CN107963644A - A kind of method that magnesium salts is prepared using titanium white waste acid - Google Patents
A kind of method that magnesium salts is prepared using titanium white waste acid Download PDFInfo
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- CN107963644A CN107963644A CN201711106481.4A CN201711106481A CN107963644A CN 107963644 A CN107963644 A CN 107963644A CN 201711106481 A CN201711106481 A CN 201711106481A CN 107963644 A CN107963644 A CN 107963644A
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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
- C01F5/40—Magnesium sulfates
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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
- C01F5/12—Magnesia by thermal decomposition of magnesium compounds by thermal decomposition of magnesium sulfate, with or without reduction
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Abstract
The present invention relates to a kind of method that magnesium salts is prepared using titanium white waste acid, comprise the following steps that：Separation of solid and liquid after being pre-processed to titanium white waste acid；Magnesium oxychloride is beaten, and obtains magnesium oxychloride slurry；Magnesium oxychloride slurry is added in titanium white waste acid, heating water bath, and be passed through oxidant and carry out Air Exposure, obtain magnesium sulfate slurry；Magnesium sulfate slurry separation of solid and liquid, obtains magnesium sulfate filtrate；Prepare saturated solution of sodium carbonate；（6）The crystallization of bright sulfur acid postcooling is added into magnesium sulfate filtrate, is centrifuged, drying, you can obtains epsom salt；Epsom salt with sodium carbonate liquor mixed, obtain magnesium carbonate slurry；Magnesium carbonate slurry separation of solid and liquid after agitation, and with after desalination water washing filter cake, calcining, you can obtain magnesia；The present invention is reacted using titanium white waste acid and magnesium oxychloride, and production technical grade magnesium carbonate, magnesia instead of the reaction of the industrial concentrated sulfuric acid and magnesium ore, reduce production cost；Titanium white waste acid intractability is reduced at the same time, alleviates environmental pressure.
Description
Technical field
The present invention relates to a kind of method that magnesium salts is prepared using titanium white waste acid, is exactly a kind of titanium dioxide waste acid by sulfuric acid process
Technical grade sulfuric acid magnesium, method of magnesium oxide are produced, the pair circulation comprehensive that gives up for belonging to titanium chemical industry utilizes technical field.
Background technology
In the technical process of Titanium White Production By Sulfuric Acid Process, for sulfuric acid as intermediate medium, it is only involved in reaction without entering
Final products, thus in hydrolyzing process by discharge concentration be about 20% spent acid.Shown according to ASSOCIATE STATISTICS, often produce 1t titaniums
Generation concentration is 20% spent acid 8t or so by white powder.Meanwhile will discharge in the processes such as titanium sulfate, the purification of metatitanic acid, washing
Concentration is about 2% spent acid, is shown according to ASSOCIATE STATISTICS, and it is 2% spent acid 80t or so often to produce 1t titanium dioxides by generation concentration.
Titanium white waste acid mainly contains free sulfuric acid, ferrous sulfate, metatitanic acid and other sulfate etc., it is formed also because its concentration is different
And there is larger difference.It is usually qualified discharge after being neutralized with alkaline waste water for the spent acid that concentration is 2%.And for 20% it is useless
Acid, since its acid concentration is higher, discharge capacity is larger, if directly discharge will cause environment very big pollution, while to money
Source is also a kind of serious waste.In order to solve the problems, such as the pollution of spent acid and recycle, domestic and international scientific worker causes always
Power is in the Controlling research of spent acid.Due to titanium white waste acid complicated component, it is administered, and there are larger technical difficulty, Processing tecchnics also to have more
Kind.At present at home in titanium white enterprise, the titanium white waste acid processing methods of industrial applications mainly has vacuum concentration, lime to neutralize,
Leach phosphorus ore tricresyl phosphate kind technique.It is concentrated in vacuo higher to the more demanding of equipment, cost；By-product caused by lime neutralization
Thing is more, and post-processing is relatively difficult；The pollution problem of early period is simply transferred to the later stage and prepares phosphoric acid by leaching phosphorus ore phosphoric acid
Technique in, post-processing is still severeer.
Titanium white waste acid production magnesium sulfate, magnesia can efficiently reduce the environmental protection pressure of titanium powder industry, take full advantage of me
The magnesium ore resources that state enriches.CN102190333A is using Waste Sulfuric Acid dissolving serpentine, the process such as salkali waste neutralization precipitation, pyrolytic
Produce high-purity magnesium sulfate.It is there are technological process length, the problem of accessory substance is more, and production cost is high.CN1063730C uses titanium white
Spent acid and magnesia or oxidation reactive magnesium production magnesium sulfate, are separated, steam hair concentration, hydrogen peroxide oxidation mode using press filtration twice
Produce technical grade sulfuric acid magnesium.It is there are technological process length, the problem of high energy consumption is of high cost, and magnesium yield is low.CN101104521A is adopted
With magnesium sulfate waste liquid, magnesia is prepared through pervaporation-calcine technology, there are high energy consumption, environmental pollution is larger, will to equipment for it
Ask the problem of higher.
In conclusion titanium white waste acid production magnesium system inorganic salts（Magnesium sulfate, magnesia etc.）, magnesium sulfate, the product of magnesia
It is difficult the problem of coordination that quality and production cost, which are one,.Restrict the major influence factors of titanium white waste acid production magnesium system inorganic salts
Have：The impurity that titanium white waste acid introduces, causes the yield of product generally relatively low, which is that magnesium system inorganic salts industry wishes to solve always
Certainly unsolved technical barrier.
The content of the invention
The present invention is directed to the deficiencies in the prior art, there is provided a kind of method that magnesium salts is prepared using titanium white waste acid,
To solve problems of the prior art.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of method that magnesium salts is prepared using titanium white waste acid, it is characterised in that comprise the following steps that：
（1）Titanium white waste acid cleans：After being pre-processed to titanium white waste acid, waste water is passed through into equipment for separating liquid from solid and carries out solid-liquid
Separation, the titanium white waste acid after separation of solid and liquid is added in acidolysis groove, is stirred continuously and is warming up to 60-70 DEG C；
（2）Magnesium oxychloride is beaten：Magnesium oxychloride and clear water are mixed with beating, obtain magnesium oxychloride slurry；
（3）Acidolysis reaction：By step（2）Obtained magnesium oxychloride slurry is added to step（1）In obtained titanium white waste acid, and make to mix
Compound carries out heating water bath at 60-70 DEG C, stirring while adding and to adjust pH be 7.5-8, and mixing 25- is carried out after adding
40 minutes, continue to stir and be slowly introducing into mixed liquor oxidant carry out Air Exposure 1-3 it is small when after, add bright sulfur acid
PH value is adjusted to 7.0-7.5, obtains magnesium sulfate slurry；
（4）Purification and impurity removal：By step（3）Obtained magnesium sulfate slurry carries out separation of solid and liquid, obtains magnesium sulfate filtrate and filter residue,
Desalted water is added into filter residue and continues washing separation, and obtains washing lotion；
（5）Prepare saturated solution of sodium carbonate：Sodium carbonate is mixed with clear water, and controlling reaction temperature is 40-50 DEG C, to mixture
In be continuously added sodium carbonate until sodium carbonate cannot dissolve, you can obtain saturated sodium carbonate solution；
（6）The preparation of magnesium sulfate：To step（4）Bright sulfur acid is added in obtained magnesium sulfate filtrate adjusts pH value to be mixed to 4-4.5
After liquid carries out crystallisation by cooling, centrifuge, obtain crystal and mother liquor, crystal is put into drying unit and is dried, you can
Obtain epsom salt；
（7）Magnesium sulfate is reacted with sodium carbonate：By step（6）Obtained epsom salt and step（5）Obtained sodium carbonate liquor
Mixed, and make mixed liquor be reacted to obtain magnesium carbonate slurry at 60-70 DEG C；
（8）It is prepared by magnesia：By step（7）Obtained magnesium carbonate slurry carries out solid-liquid after being stirred 25-35 minutes at 60-70 DEG C
Separation, and with after desalination water washing filter cake, filter cake is dried and is calcined, you can obtains magnesia.
As a modification of the present invention, the step（2）In, the content of magnesium oxychloride is 40-50% in magnesium oxychloride slurry.
As a modification of the present invention, the step（3）The mass ratio of middle magnesium oxychloride and titanium white waste acid is 1：2.5-
2.9。
As a modification of the present invention, the step（1）In, the pre-treatment step of titanium white waste acid is as follows：At room temperature, to
Flocculant is added in titanium white waste acid, separation of solid and liquid is carried out after sedimentation recycling metatitanic acid and collects filtered fluid, you can obtain titanium white and give up
Acid.
As a modification of the present invention, the flocculant is polyacrylamide.
As a modification of the present invention, the mass ratio of the titanium white waste acid and polyacrylamide is 1：0.0005.
As a modification of the present invention, the step（3）In the oxidant that is passed through be compressed air.Using compressed air
Stirring is played, accelerates the effect of reaction, and other impurities can be introduced to avoid to system.
As a modification of the present invention, the step（4）In obtained washing lotion add to step（2）In, and continue into
Row recycles.
As a modification of the present invention, the step（6）In obtained mother liquor add to step（3）In, and continue into
Row recycles.
Light spent acid in the present invention to be produced in sulfuric acid method titanium pigment production process（Sulfuric acid concentration is more than 20%）For raw material；
Step（2）The MgO contents of middle magnesium oxychloride are more than 85%.
Solid content in magnesium oxychloride slurry is 50% or so, in magnesium oxychloride slurry, the too low magnesium oxychloride free settling of solid content, Gu
Too high levels cause the viscosity of slurry larger, are unfavorable for effecting reaction progress, reduce reaction efficiency.
Titanium white waste acid prepares magnesium sulfate, magnesia, general to require using magnesium system ore more than 85% content of magnesia, titanium
Impurity after white spent acid and the ore acidolysis of magnesium system in liquid phase, it is general using pH value mode purification and impurity removal is adjusted, to product purity shadow
Ringing larger element can remove during the reaction for materials such as ferrous iron, calcium, manganese, titaniums, and end product quality will not be caused
Influence.
For ferrous iron, after being oxidized to ferric iron, it precipitates pH and magnesium gap is larger, will not be to the yield and quality of product
Impact.For calcium constituent, because the calcium content of titanium white waste acid and ore is natively very low, so the influence of calcium is ignored not
Meter.And to the manganese element in spent acid, higher pH value is adjusted at the beginning, can effectively remove the manganese sulfate in liquid phase, but at the same time
Magnesium sulfate can also generate magnesium hydrate precipitate, cause the loss of magnesium elements, in alkaline conditions, be passed through compressed air, make sulfuric acid
Manganese ultimately generates manganese dioxide removing, then returns tune with bright sulfur acid, the magnesium hydroxide of generation is become magnesium sulfate again, and dioxy
Change manganese separation of solid and liquid to remove, while so eliminating manganese element, also ensure that magnesium sulfate in high yield.
The reaction equation of the present invention is as follows：
MgO+H2SO4=MgSO4
FeSO4+Ca(OH)2=Fe(OH)2+CaSO4
MnSO4+Ca(OH)2=Mn(OH)2+CaSO4
4Fe(OH)2+O2+2H2O=4Fe(OH)3
2Mn(OH)2+O2=2MnO2+2H2O
MgSO4+Na2CO3=MgCO3+Na2SO4
MgCO3=MgO+H2O
As a result of above technology, the present invention compared with the prior art, has the advantage that as follows：
The present invention is reacted using titanium white waste acid and magnesium oxychloride, production technical grade magnesium carbonate, magnesia.Instead of the industrial concentrated sulfuric acid with
The reaction of magnesium ore, reduces production cost；Titanium white waste acid intractability is reduced at the same time, alleviates environmental pressure, the work of generation
Industry level magnesium carbonate, magnesia, value is higher, and economic benefit is very notable, and that has widened titanium white waste acid to a certain extent applies model
Enclose, simple production process, small investment, being effectively utilized titanium white waste acid reduces production cost, high income, product purity height.This
Whole technique is invented without useless secondary discharge, there is significant social benefit and larger economic benefit.
Brief description of the drawings
Fig. 1 is a kind of process flow chart that magnesium salts is prepared using titanium white waste acid.
Embodiment
With reference to embodiment, the present invention is furture elucidated.
Embodiment 1：
A kind of method that magnesium salts is prepared using titanium white waste acid, it is characterised in that comprise the following steps that：
（1）Titanium white waste acid cleans：To titanium white waste acid（Its main component, is calculated as in mass ratio：H2SO430.11%, FeSO4
7.48%, Al2(SO4)30.57%, MgSO42.45%, TiO20.45%）After being pre-processed, waste water is passed through to solid-liquid point
From separation of solid and liquid is carried out in device, the titanium white waste acid after separation of solid and liquid is added in acidolysis groove, is stirred continuously and is warming up to 60
℃；
（2）Magnesium oxychloride is beaten：By magnesium oxychloride（Its main component, is calculated as in mass ratio：MgO 95.66%, CaO 1.39%）With it is clear
Water is mixed with beating, and obtains magnesium oxychloride slurry；The content of magnesium oxychloride is 50% in magnesium oxychloride slurry；
（3）Acidolysis reaction：By step（2）Obtained magnesium oxychloride slurry and step（1）In obtained titanium white waste acid, and make mixture
Carry out heating water bath at 60 DEG C, it is stirring while adding and adjust pH as 7.5, carry out being mixed 25 minutes after adding, continue into
Row stir and be slowly introducing into mixed liquor oxidant carry out Air Exposure 1 it is small when after, add bright sulfur acid for adjusting pH value to 7.0,
Obtain magnesium sulfate slurry；The mass ratio of magnesium oxychloride and titanium white waste acid is 1:2.85；The oxidant entered is compressed air.
（4）Purification and impurity removal：By step（3）Obtained magnesium sulfate slurry carries out separation of solid and liquid, obtain magnesium sulfate filtrate and
Filter residue, desalted water is added into filter residue and continues washing separation, and obtains washing lotion；Obtained washing lotion is added to step（2）In,
And continue to recycle；
（5）Prepare saturated solution of sodium carbonate：Sodium carbonate is mixed with clear water, and controlling reaction temperature is 40 DEG C, into mixture
Sodium carbonate is continuously added until sodium carbonate cannot dissolve, you can obtain saturated sodium carbonate solution；
（6）The preparation of magnesium sulfate：To step（4）Bright sulfur acid is added in obtained magnesium sulfate filtrate and adjusts pH value to 4.5, by mixed liquor
After carrying out crystallisation by cooling, centrifuge, obtain crystal and mother liquor, crystal is put into drying unit and is dried, you can
To epsom salt；Obtained mother liquor is added to step（3）In, and continue to recycle；
（7）Magnesium sulfate is reacted with sodium carbonate：By step（6）Obtained epsom salt and step（5）Obtained sodium carbonate liquor
Mixed, and make mixed liquor be reacted to obtain magnesium carbonate slurry at 60 DEG C；
（8）It is prepared by magnesia：By step（7）Obtained magnesium carbonate slurry carries out separation of solid and liquid after being stirred 25 minutes at 60 DEG C,
And with after desalination water washing filter cake, filter cake is dried and is calcined, you can obtains magnesia.
The pre-treatment step of titanium white waste acid is as follows：At room temperature, flocculant is added into titanium white waste acid（Polyacrylamide）, titanium
The quality of white spent acid and the mass ratio of polyacrylamide are 1：0.0005, sedimentation carries out separation of solid and liquid after recycling metatitanic acid and collects
Filtered fluid, you can obtain titanium white waste acid.
Analyze magnesium sulfate and magnesium oxide product component shows, 95.45% magnesia purity 95.3% of magnesium sulfate purity.
Embodiment 2：
A kind of method that magnesium salts is prepared using titanium white waste acid, it is characterised in that comprise the following steps that：
（1）Titanium white waste acid cleans：To titanium white waste acid（Its main component, is calculated as in mass ratio：H2SO430.11%, FeSO4
7.48%, Al2(SO4)30.57%, MgSO42.45%, TiO20.45%）After being pre-processed, waste water is passed through to solid-liquid point
From separation of solid and liquid is carried out in device, the titanium white waste acid after separation of solid and liquid is added in acidolysis groove, is stirred continuously and is warming up to 65
℃；
（2）Magnesium oxychloride is beaten：By magnesium oxychloride（Its main component, is calculated as in mass ratio：MgO 95.66%, CaO 1.39%）With it is clear
Water is mixed with beating, and obtains magnesium oxychloride slurry；The content of magnesium oxychloride is 45% in magnesium oxychloride slurry；
（3）Acidolysis reaction：By step（2）Obtained magnesium oxychloride slurry and step（1）In obtained titanium white waste acid, and make mixture
Carry out heating water bath at 65 DEG C, it is stirring while adding and adjust pH as 7.5, carry out being mixed 30 minutes after adding, continue into
Row stir and be slowly introducing into mixed liquor oxidant carry out Air Exposure 2 it is small when after, add bright sulfur acid for adjusting pH value to 7.5,
Obtain magnesium sulfate slurry；The mass ratio of magnesium oxychloride and titanium white waste acid is 1：2.5；The oxidant being passed through is compressed air；
（4）Purification and impurity removal：By step（3）Obtained magnesium sulfate slurry carries out separation of solid and liquid, obtains magnesium sulfate filtrate and filter residue,
Desalted water is added into filter residue and continues washing separation, and obtains washing lotion；Obtained washing lotion is added to step（2）In, and after
It is continuous to be recycled；
（5）Prepare saturated solution of sodium carbonate：Sodium carbonate is mixed with clear water, and controlling reaction temperature is 45 DEG C, into mixture
Sodium carbonate is continuously added until sodium carbonate cannot dissolve, you can obtain saturated sodium carbonate solution；
（6）The preparation of magnesium sulfate：To step（4）Bright sulfur acid is added in obtained magnesium sulfate filtrate and adjusts pH value to 4, by mixed liquor into
After row crystallisation by cooling, centrifuge, obtain crystal and mother liquor, crystal is put into drying unit and is dried, you can obtain
Epsom salt；Obtained mother liquor is added to step（3）In, and continue to recycle；
（7）Magnesium sulfate is reacted with sodium carbonate：By step（6）Obtained epsom salt and step（5）Obtained sodium carbonate liquor
Mixed, and make mixed liquor be reacted to obtain magnesium carbonate slurry at 68 DEG C；
（8）It is prepared by magnesia：By step（7）Obtained magnesium carbonate slurry carries out separation of solid and liquid after being stirred 30 minutes at 65 DEG C,
And with after desalination water washing filter cake, filter cake is dried and is calcined, you can obtains magnesia.
The pre-treatment step of titanium white waste acid is as follows：At room temperature, flocculant is added into titanium white waste acid（Polyacrylamide）, titanium
The quality of white spent acid and the mass ratio of polyacrylamide are 1：0.0005, sedimentation carries out separation of solid and liquid after recycling metatitanic acid and collects
Filtered fluid, you can obtain titanium white waste acid.
Analyze magnesium sulfate and magnesium oxide product component shows, 95.87% magnesia purity 96.03% of magnesium sulfate purity.
Embodiment 3：
A kind of method that magnesium salts is prepared using titanium white waste acid, it is characterised in that comprise the following steps that：
（1）Titanium white waste acid cleans：To titanium white waste acid（Its main component, is calculated as in mass ratio：H2SO430.11%, FeSO4
7.48%, Al2(SO4)30.57%, MgSO42.45%, TiO20.45%）After being pre-processed, waste water is passed through to solid-liquid point
From separation of solid and liquid is carried out in device, the titanium white waste acid after separation of solid and liquid is added in acidolysis groove, is stirred continuously and is warming up to 70
℃；
（2）Magnesium oxychloride is beaten：By magnesium oxychloride（Its main component, is calculated as in mass ratio：MgO 95.66%, CaO 1.39%）With it is clear
Water is mixed with beating, and obtains magnesium oxychloride slurry；The content of magnesium oxychloride is 40% in magnesium oxychloride slurry；
（3）Acidolysis reaction：By step（2）Obtained magnesium oxychloride slurry and step（1）In obtained titanium white waste acid, and make mixture
Carry out heating water bath at 70 DEG C, it is stirring while adding and adjust pH as 8, carry out being mixed 40 minutes after adding, continue
Stir and be slowly introducing into mixed liquor oxidant carry out Air Exposure 3 it is small when after, add bright sulfur acid for adjusting pH value to 7.0, obtain
To magnesium sulfate slurry；The mass ratio of magnesium oxychloride and titanium white waste acid is 1：2.9；The oxidant being passed through is compressed air；
（4）Purification and impurity removal：By step（3）Obtained magnesium sulfate slurry carries out separation of solid and liquid, obtains magnesium sulfate filtrate and filter residue,
Desalted water is added into filter residue and continues washing separation, and obtains washing lotion；Obtained washing lotion is added to step（2）In, and after
It is continuous to be recycled；
（5）Prepare saturated solution of sodium carbonate：Sodium carbonate is mixed with clear water, and controlling reaction temperature is 50 DEG C, into mixture
Sodium carbonate is continuously added until sodium carbonate cannot dissolve, you can obtain saturated sodium carbonate solution；
（6）The preparation of magnesium sulfate：To step（4）Bright sulfur acid is added in obtained magnesium sulfate filtrate and adjusts pH value to 4.5, by mixed liquor
After carrying out crystallisation by cooling, centrifuge, obtain crystal and mother liquor, crystal is put into drying unit and is dried, you can
To epsom salt；Obtained mother liquor is added to step（3）In, and continue to recycle；
（7）Magnesium sulfate is reacted with sodium carbonate：By step（6）Obtained epsom salt and step（5）Obtained sodium carbonate liquor
Mixed, and make mixed liquor be reacted to obtain magnesium carbonate slurry at 70 DEG C；
（8）It is prepared by magnesia：By step（7）Obtained magnesium carbonate slurry carries out separation of solid and liquid after being stirred 35 minutes at 70 DEG C,
And with after desalination water washing filter cake, filter cake is dried and is calcined, you can obtains magnesia.
The pre-treatment step of titanium white waste acid is as follows：At room temperature, flocculant is added into titanium white waste acid（Polyacrylamide）, titanium
The quality of white spent acid and the mass ratio of polyacrylamide are 1：0.0005, sedimentation carries out separation of solid and liquid after recycling metatitanic acid and collects
Filtered fluid, you can obtain titanium white waste acid.
Analyze magnesium sulfate and magnesium oxide product component shows, 95.65% magnesia purity 95.54% of magnesium sulfate purity.
Above-described embodiment is only the preferred technical solution of the present invention, and is not construed as the limitation for the present invention, the present invention
Protection domain should with claim record technical solution, including claim record technical solution in technical characteristic etc.
It is protection domain with alternative, i.e., equivalent substitution within this range is improved, also within protection scope of the present invention.
Claims (9)
- A kind of 1. method that magnesium salts is prepared using titanium white waste acid, it is characterised in that comprise the following steps that：（1）Titanium white waste acid cleans：After being pre-processed to titanium white waste acid, waste water is passed through into equipment for separating liquid from solid and carries out solid-liquid Separation, the titanium white waste acid after separation of solid and liquid is added in acidolysis groove, is stirred continuously and is warming up to 60-70 DEG C；（2）Magnesium oxychloride is beaten：Magnesium oxychloride and clear water are mixed with beating, obtain magnesium oxychloride slurry；（3）Acidolysis reaction：By step（2）Obtained magnesium oxychloride slurry is added to step（1）In obtained titanium white waste acid, and make to mix Compound carries out heating water bath at 60-70 DEG C, stirring while adding and to adjust pH be 7.5-8, and mixing 25- is carried out after adding 40 minutes, continue to stir and be slowly introducing into mixed liquor oxidant carry out Air Exposure 1-3 it is small when after, add bright sulfur acid PH value is adjusted to 7.0-7.5, obtains magnesium sulfate slurry；（4）Purification and impurity removal：By step（3）Obtained magnesium sulfate slurry carries out separation of solid and liquid, obtains magnesium sulfate filtrate and filter residue, Desalted water is added into filter residue and continues washing separation, and obtains washing lotion；（5）Prepare saturated solution of sodium carbonate：Sodium carbonate is mixed with clear water, and controlling reaction temperature is 40-50 DEG C, to mixture In be continuously added sodium carbonate until sodium carbonate cannot dissolve, you can obtain saturated sodium carbonate solution；（6）The preparation of magnesium sulfate：To step（4）Bright sulfur acid is added in obtained magnesium sulfate filtrate adjusts pH value to be mixed to 4-4.5 After liquid carries out crystallisation by cooling, centrifuge, obtain crystal and mother liquor, crystal is put into drying unit and is dried, you can Obtain epsom salt；（7）Magnesium sulfate is reacted with sodium carbonate：By step（6）Obtained epsom salt and step（5）Obtained sodium carbonate liquor Mixed, and make mixed liquor be reacted to obtain magnesium carbonate slurry at 60-70 DEG C；（8）It is prepared by magnesia：By step（7）Obtained magnesium carbonate slurry carries out solid-liquid after being stirred 25-35 minutes at 60-70 DEG C Separation, and with after desalination water washing filter cake, filter cake is dried and is calcined, you can obtains magnesia.
- A kind of 2. method that magnesium salts is prepared using titanium white waste acid according to claim 1, it is characterised in that：The step（2） In, the content of magnesium oxychloride is 40-50% in magnesium oxychloride slurry.
- A kind of 3. method that magnesium salts is prepared using titanium white waste acid according to claim 1, it is characterised in that：The step（3） The mass ratio of middle magnesium oxychloride and titanium white waste acid is 1：2.5-2.9.
- A kind of 4. method that magnesium salts is prepared using titanium white waste acid according to claim 1, it is characterised in that：The step（1） In, the pre-treatment step of titanium white waste acid is as follows：At room temperature, flocculant is added into titanium white waste acid, sedimentation recycling metatitanic acid is laggard Row separation of solid and liquid simultaneously collects filtered fluid, you can obtains titanium white waste acid.
- A kind of 5. method that magnesium salts is prepared using titanium white waste acid according to claim 4, it is characterised in that：The flocculant is Polyacrylamide.
- A kind of 6. method that magnesium salts is prepared using titanium white waste acid according to claim 5, it is characterised in that：The titanium white waste acid Mass ratio with polyacrylamide is 1：0.0005.
- A kind of 7. method that magnesium salts is prepared using titanium white waste acid according to claim 1, it is characterised in that：The step（3） In the oxidant that is passed through be compressed air.
- A kind of 8. method that magnesium salts is prepared using titanium white waste acid according to claim 1, it is characterised in that：The step（4） In obtained washing lotion add to step（2）In, and continue to recycle.
- A kind of 9. method that magnesium salts is prepared using titanium white waste acid according to claim 1, it is characterised in that：The step（6） In obtained mother liquor add to step（3）In, and continue to recycle.
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| CN110040698A (en) * | 2019-05-17 | 2019-07-23 | 成都先进金属材料产业技术研究院有限公司 | The method of magnesium sulfate processing titanium dioxide waste acid by sulfuric acid process |
| CN110104616A (en) * | 2019-04-24 | 2019-08-09 | 成都先进金属材料产业技术研究院有限公司 | Utilize the method for sodium tetraborate concentration titanium white waste acid |
| CN111017968A (en) * | 2019-12-27 | 2020-04-17 | 河北邢台冶金镁业有限公司 | Method for preparing pure magnesium sulfate by using light burned bitter soil as raw material without adding any impurity removing agent |
| CN113582224A (en) * | 2021-09-06 | 2021-11-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Resource utilization method for titanium white waste acid leaching fused salt chlorination slag |
| WO2022123546A1 (en) | 2020-12-11 | 2022-06-16 | Amateq Holding Gmbh | Process for preparing magnesium sulphate, magnesium sulphate obtained by said process, and use of said magnesium sulphate as a fertilizer |
| WO2023237737A1 (en) * | 2022-06-10 | 2023-12-14 | Amateq Holding Gmbh | Process for preparing magnesium sulphate, magnesium sulphate obtainable by said process, and use of said magnesium sulphate as a fertilizer |
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| CN106348319A (en) * | 2016-11-18 | 2017-01-25 | 营口东吉科技（集团）有限公司 | Method for utilizing serpentine for preparing high-purity magnesium oxide |
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| CN106348319A (en) * | 2016-11-18 | 2017-01-25 | 营口东吉科技（集团）有限公司 | Method for utilizing serpentine for preparing high-purity magnesium oxide |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110104616A (en) * | 2019-04-24 | 2019-08-09 | 成都先进金属材料产业技术研究院有限公司 | Utilize the method for sodium tetraborate concentration titanium white waste acid |
| CN110040698A (en) * | 2019-05-17 | 2019-07-23 | 成都先进金属材料产业技术研究院有限公司 | The method of magnesium sulfate processing titanium dioxide waste acid by sulfuric acid process |
| CN110040698B (en) * | 2019-05-17 | 2022-07-29 | 成都先进金属材料产业技术研究院股份有限公司 | Method for treating titanium dioxide waste acid by using magnesium sulfate |
| CN111017968A (en) * | 2019-12-27 | 2020-04-17 | 河北邢台冶金镁业有限公司 | Method for preparing pure magnesium sulfate by using light burned bitter soil as raw material without adding any impurity removing agent |
| WO2022123546A1 (en) | 2020-12-11 | 2022-06-16 | Amateq Holding Gmbh | Process for preparing magnesium sulphate, magnesium sulphate obtained by said process, and use of said magnesium sulphate as a fertilizer |
| CN113582224A (en) * | 2021-09-06 | 2021-11-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Resource utilization method for titanium white waste acid leaching fused salt chlorination slag |
| WO2023237737A1 (en) * | 2022-06-10 | 2023-12-14 | Amateq Holding Gmbh | Process for preparing magnesium sulphate, magnesium sulphate obtainable by said process, and use of said magnesium sulphate as a fertilizer |
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