CN114702052A - Method for producing light magnesium carbonate by using byproduct magnesium hydroxide - Google Patents
Method for producing light magnesium carbonate by using byproduct magnesium hydroxide Download PDFInfo
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- CN114702052A CN114702052A CN202210568198.8A CN202210568198A CN114702052A CN 114702052 A CN114702052 A CN 114702052A CN 202210568198 A CN202210568198 A CN 202210568198A CN 114702052 A CN114702052 A CN 114702052A
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- magnesium
- magnesium hydroxide
- activated carbon
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- slurry
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 71
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 71
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 71
- 239000006227 byproduct Substances 0.000 title claims abstract description 62
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 62
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical class [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 50
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000292 calcium oxide Substances 0.000 claims abstract description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 124
- 239000002002 slurry Substances 0.000 claims description 59
- 238000003756 stirring Methods 0.000 claims description 59
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 54
- 238000002386 leaching Methods 0.000 claims description 54
- 239000008367 deionised water Substances 0.000 claims description 50
- 229910021641 deionized water Inorganic materials 0.000 claims description 50
- 239000011777 magnesium Substances 0.000 claims description 48
- 229910052749 magnesium Inorganic materials 0.000 claims description 48
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 27
- 239000012065 filter cake Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 25
- 239000011347 resin Substances 0.000 claims description 25
- 229920005989 resin Polymers 0.000 claims description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 238000003825 pressing Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000000113 methacrylic resin Substances 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 238000000746 purification Methods 0.000 claims description 12
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 11
- -1 polydimethylsiloxane Polymers 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 10
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 10
- 238000001694 spray drying Methods 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 9
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 9
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 9
- 239000001099 ammonium carbonate Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 abstract description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- UOVKYUCEFPSRIJ-UHFFFAOYSA-D hexamagnesium;tetracarbonate;dihydroxide;pentahydrate Chemical compound O.O.O.O.O.[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O UOVKYUCEFPSRIJ-UHFFFAOYSA-D 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 229940072033 potash Drugs 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/24—Magnesium carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
-
- 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
- C01F5/14—Magnesium hydroxide
- C01F5/145—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for producing light magnesium carbonate by using by-product magnesium hydroxide, belonging to the field of magnesium metal compounds. The light magnesium carbonate produced by the invention has high content of magnesium oxide and less impurities, the content of magnesium oxide in the product is 43.0-43.5wt%, the content of calcium oxide is 0.1-0.2wt%, the content of acid insoluble substances is 0.10-0.12wt%, the content of iron is 0.01-0.02wt%, the content of chlorine radical is 0.08-0.09wt%, the bulk density is 0.15-0.16g/mL, and the content of water is 2.4-2.5 wt%.
Description
Technical Field
The invention relates to a method for producing light magnesium carbonate by using byproduct magnesium hydroxide, belonging to the field of magnesium metal compounds.
Background
The Qinghai is a great province of salt lake resources, the salt lake is distributed throughout the Chaida basin, and the magnesium resource reserve which is only proved accounts for more than 90 percent of the total magnesium resource amount in China. For a long time, the development of the resource of the salt lake of the faaidam is mainly to extract lithium and produce potash fertilizer, and a large amount of by-product magnesium hydroxide can be produced while extracting lithium and producing potash fertilizer, which is called as 'magnesium harm'.
The national advocates that the Qinghai province not only needs to produce products with high added values such as lithium and boron in the process of brine extraction, but also strictly controls the emission of magnesium, but because the purity of the byproduct magnesium hydroxide is low, the impurity ions are of various types, and cannot be directly utilized and are abandoned by most enterprises, the environmental pollution is caused, the resource waste is caused, and the green recycling economy advocated by China is not met, so that the problem to be urgently solved is how to realize the comprehensive utilization of the byproduct magnesium hydroxide.
The light magnesium carbonate is also called as hydrated basic magnesium carbonate, is usually prepared by an ore method or a brine method, and has no report of a process for directly producing the hydrated basic magnesium carbonate by using a byproduct magnesium hydroxide, wherein a large amount of crude magnesium hydroxide which is a byproduct magnesium hydroxide generated in a lithium extraction process is generated as a byproduct, the content of the magnesium hydroxide is low and is about 70 percent, the content of the magnesium hydroxide can only reach about 93 percent after refining pretreatment, the chlorine radical is about 1.5 percent, the content of the borate is about 4 percent, the hydrated basic magnesium carbonate produced by using the byproduct hydrogen magnesium oxide after refining pretreatment can not reach the standard, the content of the magnesium oxide is low, the impurity content is high, and the application value of the hydrated basic magnesium carbonate can not be exerted.
In conclusion, the prior art can not produce light magnesium carbonate meeting the standard by using the byproduct magnesium hydroxide, and the produced light magnesium carbonate has low magnesium oxide content and high impurity content.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and the light magnesium carbonate is further produced by purifying the byproduct magnesium oxide twice and leaching the byproduct magnesium oxide twice, so that the light magnesium carbonate has high magnesium oxide content and less impurities.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for producing light magnesium carbonate by using by-product magnesium hydroxide comprises the steps of crushing, primary purification, secondary purification, synthesis reaction, leaching, filter pressing and drying the by-product magnesium hydroxide;
the following is a further improvement of the above technical solution:
the method for crushing the byproduct magnesium hydroxide comprises the steps of crushing the byproduct magnesium hydroxide dry filter cake to the fineness of 180-250 meshes to obtain byproduct magnesium hydroxide fine powder;
the water content of the by-product magnesium hydroxide dry filter cake is 23-28wt%, and the solid content is 72-77 wt%;
the indexes of the solid in the byproduct magnesium hydroxide dry filter cake are as follows: 93.6 to 93.8 weight percent of magnesium hydroxide, 0.30 to 0.32 weight percent of calcium oxide, 0.28 to 0.30 weight percent of acid insoluble substance, 0.03 to 0.06 weight percent of iron, 1.32 to 1.5 weight percent of chlorine radical and 3.9 to 4.1 weight percent of borate;
the primary purification method comprises the steps of mixing the byproduct magnesium hydroxide fine powder with deionized water to obtain magnesium slurry, adding caustic soda flakes and ethylene glycol, heating to 90-95 ℃, stirring at the speed of 300-400r/min for 1.8-2.5h to obtain primary purified magnesium slurry;
the mass ratio of the byproduct magnesium hydroxide fine powder to the deionized water is 6: 18-22;
the mass ratio of the caustic soda flakes to the deionized water is 1: 95-105;
the mass ratio of the ethylene glycol to the deionized water is 1: 95-105;
mixing the activated carbon loaded resin with the primary purified magnesium slurry, heating to 50-60 ℃, stirring at the speed of 400-;
the mass ratio of the activated carbon loaded resin to the primarily purified magnesium slurry is 1: 45-55;
the indexes of the solid in the purified magnesium slurry are as follows: 97.3 to 97.6 weight percent of magnesium hydroxide, 0.16 to 0.21 weight percent of calcium chloride, 0.2 to 0.23 weight percent of acid insoluble substance, 0.03 to 0.05 weight percent of iron, 1.18 to 1.24 weight percent of chlorine radical and 0.6 to 0.8 weight percent of borate.
The preparation method of the activated carbon loaded resin comprises the steps of preparing expanded activated carbon and loaded resin;
the preparation method of the expanded activated carbon comprises the steps of crushing activated carbon powder to the fineness of 80-120 meshes, mixing the crushed activated carbon with sodium bicarbonate, sending the mixture into a high-pressure homogenizer, carrying out high-pressure homogenization treatment under the pressure of 23-27MPa for 25-40min to obtain a mixture, dropwise adding a hydrochloric acid aqueous solution into the mixture, stirring at the speed of 150-250r/min while dropwise adding the hydrochloric acid aqueous solution, stirring at the speed of 300-400r/min after the hydrochloric acid aqueous solution is added, stirring for 25-40min, standing, filtering and drying to obtain the expanded activated carbon;
the aperture of the activated carbon is 22000-25000 nm;
the dropping speed of the hydrochloric acid aqueous solution is that the hydrochloric acid aqueous solution accounting for 3-7wt% of the mixture is added every minute, and the dropping time is 85-200 min;
the mass ratio of the crushed active carbon to the sodium bicarbonate is 1: 20-30;
the mass concentration of the hydrochloric acid aqueous solution is 18-22%;
mixing expanded activated carbon with ethyl acetate, adding methacrylic resin, heating to 50-60 ℃, stirring at the speed of 1400-1600r/min for 30-40min, then carrying out ultrasonic treatment at the frequency of 75-85kHz for 10-20min to obtain a negative carrier liquid after the ultrasonic treatment is finished, standing the load liquid for 15-25min, and carrying out spray drying in a vacuum environment of 18-25Pa to obtain activated carbon loaded resin;
the mass ratio of the expanded activated carbon to the ethyl acetate is 1: 9-11;
the mass ratio of the methacrylic resin to the expanded activated carbon is 2.5-3.5: 2;
the molecular weight of the methacrylic resin is 15000-25000;
the temperature of the spray drying is 75-90 ℃.
Adding purified magnesium slurry into deionized water, adjusting the temperature to be 35-39 ℃, adding ammonium bicarbonate, stirring at the speed of 200-300r/min for 13-20min, adjusting the temperature to be 55-65 ℃ after stirring, and preserving heat to obtain light magnesium carbonate slurry;
the volume ratio of the purified magnesium slurry to the deionized water is 10: 20-30;
the carbonThe mass-volume ratio of the ammonium to the purified magnesium slurry is 2.3-3t:10m3;
The leaching and filter pressing comprises one-step leaching, two-step leaching and filter pressing;
the one-step leaching method comprises the steps of pumping the light magnesium carbonate slurry with the temperature of 55-65 ℃ after heat preservation into a filter, and introducing deionized water with the temperature of 55-65 ℃ for leaching to obtain a one-step leaching product;
the volume ratio of the light magnesium carbonate slurry to the deionized water is 12: 38-45;
the two-step leaching and filter pressing method comprises the steps of preserving heat of the one-step leaching object in a filter, keeping the temperature at 55-65 ℃, leaching the one-step leaching object by using the mixed solution at 55-65 ℃, and squeezing after leaching to obtain a light magnesium carbonate filter cake;
the mass ratio of the one-step showering washing matter to the mixed liquid is 1: 18-25;
the mixed solution comprises the following components in parts by mass: 800-1200 parts of deionized water, 2-4 parts of polydimethylsiloxane, 4-6 parts of aqueous hydrogen peroxide and 7-13 parts of absolute ethyl alcohol;
the mass concentration of the aqueous hydrogen peroxide solution is 20-30%;
the preparation method of the mixed solution comprises the steps of mixing polydimethylsiloxane and absolute ethyl alcohol, stirring at the speed of 400-600r/min for 15-25min, adding deionized water and aqueous hydrogen peroxide, stirring at the speed of 400-600r/min for 25-35min, and stirring to obtain the mixed solution.
The drying method comprises the steps of drying the light magnesium carbonate filter cake at the temperature of 150-170 ℃ until the water content is 2.4-2.6wt% to obtain the light magnesium carbonate.
Compared with the prior art, the invention has the following beneficial effects:
the light magnesium carbonate produced by the invention has high content of magnesium oxide and less impurities, the content of magnesium oxide in the product is 43.0-43.5wt%, the content of calcium oxide is 0.1-0.2wt%, the content of acid insoluble substances is 0.10-0.12wt%, the content of iron is 0.01-0.02wt%, the content of chlorine radical is 0.08-0.09wt%, the bulk density is 0.15-0.16g/mL, and the content of water is 2.4-2.5 wt%.
Detailed Description
Example 1
(1) Pulverizing byproduct magnesium hydroxide
Crushing the by-product magnesium hydroxide dry filter cake to the fineness of 200 meshes to obtain by-product magnesium hydroxide fine powder;
the water content of the by-product magnesium hydroxide dry filter cake is 25wt%, and the solid content is 75 wt%;
the indexes of the solid in the byproduct magnesium hydroxide dry filter cake are as follows: 93.7wt% of magnesium hydroxide, 0.31wt% of calcium oxide, 0.29wt% of acid-insoluble matter, 0.05wt% of iron, 1.5wt% of chloride and 4wt% of borate.
(2) Primary purification
Mixing the byproduct magnesium hydroxide fine powder with deionized water to obtain magnesium slurry, adding caustic soda flakes and ethylene glycol, heating to 92 ℃, stirring at the speed of 350r/min for 2 hours to obtain primary purified magnesium slurry;
the mass ratio of the byproduct magnesium hydroxide fine powder to the deionized water is 6: 20;
the mass ratio of the caustic soda flakes to the deionized water is 1: 100;
the mass ratio of the ethylene glycol to the deionized water is 1: 100;
(3) secondary purification
Mixing the activated carbon loaded resin with the primary purified magnesium slurry, heating to 55 ℃, stirring at the speed of 450r/min for 4 hours, and filtering through a 200-mesh screen after stirring to obtain purified magnesium slurry;
the mass ratio of the activated carbon loaded resin to the primarily purified magnesium slurry is 1: 50;
the indexes of the solid matters in the purified magnesium slurry are as follows: 97.5wt% of magnesium hydroxide, 0.2wt% of calcium oxide, 0.2wt% of acid-insoluble matter, 0.05wt% of iron, 1.2wt% of chloride, and 0.8wt% of borate.
The preparation method of the activated carbon loaded resin comprises the following steps:
a. preparation of expanded activated carbon
Crushing activated carbon powder to the fineness of 100 meshes, mixing the crushed activated carbon with sodium bicarbonate, feeding the mixture into a high-pressure homogenizer, carrying out high-pressure homogenization treatment under the pressure of 25MPa for 30min to obtain a mixture, slowly dropwise adding a hydrochloric acid aqueous solution into the mixture, stirring at the speed of 200r/min while dropwise adding, stirring at the speed of 350r/min after the hydrochloric acid aqueous solution is added, stirring for 30min, standing for 20min, filtering and drying to obtain expanded activated carbon;
the aperture of the active carbon is 23000 nm;
the adding speed of the hydrochloric acid aqueous solution is that the hydrochloric acid aqueous solution accounting for 5wt% of the mixture is added every minute, and the dropping time is 120 min;
the mass ratio of the crushed active carbon to the sodium bicarbonate is 1: 25;
the mass concentration of the hydrochloric acid aqueous solution is 20%;
b. supported resin
Mixing expanded activated carbon and ethyl acetate, adding methacrylic resin, heating to 55 ℃, stirring at the speed of 1500r/min for 35min, performing ultrasonic treatment at the frequency of 80kHz for 15min to obtain a negative carrier liquid after the ultrasonic treatment is finished, standing the load liquid for 20min, and performing spray drying in a vacuum environment of 20Pa to obtain activated carbon loaded resin;
the mass ratio of the expanded activated carbon to the ethyl acetate is 1: 10;
the mass ratio of the methacrylic resin to the expanded activated carbon is 3: 2;
the molecular weight of the methacrylic resin is 20000;
the temperature of the spray drying was 80 ℃.
(4) Synthesis reaction
Adding the purified magnesium slurry into deionized water, adjusting the temperature to be 37 ℃, adding ammonium bicarbonate, stirring at the speed of 250r/min for 15min, adjusting the temperature to be 60 ℃ after stirring, and preserving the heat for 60min to obtain light magnesium carbonate slurry;
the volume ratio of the purified magnesium slurry to the deionized water is 10: 25;
the mass volume ratio of the ammonium bicarbonate to the purified magnesium slurry is 2.5 t:10m3;
(5) Leaching and filter pressing
a. One-step leaching
Pumping the light magnesium carbonate slurry with the temperature of 60 ℃ after heat preservation into a filter, and introducing deionized water with the temperature of 60 ℃ for leaching to obtain a one-step leaching product;
the volume ratio of the light magnesium carbonate slurry to the deionized water is 12: 40;
b. two-step leaching and filter pressing
Keeping the temperature of the one-step leaching object in a filter at 60 ℃, leaching the one-step leaching object by using a mixed solution at 60 ℃, leaching and squeezing to obtain a light magnesium carbonate filter cake;
the mass ratio of the one-step showering and washing matter to the mixed solution is 1: 20;
the mixed solution comprises the following components in parts by mass: 1000 parts of deionized water, 3 parts of polydimethylsiloxane, 5 parts of aqueous hydrogen peroxide solution and 10 parts of absolute ethyl alcohol;
the mass concentration of the aqueous hydrogen peroxide solution is 25 percent;
the preparation method of the mixed liquid comprises the steps of mixing polydimethylsiloxane and absolute ethyl alcohol, stirring at the speed of 500r/min for 20min, adding deionized water and aqueous hydrogen peroxide, stirring at the speed of 500r/min for 30min, and stirring to obtain the mixed liquid.
(6) Drying by baking
And drying the light magnesium carbonate filter cake at 160 ℃, and drying until the water content is 2.5wt% to obtain the light magnesium carbonate.
Example 2
(1) Pulverizing byproduct magnesium hydroxide
Crushing the by-product magnesium hydroxide dry filter cake to the fineness of 180 meshes to obtain by-product magnesium hydroxide fine powder;
the water content of the by-product magnesium hydroxide dry filter cake is 23wt%, and the solid content is 77 wt%;
the indexes of the solid in the byproduct magnesium hydroxide dry filter cake are as follows: 93.6wt% of magnesium hydroxide, 0.32wt% of calcium oxide, 0.28wt% of acid-insoluble matter, 0.06wt% of iron, 1.45wt% of chloride and 3.9wt% of borate.
(2) Primary purification
Mixing the byproduct magnesium hydroxide fine powder with deionized water to obtain magnesium slurry, adding caustic soda flakes and ethylene glycol, heating to 90 ℃, stirring at the speed of 300r/min for 2.5 hours to obtain primary purified magnesium slurry;
the mass ratio of the byproduct magnesium hydroxide fine powder to the deionized water is 6: 18;
the mass ratio of the caustic soda flakes to the deionized water is 1: 95;
the mass ratio of the ethylene glycol to the deionized water is 1: 95;
(3) secondary purification
Mixing the activated carbon loaded resin with the primary purified magnesium slurry, heating to 50 ℃, stirring at the speed of 500r/min for 3.5 hours, and filtering through a 200-mesh screen after stirring to obtain purified magnesium slurry;
the mass ratio of the activated carbon loaded resin to the primarily purified magnesium slurry is 1: 45;
the indexes of the solid matters in the purified magnesium slurry are as follows: the content of magnesium hydroxide was 97.3wt%, the content of calcium oxide was 0.16wt%, the content of acid-insoluble matter was 0.23wt%, the content of iron was 0.04wt%, the content of chloride was 1.24wt%, and the content of borate was 0.7 wt%.
The preparation method of the activated carbon loaded resin comprises the following steps:
a. preparation of expanded activated carbon
Crushing the activated carbon into 80-mesh powder, mixing the crushed activated carbon with sodium bicarbonate, feeding the mixture into a high-pressure homogenizer, carrying out high-pressure homogenization treatment under the pressure of 23MPa for 40min to obtain a mixture, slowly dropwise adding a hydrochloric acid aqueous solution into the mixture, stirring at the speed of 150r/min while dropwise adding, stirring at the speed of 300r/min after the hydrochloric acid aqueous solution is added, stirring for 40min, standing for 15min, filtering and drying to obtain expanded activated carbon;
the aperture of the active carbon is 22000 nm;
the addition speed of the hydrochloric acid aqueous solution is as follows: adding hydrochloric acid aqueous solution accounting for 3wt% of the mixture every minute, and dropwise adding for 200 min;
the mass ratio of the crushed active carbon to the sodium bicarbonate is 1: 20;
the mass concentration of the hydrochloric acid aqueous solution is 18%;
b. supported resin
Mixing expanded activated carbon and ethyl acetate, adding methacrylic resin, heating to 50 ℃, stirring at the speed of 1600r/min for 30min, performing ultrasonic treatment at the frequency of 75kHz for 20min to obtain a negative carrier liquid after the ultrasonic treatment is finished, standing the load liquid for 15min, and performing spray drying in a vacuum environment of 18Pa to obtain activated carbon loaded resin;
the mass ratio of the expanded activated carbon to the ethyl acetate is 1: 9;
the mass ratio of the methacrylic resin to the expanded activated carbon is 2.5: 2;
the molecular weight of the methacrylic resin is 15000;
the temperature of the spray drying was 75 ℃.
(4) Synthesis reaction
Adding the purified magnesium slurry into deionized water, adjusting the temperature to 35 ℃, adding ammonium bicarbonate, stirring at the speed of 200r/min for 20min, adjusting the temperature to 55 ℃ after stirring, and keeping the temperature for 65min to obtain light magnesium carbonate slurry;
the volume ratio of the purified magnesium slurry to the deionized water is 10: 20;
the mass volume ratio of the ammonium bicarbonate to the purified magnesium slurry is 2.3t:10m3;
(5) Leaching and filter pressing
a. One-step leaching
Pumping the light magnesium carbonate slurry with the temperature of 55 ℃ after heat preservation into a filter, and introducing deionized water with the temperature of 55 ℃ for leaching to obtain a one-step leaching product;
the volume ratio of the light magnesium carbonate slurry to the deionized water is 12: 38;
b. two-step leaching and filter pressing
Keeping the temperature of the one-step leaching object in a filter at 55 ℃, leaching the one-step leaching object by using a mixed solution at 55 ℃, leaching and squeezing to obtain a light magnesium carbonate filter cake;
the mass ratio of the one-step showering washing matter to the mixed liquid is 1: 18;
the mixed solution comprises the following components in parts by mass: 800 parts of deionized water, 2 parts of polydimethylsiloxane, 4 parts of aqueous hydrogen peroxide solution and 7 parts of absolute ethyl alcohol;
the mass concentration of the aqueous hydrogen peroxide solution is 30 percent;
the preparation method of the mixed liquid comprises the steps of mixing polydimethylsiloxane and absolute ethyl alcohol, stirring at the speed of 400r/min for 25min, adding deionized water and aqueous hydrogen peroxide, stirring at the speed of 400r/min for 35min, and stirring to obtain the mixed liquid.
(6) Drying by baking
And drying the light magnesium carbonate filter cake at 150 ℃, and drying until the water content is 2.4wt% to obtain the light magnesium carbonate.
Example 3
(1) Pulverizing byproduct magnesium hydroxide
Crushing the by-product magnesium hydroxide dry filter cake to the fineness of 250 meshes to obtain by-product magnesium hydroxide fine powder;
the water content of the by-product magnesium hydroxide dry filter cake is 28wt%, and the solid content is 72 wt%;
the indexes of the solid in the byproduct magnesium hydroxide dry filter cake are as follows: 93.8wt% of magnesium hydroxide, 0.30wt% of calcium oxide, 0.30wt% of acid-insoluble matter, 0.03wt% of iron, 1.32wt% of chloride and 4.1wt% of borate.
(2) Primary purification
Mixing the byproduct magnesium hydroxide fine powder with deionized water to obtain magnesium slurry, adding caustic soda flakes and ethylene glycol, heating to 95 ℃, stirring at the speed of 400r/min for 1.8h to obtain primary purified magnesium slurry;
the mass ratio of the byproduct magnesium hydroxide fine powder to the deionized water is 6: 22;
the mass ratio of the caustic soda flakes to the deionized water is 1: 105;
the mass ratio of the ethylene glycol to the deionized water is 1: 105;
(3) secondary purification
Mixing the activated carbon loaded resin with the primary purified magnesium slurry, heating to 60 ℃, stirring at the speed of 400r/min for 4.5 hours, and filtering through a 200-mesh screen after stirring to obtain purified magnesium slurry;
the mass ratio of the activated carbon loaded resin to the primarily purified magnesium slurry is 1: 55;
the indexes of the solid matters in the purified magnesium slurry are as follows: the content of magnesium hydroxide was 97.6wt%, the content of calcium oxide was 0.21wt%, the content of acid-insoluble matter was 0.21wt%, the content of iron was 0.03wt%, the content of chloride was 1.18wt%, and the content of borate was 0.6 wt%.
The preparation method of the activated carbon loaded resin comprises the following steps:
a. preparation of expanded activated carbon
Crushing activated carbon powder to a fineness of 120 meshes, mixing the crushed activated carbon with sodium bicarbonate, feeding the mixture into a high-pressure homogenizer, carrying out high-pressure homogenization treatment under a pressure of 27MPa for 25min to obtain a mixture, slowly dropwise adding a hydrochloric acid aqueous solution into the mixture, stirring at a speed of 250r/min while dropwise adding, stirring at a speed of 400r/min after the hydrochloric acid aqueous solution is added, stirring for 25min, standing for 25min, filtering, and drying to obtain expanded activated carbon;
the aperture of the activated carbon is 25000 nm;
the addition speed of the hydrochloric acid aqueous solution is as follows: adding hydrochloric acid aqueous solution 7wt% of the mixture every minute, and dripping for 85 min;
the mass ratio of the crushed active carbon to the sodium bicarbonate is 1: 30;
the mass concentration of the hydrochloric acid aqueous solution is 22%;
b. supported resin
Mixing expanded activated carbon and ethyl acetate, adding methacrylic resin, heating to 60 ℃, stirring at the speed of 1400r/min for 40min, then carrying out ultrasonic treatment at the frequency of 85kHz for 10min to obtain a negative carrier liquid after the ultrasonic treatment is finished, standing and standing the load liquid for 25min, and carrying out spray drying in a vacuum environment of 25Pa to obtain activated carbon load resin;
the mass ratio of the expanded activated carbon to the ethyl acetate is 1: 11;
the mass ratio of the methacrylic resin to the expanded activated carbon is 3.5: 2;
the molecular weight of the methacrylic resin is 25000;
the temperature of the spray drying was 90 ℃.
(4) Synthesis reaction
Adding the purified magnesium slurry into deionized water, adjusting the temperature to 39 ℃, adding ammonium bicarbonate, stirring at the speed of 300r/min for 13min, adjusting the temperature to 65 ℃ after stirring, and keeping the temperature for 55min to obtain light magnesium carbonate slurry;
the volume ratio of the purified magnesium slurry to the deionized water is 10: 30;
the mass volume ratio of the ammonium bicarbonate to the purified magnesium slurry is 3t:10m3;
(5) Leaching and filter pressing
a. One-step leaching
Pumping the light magnesium carbonate slurry with the temperature of 65 ℃ after heat preservation into a filter, and introducing deionized water with the temperature of 65 ℃ for leaching to obtain a one-step leaching product;
the volume ratio of the light magnesium carbonate slurry to the deionized water is 12: 45;
b. two-step leaching and filter pressing
Keeping the temperature of the one-step leaching object in a filter at 65 ℃, leaching the one-step leaching object by using a 65 ℃ mixed solution, leaching and squeezing to obtain a light magnesium carbonate filter cake;
the mass ratio of the one-step showering washing matter to the mixed liquid is 1: 25;
the mixed solution comprises the following components in parts by mass: 1200 parts of deionized water, 4 parts of polydimethylsiloxane, 6 parts of aqueous hydrogen peroxide solution and 13 parts of absolute ethyl alcohol;
the mass concentration of the aqueous hydrogen peroxide solution is 20 percent;
the preparation method of the mixed liquid comprises the steps of mixing polydimethylsiloxane and absolute ethyl alcohol, stirring at the speed of 600r/min for 15min, adding deionized water and aqueous hydrogen peroxide, stirring at the speed of 600r/min for 25min, and stirring to obtain the mixed liquid.
(6) Drying by baking
And drying the light magnesium carbonate filter cake at 170 ℃, and drying until the water content is 2.6wt% to obtain the light magnesium carbonate.
Comparative example 1
On the basis of the embodiment 1, the secondary purification step is omitted, and the other steps are the same, so that the light magnesium carbonate is produced.
Comparative example 2
On the basis of the embodiment 1, in the leaching and filter pressing steps, the two leaching and filter pressing steps are omitted, and the rest steps are the same, so that the light magnesium carbonate is produced.
The indexes of the light magnesium carbonate produced by each example and comparative example are shown in Table 1.
Claims (10)
1. A method for producing light magnesium carbonate by using byproduct magnesium hydroxide is characterized by comprising the steps of crushing the byproduct magnesium hydroxide, purifying for the first time, purifying for the second time, carrying out synthesis reaction, leaching, filter pressing and drying;
the method for crushing the byproduct magnesium hydroxide comprises the steps of crushing the byproduct magnesium hydroxide dry filter cake to the fineness of 180-250 meshes to obtain byproduct magnesium hydroxide fine powder;
the primary purification method comprises the steps of mixing the byproduct magnesium hydroxide fine powder with deionized water to obtain magnesium slurry, adding caustic soda flakes and ethylene glycol, heating to 90-95 ℃, stirring at the speed of 300-400r/min for 1.8-2.5h to obtain primary purified magnesium slurry;
the secondary purification method comprises the steps of mixing the activated carbon loaded resin with the primary purified magnesium slurry, heating to 50-60 ℃, stirring at the speed of 400-500r/min for 3.5-4.5h, and filtering after stirring to obtain the purified magnesium slurry.
2. The method for producing light magnesium carbonate by using magnesium hydroxide as a by-product according to claim 1, which is characterized in that:
the mass ratio of the byproduct magnesium hydroxide fine powder to the deionized water is 6: 18-22;
the mass ratio of the caustic soda flakes to the deionized water is 1: 95-105;
the mass ratio of the ethylene glycol to the deionized water is 1: 95-105;
the mass ratio of the activated carbon loaded resin to the primarily purified magnesium slurry is 1: 45-55.
3. The method for producing light magnesium carbonate by using magnesium hydroxide as a by-product according to claim 1, which is characterized in that:
the preparation method of the activated carbon loaded resin comprises the steps of preparing expanded activated carbon and loaded resin;
the preparation method of the expanded activated carbon comprises the steps of crushing the activated carbon to the fineness of 80-120 meshes, mixing the crushed activated carbon and sodium bicarbonate, sending the mixture into a high-pressure homogenizer, carrying out high-pressure homogenization treatment under the pressure of 23-27MPa for 25-40min to obtain a mixture, dropwise adding a hydrochloric acid aqueous solution into the mixture, stirring at the speed of 150-250r/min while dropwise adding the hydrochloric acid aqueous solution, stirring at the speed of 300-400r/min after the hydrochloric acid aqueous solution is added, stirring for 25-40min, standing, filtering and drying to obtain the expanded activated carbon.
4. The method for producing light magnesium carbonate by using magnesium hydroxide as a by-product according to claim 3, which is characterized in that:
the aperture of the activated carbon is 22000-25000 nm;
the dropping speed of the hydrochloric acid aqueous solution is that the hydrochloric acid aqueous solution accounting for 3-7wt% of the mixture is added every minute, and the dropping time is 85-200 min;
the mass ratio of the crushed active carbon to the sodium bicarbonate is 1: 20-30;
the mass concentration of the hydrochloric acid aqueous solution is 18-22%.
5. The method for producing light magnesium carbonate by using magnesium hydroxide as a by-product according to claim 3, which is characterized in that:
mixing expanded activated carbon with ethyl acetate, adding methacrylic resin, heating to 50-60 ℃, stirring at the speed of 1400-1600r/min for 30-40min, then carrying out ultrasonic treatment at the frequency of 75-85kHz for 10-20min to obtain a negative carrier liquid after the ultrasonic treatment is finished, standing the carrier liquid for 15-25min, and carrying out spray drying in a vacuum environment of 18-25Pa to obtain the activated carbon loaded resin.
6. The method for producing light magnesium carbonate from magnesium hydroxide byproduct as claimed in claim 5, wherein the method comprises the following steps:
the mass ratio of the expanded activated carbon to the ethyl acetate is 1: 9-11;
the mass ratio of the methacrylic resin to the expanded activated carbon is 2.5-3.5: 2;
the molecular weight of the methacrylic resin is 15000-25000;
the temperature of the spray drying is 75-90 ℃.
7. The method for producing light magnesium carbonate by using magnesium hydroxide as a by-product according to claim 1, which is characterized in that:
adding the purified magnesium slurry into deionized water, adjusting the temperature to be 35-39 ℃, adding ammonium bicarbonate, stirring at the speed of 200-300r/min for 13-20min, adjusting the temperature to be 55-65 ℃ after stirring, and preserving heat to obtain light magnesium carbonate slurry;
the volume ratio of the purified magnesium slurry to the deionized water is 10: 20-30;
the mass volume ratio of the ammonium bicarbonate to the purified magnesium slurry is 2.3-3t:10m3。
8. The method for producing light magnesium carbonate by using magnesium hydroxide as a by-product according to claim 1, which is characterized in that:
the leaching and filter pressing comprises one-step leaching, two-step leaching and filter pressing;
the one-step leaching method comprises the steps of pumping the light magnesium carbonate slurry with the temperature of 55-65 ℃ after heat preservation into a filter, and introducing deionized water with the temperature of 55-65 ℃ for leaching to obtain a one-step leaching product;
the volume ratio of the light magnesium carbonate slurry to the deionized water is 12: 38-45;
the two-step leaching and filter pressing method comprises the steps of preserving heat of the one-step leaching object in a filter, keeping the temperature at 55-65 ℃, leaching the one-step leaching object by using the mixed solution at 55-65 ℃, and squeezing after leaching to obtain a light magnesium carbonate filter cake;
the mass ratio of the one-step showering and washing matter to the mixed solution is 1: 18-25;
the mixed solution comprises the following components in parts by mass: 800-1200 parts of deionized water, 2-4 parts of polydimethylsiloxane, 4-6 parts of aqueous hydrogen peroxide and 7-13 parts of absolute ethyl alcohol;
the mass concentration of the aqueous hydrogen peroxide solution is 20-30%;
the preparation method of the mixed solution comprises the steps of mixing polydimethylsiloxane and absolute ethyl alcohol, stirring at the speed of 400-600r/min for 15-25min, adding deionized water and aqueous hydrogen peroxide, stirring at the speed of 400-600r/min for 25-35min, and stirring to obtain the mixed solution.
9. The method for producing light magnesium carbonate by using magnesium hydroxide as a by-product according to claim 1, which is characterized in that:
the drying method comprises the steps of drying the light magnesium carbonate filter cake at the temperature of 150-170 ℃ until the water content is 2.4-2.6wt% to obtain the light magnesium carbonate.
10. The method for producing light magnesium carbonate from by-product magnesium hydroxide according to claim 1, wherein the method comprises the following steps:
the water content of the by-product magnesium hydroxide dry filter cake is 23-28wt%, and the solid content is 72-77 wt%;
the indexes of the solid in the byproduct magnesium hydroxide dry filter cake are as follows: 93.6 to 93.8 weight percent of magnesium hydroxide, 0.30 to 0.32 weight percent of calcium oxide, 0.28 to 0.30 weight percent of acid insoluble substance, 0.03 to 0.06 weight percent of iron, 1.32 to 1.5 weight percent of chlorine radical and 3.9 to 4.1 weight percent of borate;
the indexes of the solid matters in the purified magnesium slurry are as follows: 97.3 to 97.6 weight percent of magnesium hydroxide, 0.16 to 0.21 weight percent of calcium oxide, 0.2 to 0.23 weight percent of acid insoluble substance, 0.03 to 0.05 weight percent of iron, 1.18 to 1.24 weight percent of chlorine radical and 0.6 to 0.8 weight percent of borate.
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