure water to volume
1.17L is put into 45 DEG C of water-baths, and with 18% sodium hydroxide solution section pH value of solution to 3.0,10g sodium sulfide solution, stirring is added
2h stirs 2h, solution A is obtained by filtration；
(2) it aoxidizes: under 35 DEG C of room temperature, 185 milliliter of 30% hydrogen peroxide and 9 liters of pure water, two bursts of cocurrents of peristaltic pump being added
In solution A, pump speed is respectively 12r/min and 160r/min, continues to stir 12h, obtains mixed liquid B；
(3) it generates slurry C: mixed liquid B being put into 85 DEG C of water-baths and is heated, adjust mixed liquor with 30% sodium hydroxide solution
The pH of B makes pH be maintained at 4.0, stirs 2h, generates slurry C；
(4) iron oxide red is made: slurry C sufficiently being washed with pure water, 100 DEG C of dryings, 720 DEG C of roastings obtain iron oxide red.
Comparative example 2
(1) ferrous sulfate edulcoration purification: 500g titanium white by product product ferrous sulfate heptahydrate is dissolved in pure water to volume
1.17L is put into 45 DEG C of water-baths, adjusts pH value of solution to 3.0 with 18% sodium hydroxide solution, 10g sodium sulfide solution, stirring is added
Solution A is obtained by filtration in 2h；
(2) it prepares crystal seed: under 35 DEG C of room temperature, being passed through air, flow 10L/min to solution A, and 30% hydrogen-oxygen is added
Changing sodium solution makes pH reach 12.0, stirs 3h, obtains slurry B；
(3) it generates slurry C: mixed liquid B being put into 85 DEG C of water-baths and is heated, continue to be passed through air, flow 40L/min,
The pH for adjusting mixed liquid B with 30% sodium hydroxide solution again, makes pH be maintained at 4.0, stirs 6h, generates slurry C；
(4) iron oxide red is made: slurry C sufficiently being washed with pure water, 100 DEG C of dryings, 720 DEG C of roastings obtain iron oxide red.
Hydrogen peroxide needed for being computed 1 ton of iron oxide red of production and piece alkali (98% sodium hydroxide) amount such as table 1:
Table 1
Based on the above embodiments with comparative example it is found that the method for preparation iron oxide red provided by the invention, can significantly drop
The dosage of low alkali, is effectively reduced production cost.
The Applicant declares that the present invention illustrates method detailed of the invention by examples detailed above, but the present invention is not limited to
Above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.
Claims (5)
1. a kind of ternary precursor of nickel-cobalt-lithium-manganese-oxide devil liquor recovery utilizes the method for preparing iron oxide red, which is characterized in that including following
Step:
(1) ferrous sulfate edulcoration purification: titanium white by product product ferrous sulfate heptahydrate being dissolved, is put into 30~60 DEG C of water-baths, ferrous
65~85g/L of concentration of iron in solution adjusts pH value of solution to 2.5~3.5 with sodium hydroxide solution, sodium sulfide solution is added, stirs
30min~2h is mixed, solution A is obtained by filtration；
(2) waste liquid pre-processes: filtering out insoluble matter in NCM presoma waste liquid by filter press, obtains clarification waste liquid；
(3) it prepares crystal seed: at normal temperature, solution A is added in 30% hydrogen peroxide and NCM presoma waste liquid two bursts of cocurrents of peristaltic pump
In, after adding, continues 3~12h of stirring, obtain mixed liquid B；
(4) it generates slurry C: mixed liquid B being put into 80~90 DEG C of water-baths and is heated, waste liquid regulator adjusts the pH of mixed liquid B, makes
PH is maintained at 3.5~4.5, stirs 2~10h, generates slurry C；
(5) iron oxide red is made: slurry C is sufficiently washed with pure water, re-dry, roasting obtain iron oxide red.
2. the method according to claim 1, wherein in the step (1):
The concentration of sodium hydroxide solution is 10~25%；
Vulcanized sodium additional amount is heavy metal Ni, 1.1~1.3 times of Co, Zn and Mn total mole number in ferrous sulfate.
3. the method according to claim 1, wherein in the step (3):
The hydrogen peroxide additional amount is 1.0~1.3 times of the molal quantity of iron in ferrous sulfate solution；
The hydrogen peroxide is pumped into 4~12ml/min of speed；
The precursor of nickel-cobalt-lithium-manganese-oxide waste liquid is filtrate after the separation of solid and liquid of ternary nickle cobalt lithium manganate precursor synthesis, and pH exists
10.5~12；
The precursor of nickel-cobalt-lithium-manganese-oxide waste liquid additional amount is 4~10 times of solution A total volume；
The precursor of nickel-cobalt-lithium-manganese-oxide waste liquid is pumped into 100~160ml/min of speed.
4. the method according to claim 1, wherein in the step (4):
The waste liquid regulator is formulated by sodium hydroxide and precursor of nickel-cobalt-lithium-manganese-oxide waste liquid, and wherein sodium hydroxide accounts for useless
The 10~30% of liquid regulator quality.
5. the method according to claim 1, wherein in the step (5):
The drying temperature is 80~120 DEG C；
The maturing temperature is 650~820 DEG C.
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Cited By (1)
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| CN113697868A (en) * | 2021-08-17 | 2021-11-26 | 广东邦普循环科技有限公司 | Preparation method of ternary precursor |
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