CN104016393A - Method for preparing light calcium carbonate and magnesium oxide from dolomite - Google Patents
Method for preparing light calcium carbonate and magnesium oxide from dolomite Download PDFInfo
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- CN104016393A CN104016393A CN201410261848.XA CN201410261848A CN104016393A CN 104016393 A CN104016393 A CN 104016393A CN 201410261848 A CN201410261848 A CN 201410261848A CN 104016393 A CN104016393 A CN 104016393A
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- magnesium
- reaction
- calcium
- filter cake
- calcium carbonate
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 50
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 36
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 19
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910000514 dolomite Inorganic materials 0.000 title claims abstract description 18
- 239000010459 dolomite Substances 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 64
- 239000011575 calcium Substances 0.000 claims abstract description 36
- 239000012065 filter cake Substances 0.000 claims abstract description 36
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 31
- 238000001354 calcination Methods 0.000 claims abstract description 26
- 238000003763 carbonization Methods 0.000 claims abstract description 22
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 claims abstract description 17
- 229910000022 magnesium bicarbonate Inorganic materials 0.000 claims abstract description 17
- 239000002370 magnesium bicarbonate Substances 0.000 claims abstract description 17
- 235000014824 magnesium bicarbonate Nutrition 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000006276 transfer reaction Methods 0.000 claims abstract description 7
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 5
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 5
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 30
- 210000002249 digestive system Anatomy 0.000 claims description 20
- OGWLTJRQYVEDMR-UHFFFAOYSA-F tetramagnesium;tetracarbonate Chemical compound [Mg+2].[Mg+2].[Mg+2].[Mg+2].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O OGWLTJRQYVEDMR-UHFFFAOYSA-F 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000002956 ash Substances 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 13
- 235000002918 Fraxinus excelsior Nutrition 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 238000000197 pyrolysis Methods 0.000 claims description 11
- 238000010009 beating Methods 0.000 claims description 10
- 230000029087 digestion Effects 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 8
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 4
- 239000000174 gluconic acid Substances 0.000 claims description 4
- 235000012208 gluconic acid Nutrition 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- 238000005255 carburizing Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 159000000000 sodium salts Chemical class 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 abstract description 16
- 239000000047 product Substances 0.000 abstract description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 abstract description 10
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 abstract description 9
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001424 calcium ion Inorganic materials 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000001095 magnesium carbonate Substances 0.000 abstract description 6
- 229910000021 magnesium carbonate Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- 238000010000 carbonizing Methods 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- 239000012716 precipitator Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 238000004537 pulping Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 21
- 239000012071 phase Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 8
- 239000000292 calcium oxide Substances 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 6
- 229910019440 Mg(OH) Inorganic materials 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 235000014380 magnesium carbonate Nutrition 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 229960001708 magnesium carbonate Drugs 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 229910021532 Calcite Inorganic materials 0.000 description 2
- 229910020091 MgCa Inorganic materials 0.000 description 2
- 101100003996 Mus musculus Atrn gene Proteins 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- HHSPVTKDOHQBKF-UHFFFAOYSA-J calcium;magnesium;dicarbonate Chemical compound [Mg+2].[Ca+2].[O-]C([O-])=O.[O-]C([O-])=O HHSPVTKDOHQBKF-UHFFFAOYSA-J 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 208000004434 Calcinosis Diseases 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- MKKVKFWHNPAATH-UHFFFAOYSA-N [C].N Chemical compound [C].N MKKVKFWHNPAATH-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 150000001718 carbodiimides Chemical class 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910001748 carbonate mineral Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing light calcium carbonate and magnesium oxide from dolomite. The method comprises the following steps: firstly, calcining and slaking the dolomite to obtain a slaking liquid, converting calcium hydroxide in the slaking liquid to a soluble calcium ion solution through a phase-transfer reaction, meanwhile filtering out magnesium hydrate filter cakes containing impurities, feeding CO2 into the soluble calcium ion solution, precipitating and separating to obtain calcium carbonate and a filter liquor, pulping and carbonizing the magnesium hydrate filter cakes containing impurities to obtain a magnesium bicarbonate solution, then performing a pyrolytic reaction to obtain basic magnesium carbonate, and calcining to obtain light magnesium oxide. The method is simple in technical process and low in energy consumption without strong acid to leach and addition of an impurity removing precipitator, the calcium and magnesium separation effect is good, a common carbonization liquid-solid-gas three-phase reaction is avoided, the reaction condition is easily controlled, and prepared light calcium carbonate accords with demands of national corresponding product standard and lays research basis for industrial scale production.
Description
One, technical field
The present invention relates to the comprehensive utilization of rhombspar raw ore, be exactly a kind of by dolomite made for light calcium carbonate and method of magnesium oxide.
Two, background technology
Rhombspar is the compound of calcium and two kinds of carbonate of magnesium, and main component is MgO, CaO, SiO
2, Fe
2o
3, average content is respectively 21.29%, 30.42%, 0.78%, 0.13%, and wherein the theoretical maximum content of magnesium oxide in rhombspar is 21.4%.DOLOMITE CRYSTALS belongs to the carbonate minerals of trigonal system, is rhombohedron; Generally be white in color, canescence, relative density 2.8-2.9, Mohs' hardness 3.4-4, has vitreous luster; Water insoluble, with diluted acid sluggish, only under powder or heated condition, slowly bubble.
Along with China's economy develops rapidly, the exploitation dynamics of Mineral Resources in China is increasing, market will increase year by year to the demand of high-quality magnesium compound, and the magnesite of China, and Brine resources distributed areas are limited, but the distributed areas of rhombspar are wide, standing stock are abundant, and the comprehensive utilization of rhombspar has important realistic meaning to the magnesium resource exploitation of China.
The Application and Development of China's rhombspar relates generally in metallurgy industry as fusing agent ore use and by rhombspar carborization production Magnesium Carbonate Light 41-45 at present, rhombspar mostly is the elementary processing of simple mineral at metallurgy industry and environmental protection industry (epi) application, and added value of product is on the low side.
Rhombspar calcium magnesium separates and mainly contains at present rhombspar carborization, bittern-rhombspar method, and acid hydrolyzation, ammonium soaks method etc.The industrial carborization separating calcium and magnesium from rhombspar that mainly utilizes.Rhombspar carborization basic skills is that rhombspar is made to magnesium oxide and calcium oxide in 950-1200 DEG C of calcining.Forge add water digestion slagging-off of powder and be refined into slurry, slurry is used CO in carbonating tower
2gas carbonization, by Ca (OH)
2be converted into CaCO
3, MgO changes Mg (HCO into
3)
2.Carbodiimide solution is filtered, and filter residue is for containing magnesium calcium carbonate, and filtrate obtains Magnesium Carbonate Light 41-45 through pyrolysis.Magnesiumcarbonate is calcined to obtain to magnesium oxide.
Principal reaction equation is as follows:
Calcining: MgCO
3caCO
3→ MgOCaO+2CO
2↑;
Digestion: MgO+CaO+2H
2o → Mg (OH)
2+ Ca (OH)
2;
Carbonization: Mg (OH)
2+ Ca (OH)
2+ 3CO
2→ Mg (HCO
3)
2+ CaCO
3↓+H
2o;
Pyrolysis: Mg (HCO
3)
2+ H
2o → MgCO
33H
2o+CO
2↑;
5(MgCO
3·3H
2O)→4MgCO
3·Mg(OH)
2·4H
2O+10H
2O+CO
2↑。
In carborization, carbonization process is to make magnesium calcium separation key by rhombspar, and carbonization is to make the magnesium of slurry be converted into magnesium solution, and calcium exists with calcium carbonate solid, realizes calcium magnesium separate by the mode of solid-liquid separation.Because carburizing reagent is gas-liquid-solid reaction, process is comparatively complicated, and scientific research personnel, according to the problem of actual production, constantly improves carbonization technique, and carbonization technique is further optimized.Studied scale pressure carbonization method if any people and extracted magnesian technique, scale pressure carbonization method can strengthen the solvability of carbonic acid gas, improves carbonization efficiency, improves CO
2utilization ratio, the content of Magnesium hydrogen carbonate in increase liquid phase.But scale pressure carbonization method is owing to increasing pressure, large to equipment requirements, power consumption increases, the DeGrain that calcium magnesium separates simultaneously, and it is more difficult to promote.Somebody studies the normal pressure secondary carbonization technique of continuous spraying and bubbling combination, secondary carbonization is the calcic heavy magnesium water pyrolysis after carbonization for the first time to be obtained to calcic magnesiumcarbonate carry out carbonization for the second time, calcium deposit in calcic magnesiumcarbonate is got off, the magnesium oxide that preparation purity is 99.2%, but secondary carbonization technique makes Production Flow Chart elongated, energy consumption increases, and carbonizing apparatus drops into higher.Therefore someone proposes rhombspar carbon ammonia double-loop method, this method ammonia precipitation process heavy magnesium water, and by the ammonia still process of digestion section, recycle ammoniacal liquor, has saved the operation of pyrolysis, although this technique is saved pyrolytic process, has reduced a part of energy consumption.But in the ammonia still process of digestion workshop section, ammonia has strong volatility, cause environmental pollution and reduce workman's operability.
In sum, produce Magnesium Carbonate Light 41-45 or magnesium oxide by rhombspar carborization, exist high such as energy consumption, need shortcoming, the especially product purities such as the leaching of secondary strong acid, flow process complexity not high, the magnesiumcarbonate calcic of being produced by rhombspar carborization, calcium carbonate is all higher containing magnesium and other foreign matter content.Result causes magnesium products purity low, and added value of product reduces; The calcium carbonate of being produced by rhombspar carborization cannot effectively use owing to containing a large amount of impurity, has reduced the income of factory.Therefore,, in the urgent need to using novel process novel method that the calcium magnesium of rhombspar is effectively separated, the different calcium magnesium compound product that production purity is higher is simplified technique simultaneously, reduces environmental pollution.
Three, summary of the invention
The present invention is that flow process complexity, is difficult to realize the weak points such as industrialization in order to avoid the existing apparatus expensive of above-mentioned prior art, aim to provide a kind of by dolomite made for light calcium carbonate and method of magnesium oxide.The inventive method raw material is cheap and easy to get, and preparation technology is simple, and flow process is short, environmentally safe, and calcium carbonate purity is high.
The present invention extracts calcium carbonate and magnesium oxide from rhombspar by phase transition-precipitator method, first rhombspar is pulverized to calcining, digestion obtains ash breast, by phase transfer reaction, grey Ruzhong calcium hydroxide is converted into solubility calcium solion, filter out impure magnesium hydroxide filter cake simultaneously, then in solubility calcium solion, pass into CO
2, precipitate and separate obtains calcium carbonate and filtrate, consisting of phase-transferring agent recycling in filtrate.Phase transfer reaction step gained filter cake making beating carbonization obtains magnesium bicarbonate solution, then solves magnesium basic carbonate through Low Temperature Thermal, then the high-temperature calcination of gained magnesium basic carbonate is obtained to light magnesium oxide.The technique that the present invention adopts is simple, less energy consumption, and product purity is high, has good industrial applications prospect.
The present invention is by dolomite made for light calcium carbonate and method of magnesium oxide, and concrete operation step is as follows:
A, calcination reaction
Be 0.5-5mm by rhombspar crushing raw ore to particle diameter, be placed in retort furnace in 950 DEG C of calcining 1.5h, obtain rhombspar ashes, sealing is preserved.The chemical equation of this step is:
MgCO
3·CaCO
3→MgO·CaO+2CO
2↑
The CO that the calcining of this step can be produced
2collect, after purifying compression, be transported in steps d and step e and use.
B, digestion reaction
The rhombspar ashes that step a is obtained is placed in the water of 80-90 DEG C and digests, and liquid-solid ratio is 20mL:1g, and constant temperature stirs 30-60min, and rotating speed is 400r/min, and reaction finishes rear cooling, and ageing 24h, obtains Digestive system; The chemical equation of this step is:
MgO+CaO+2H
2O→Mg(OH)
2+Ca(OH)
2
C, phase transfer reaction
Consisting of phase-transferring agent solution is added in the Digestive system that step b obtains, constant temperature stirring reaction 0.5-2 hour at 25-40 DEG C, rotating speed is 300-500r/min; After reaction finishes, under room temperature, filtering separation obtains solubility calcium solion and filter cake; Represent consisting of phase-transferring agent with NY, the chemical equation of this step is:
Ca(OH)
2+2NY→CaY
2+2NOH
Described consisting of phase-transferring agent is selected from one or more in the sodium salt of glucose, citric acid, sucrose, gluconic acid and gluconic acid or citric acid.
In described consisting of phase-transferring agent and Digestive system, the mol ratio of calcium hydroxide is 1-4:1.
D, carbonization precipitin reaction
By step
cgained solubility calcium solion is heated with stirring to 30-50 DEG C, then in solubility calcium solion, passes into CO with the flow velocity of 60-100mL/min
2, constant temperature stirring reaction 1-3 hour, rotating speed is 400-500r/min; After reaction finishes, ageing 5 hours under room temperature, filtering separation obtains filtrate and filter cake, uses distilled water wash gained filter cake 2-3 time, then the filter cake after washing is obtained to light calcium carbonate for dry 12 hours in 60 DEG C.The phase transition solution that filtrate obtains after removal of impurities can be recycled in step c.The chemical equation of this step is:
CaY
2+CO
2+H
2O→CaCO
3↓+2HY
E, making beating carburizing reagent
By the making beating of step c gained filter cake, concentration is 10g/L (in MgO), then passes into CO with the flow velocity of 60-100mL/min
2, 20-50 DEG C of constant temperature stirring reaction 1-3 hour, rotating speed is 400r/min; After finishing, reaction filters to obtain magnesium bicarbonate solution.The chemical equation of this step is:
Mg(OH)
2+2CO
2→Mg(HCO
3)
2
F, pyrolytic reaction
By step e gained magnesium bicarbonate solution pyrolysis 1-3 hour at 80-100 DEG C, obtain magnesium basic carbonate.The chemical equation of this step is:
5Mg(HCO
3)
2→4MgCO
3·Mg(OH)
2·4H
2O↓+6CO
2↑
G, calcination reaction
Step f gained magnesium basic carbonate, at 700-1000 DEG C of calcining 1-3 hour, is obtained to light magnesium oxide.The chemical equation of this step is:
4MgCO
3·Mg(OH)
2·4H
2O→5MgO+5H
2O↑+4CO
2↑
Compared with prior art, advantage of the present invention shows the following aspects:
1, in the inventive method, utilize phase transfer reaction to realize calcium magnesium and separate, overcome liquid-solid in carborization-gas phase reaction complicated condition, uppity problem, the reaction conditions of phase transition separation method is simple, easy to control, and separation efficiency is higher.
2, technical process of the present invention is short, without " strong acid leaching and the agent of interpolation impurity-removing precipitating ", carbonization precipitation process CO used
2by producing in dolomite calcination process, the CO obtaining after purifying compression
2, avoided CO
2to the secondary pollution of environment, and light calcium carbonate, the magnesium oxide of preparation meets the requirement of national corresponding product standard, for Research foundation has been established in commercial scale production.
3, raw material availability of the present invention is higher, filtrate after the carbonization of solubility calcium solution finishes, the phase transition solution circulated obtaining after removal of impurities is used in phase transition step, filtrate cycle after Magnesium hydrogen carbonate pyrolysis is used in digestion step, all realize recycle, improved the utilization ratio of calcium magnesium raw material and consisting of phase-transferring agent.
Four, brief description of the drawings
Fig. 1 is the X-ray diffraction analysis collection of illustrative plates of rhombspar raw material.As shown in Figure 1, ground dolomite main component is MgCa (CO
3)
2(JCPDS36-0426).
Fig. 2 is the calcium carbonate X-ray diffraction analysis collection of illustrative plates that embodiment 1 obtains.Analyzed from Fig. 2, product is stable calcite type calcium carbonate, and characteristic diffraction peak and standard card (JCPDS05-0586) are substantially identical, and product purity is higher, compound with regular structure.
Fig. 3 is the magnesium oxide X-ray diffraction analysis collection of illustrative plates that embodiment 1 obtains.In Fig. 3, there is the light magnesium oxide characteristic diffraction peak (JCPDS45-0946) of (111), (200), (220), (311) crystal face, baseline is steady, peak type is sharp-pointed, almost occur without assorted peak, illustrate that product is high purity light magnesium oxide.
Fig. 4 is that dolomite made is for nano-calcium carbonate and light magnesium oxide process flow sheet.
Five, embodiment
The rhombspar using in the embodiment of the present invention, its chemical constitution is as shown in table 1:
The chemical constitution of table 1 rhombspar
Composition | CaO | MgO | SiO 2 | T Fe | Al 2O 3 |
Mass percent/% | 29.67 | 21.33 | 5.40 | 0.20 | 0.10 |
Embodiment 1:
In the present embodiment, be to operate as follows by dolomite made for light calcium carbonate and method of magnesium oxide:
A, be 0.5-5mm by rhombspar crushing raw ore to particle diameter, be placed in retort furnace in 950 DEG C of calcining 1.5h, obtain rhombspar ashes, sealing is preserved;
B, the rhombspar ashes that step a is obtained are placed in the water of 80 DEG C and digest, and liquid-solid ratio is 20mL:1g, constant temperature stirring reaction 30min, and rotating speed is 400r/min, and reaction finishes rear cooling, and ageing 24h, obtains Digestive system;
C, sodium gluconate solution is added in the Digestive system that step b obtains, in Sunmorl N 60S and Digestive system, the mol ratio of calcium is 1:1, constant temperature stirring reaction 0.7 hour at 25 DEG C, and rotating speed is 400r/min; After reaction finishes, under room temperature, filtering separation obtains solubility calcium solion and filter cake;
D, step c gained solubility calcium solion is heated with stirring to 30 DEG C, then in solubility calcium solion, passes into CO with the flow velocity of 100mL/min
2, constant temperature stirring reaction 1 hour, rotating speed is 500r/min; After reaction finishes, ageing 5 hours under room temperature, filtering separation obtains filtrate and filter cake, uses distilled water wash gained filter cake 3 times, then the filter cake after washing is obtained to light calcium carbonate for dry 12 hours in 60 DEG C;
E, by step c gained filter cake making beating, concentration is 10g/L (MgO), then passes into CO with the flow velocity of 100mL/min
2, 20 DEG C of constant temperature stirring reactions 1 hour, rotating speed is 400r/min, after reaction finishes, filters to obtain magnesium bicarbonate solution;
F, by the pyrolysis 1 hour at 100 DEG C of step e gained magnesium bicarbonate solution, obtain magnesium basic carbonate;
G, by step f gained magnesium basic carbonate 900 DEG C calcining 1 hour, obtain light magnesium oxide.
The present embodiment calcium ion yield is 92.2%, and calcium carbonate sample purity is 98.2%, and whiteness is 98.0, and light magnesium oxide productive rate is 81.5%.
Fig. 1 is the X-ray diffraction analysis collection of illustrative plates of rhombspar raw material, and as shown in Figure 1, ground dolomite main component is MgCa (CO
3)
2(JCPDS36-0426).Fig. 2 is the X-ray diffraction analysis collection of illustrative plates that makes light calcium carbonate, is analyzed from Fig. 2, and product is stable calcite type calcium carbonate, and characteristic diffraction peak and standard card (JCPDS05-0586) are substantially identical, and product purity is higher, compound with regular structure.Fig. 3 is the magnesian X diffraction analysis collection of illustrative plates obtaining after magnesium basic carbonate calcining, in Fig. 3, there is the light magnesium oxide characteristic diffraction peak (JCPDS45-0946) of (111), (200), (220), (311) crystal face, baseline is steady, peak type is sharp-pointed, almost occur without assorted peak, illustrate that product is high purity light magnesium oxide.
Embodiment 2:
In the present embodiment, be to operate as follows by dolomite made for light calcium carbonate and method of magnesium oxide:
A, be 0.5-5mm by rhombspar crushing raw ore to particle diameter, be placed in retort furnace in 950 DEG C of calcining 1.5h, obtain rhombspar ashes, sealing is preserved;
B, the rhombspar ashes that step a is obtained are placed in the water of 85 DEG C and digest, and liquid-solid ratio is 20mL:1g, constant temperature stirring reaction 40min, and rotating speed is 400r/min, and reaction finishes rear cooling, and ageing 24h, obtains Digestive system;
C, sucrose solution is added in the Digestive system that step b obtains, in sucrose and Digestive system, the mol ratio of calcium is 1.5:1, constant temperature stirring reaction 0.8 hour at 30 DEG C, and rotating speed is 500r/min; After reaction finishes, under room temperature, filtering separation obtains solubility calcium solion and filter cake;
D, step c gained solubility calcium solion is heated with stirring to 35 DEG C, then in solubility calcium solion, passes into CO with the flow velocity of 90mL/min
2, constant temperature stirring reaction 1 hour, rotating speed is 400r/min; After reaction finishes, ageing 5 hours under room temperature, filtering separation obtains filtrate and filter cake, uses distilled water wash gained filter cake 3 times, then the filter cake after washing is obtained to light calcium carbonate for dry 12 hours in 60 DEG C;
E, by step c gained filter cake making beating, concentration is 10g/L (MgO), then passes into CO with the flow velocity of 90mL/min
2, 25 DEG C of constant temperature stirring reactions 1.5 hours, rotating speed is 400r/min, after reaction finishes, filters to obtain magnesium bicarbonate solution;
F, by the pyrolysis 1 hour at 90 DEG C of step e gained magnesium bicarbonate solution, obtain magnesium basic carbonate;
G, by step f gained magnesium basic carbonate 1000 DEG C calcining 1 hour, obtain light magnesium oxide.
The present embodiment calcium ion yield is 93.2%, and calcium carbonate sample purity is 98.0%, and whiteness is 99.1, and light magnesium oxide productive rate is 79.3%.
Embodiment 3:
In the present embodiment, be to operate as follows by dolomite made for light calcium carbonate and method of magnesium oxide:
A, be 0.5-5mm by rhombspar crushing raw ore to particle diameter, be placed in retort furnace in 950 DEG C of calcining 1.5h, obtain rhombspar ashes, sealing is preserved;
B, the rhombspar ashes that step a is obtained are placed in the water of 90 DEG C and digest, and liquid-solid ratio is 20mL:1g, constant temperature stirring reaction 60min, and rotating speed is 400r/min, and reaction finishes rear cooling, and ageing 24h, obtains Digestive system;
C, sodium citrate solution is added in the Digestive system that step b obtains, in Trisodium Citrate and Digestive system, the mol ratio of calcium is 4:1, constant temperature stirring reaction 1 hour at 35 DEG C, and rotating speed is 300r/min; After reaction finishes, under room temperature, filtering separation obtains solubility calcium solion and filter cake;
D, step c gained solubility calcium solion is heated with stirring to 35 DEG C, then in solubility calcium solion, passes into CO with the flow velocity of 70mL/min
2, constant temperature stirring reaction 2 hours, rotating speed is 400r/min; After reaction finishes, ageing 5 hours under room temperature, filtering separation obtains filtrate and filter cake, uses distilled water wash gained filter cake 3 times, then the filter cake after washing is obtained to light calcium carbonate for dry 12 hours in 60 DEG C;
E, by step c gained filter cake making beating, concentration is 10g/L (MgO), then passes into CO with the flow velocity of 70mL/min
2, 30 DEG C of constant temperature stirring reactions 2 hours, rotating speed is 400r/min, after reaction finishes, filters to obtain magnesium bicarbonate solution;
F, by the pyrolysis 1.5 hours at 90 DEG C of step e gained magnesium bicarbonate solution, obtain magnesium basic carbonate;
G, by step f gained magnesium basic carbonate 800 DEG C calcining 2 hours, obtain light magnesium oxide.
The present embodiment calcium ion yield is 88.2%, and calcium carbonate sample purity is 97.8%, and whiteness is 97.3, and macroscopical light magnesium oxide productive rate is 77.1%.
Embodiment 4:
In the present embodiment, be to operate as follows by dolomite made for light calcium carbonate and method of magnesium oxide:
A, be 0.5-5mm by rhombspar crushing raw ore to particle diameter, be placed in retort furnace in 950 DEG C of calcining 1.5h, obtain rhombspar ashes, sealing is preserved;
B, the rhombspar ashes that step a is obtained are placed in the water of 85 DEG C and digest, and liquid-solid ratio is 20mL:1g, constant temperature stirring reaction 60min, and rotating speed is 400r/min, and reaction finishes rear cooling, and ageing 24h, obtains Digestive system;
C, glucose solution is added in the Digestive system that step b obtains, in glucose and Digestive system, the mol ratio of calcium is 3:1, constant temperature stirring reaction 2 hours at 40 DEG C, and rotating speed is 450r/min; After reaction finishes, under room temperature, filtering separation obtains solubility calcium solion and filter cake;
D, step c gained solubility calcium solion is heated with stirring to 40 DEG C, then in solubility calcium solion, passes into CO with the flow velocity of 60mL/min
2, constant temperature stirring reaction 3 hours, rotating speed is 400r/min; After reaction finishes, ageing 5 hours under room temperature, filtering separation obtains filtrate and filter cake, uses distilled water wash gained filter cake 3 times, then the filter cake after washing is obtained to light calcium carbonate for dry 12 hours in 60 DEG C;
E, by step c gained filter cake making beating, concentration is 10g/L (MgO), then passes into CO with the flow velocity of 60mL/min
2, 50 DEG C of constant temperature stirring reactions 3 hours, rotating speed is 400r/min, after reaction finishes, filters to obtain magnesium bicarbonate solution;
F, by the pyrolysis 3 hours at 80 DEG C of step e gained magnesium bicarbonate solution, obtain magnesium basic carbonate;
G, by step f gained magnesium basic carbonate 700 DEG C calcining 3 hours, obtain light magnesium oxide.
The present embodiment calcium ion yield is 90.5%, and calcium carbonate sample purity is 98.1%, and whiteness is 97.2, and light magnesium oxide productive rate is 82.7%.
Claims (4)
- By dolomite made for light calcium carbonate and a method of magnesium oxide, it is characterized in that:First dolomite calcination, digestion are obtained to Digestive system, by phase transfer reaction, calcium hydroxide in Digestive system is converted into solubility calcium solion, filter out impure magnesium hydroxide filter cake simultaneously, then in solubility calcium solion, pass into CO 2, precipitate and separate obtains calcium carbonate and filtrate; Impure magnesium hydroxide filter cake making beating carbonization is obtained to magnesium bicarbonate solution, then obtain magnesium basic carbonate through pyrolytic reaction, after calcining, obtain light magnesium oxide.
- 2. method according to claim 1, is characterized in that comprising the following steps:A, calcination reactionBe 0.5-5mm by rhombspar crushing raw ore to particle diameter, be placed in retort furnace in 950 DEG C of calcining 1.5h, obtain rhombspar ashes, sealing is preserved;B, digestion reactionThe rhombspar ashes that step a is obtained is placed in the water of 80-90 DEG C and digests, and liquid-solid ratio is 20mL:1g, constant temperature stirring reaction 30-60min, and reaction finishes rear cooling, and ageing 24h, obtains Digestive system;C, phase transfer reactionConsisting of phase-transferring agent solution is added in the Digestive system that step b obtains, constant temperature stirring reaction 0.5-2 hour at 25-40 DEG C, after reaction finishes, under room temperature, filtering separation obtains solubility calcium solion and filter cake;D, carbonization precipitin reactionStep c gained solubility calcium solion is heated with stirring to 20-50 DEG C, then in solubility calcium solion, passes into CO with the flow velocity of 60-100mL/min 2, constant temperature stirring reaction 1-3 hour; After reaction finishes, ageing 5 hours under room temperature, filtering separation obtains filtrate and filter cake, uses distilled water wash gained filter cake 2-3 time, then the filter cake after washing is obtained to light calcium carbonate for dry 12 hours in 60 DEG C;E, making beating carburizing reagentBy the making beating of step c gained filter cake, controlled concentration is 10g/L, then passes into CO with the flow velocity of 60-100mL/min 2, 20-50 DEG C of constant temperature stirring reaction 1-3 hour, filters to obtain magnesium bicarbonate solution after reaction finishes;F, pyrolytic reactionBy step e gained magnesium bicarbonate solution pyrolysis 1-3 hour at 80-100 DEG C, obtain magnesium basic carbonate;G, calcination reactionStep f gained magnesium basic carbonate, at 700-1000 DEG C of calcining 1-3 hour, is obtained to light magnesium oxide.
- 3. method according to claim 2, is characterized in that:Consisting of phase-transferring agent described in step c is selected from one or more in the sodium salt of glucose, citric acid, sucrose, gluconic acid and gluconic acid or citric acid.
- 4. it is characterized in that according to the method in claim 2 or 3:In consisting of phase-transferring agent described in step c and described Digestive system, the mol ratio of calcium hydroxide is 1-4:1.
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