CN115784275A - Green method for preparing high-purity light magnesium oxide through mother liquor circulation-dynamic carbonization - Google Patents
Green method for preparing high-purity light magnesium oxide through mother liquor circulation-dynamic carbonization Download PDFInfo
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- 239000012452 mother liquor Substances 0.000 title claims abstract description 159
- 238000003763 carbonization Methods 0.000 title claims abstract description 133
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 64
- 238000001354 calcination Methods 0.000 claims abstract description 50
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 19
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 19
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011777 magnesium Substances 0.000 claims abstract description 13
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 13
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 13
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 13
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 128
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 73
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 73
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 73
- 239000001099 ammonium carbonate Substances 0.000 claims description 73
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 64
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 64
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 59
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 41
- 238000006243 chemical reaction Methods 0.000 claims description 36
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 28
- 239000000347 magnesium hydroxide Substances 0.000 claims description 28
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 28
- 238000001914 filtration Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- 239000010413 mother solution Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 5
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 3
- 239000011736 potassium bicarbonate Substances 0.000 claims description 3
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000002699 waste material Substances 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 64
- 239000000395 magnesium oxide Substances 0.000 description 45
- 238000010438 heat treatment Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 102220043159 rs587780996 Human genes 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010000 carbonizing Methods 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910001425 magnesium ion Inorganic materials 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
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- 238000004064 recycling Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a process for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization. Calcining the basic magnesium carbonate to obtain the high-purity light magnesium oxide. The method comprises the steps of detecting the carbide component in the mother liquor in real time, and adding the carbide into the mother liquor to prepare the carbonization liquid circularly when the carbide component in the mother liquor is lower than a threshold value; when the carbide component in the mother liquor is higher than a threshold value, using a reserve carbonization liquid; the mother liquor enters the magnesium removal and carbon dioxide carbonization processes for dynamic carbonization, and the carbide component of the mother liquor is adjusted and then added into the carbonization liquid. The mother liquor can be circularly prepared into the carbonization liquid, and high-purity light magnesium oxide with different apparent specific volumes can be produced according to needs, so that zero discharge of waste residues and waste water is realized. The product of the invention has controllable specific volume and appearance, stable quality, low cost, environmental protection, high production efficiency and convenient industrial application.
Description
Technical Field
The invention relates to a process for preparing high-purity light magnesium oxide from magnesium hydroxide, belonging to the technical field of magnesium oxide preparation.
Background
The Qinghai Chevrolet salt lake contains rich resources such as potassium, lithium and the like, a large amount of bischofite is generated in the development of Chevrolet salt lake resources, and the Qinghai Western magnesium industry Limited company adopts an ammonia method to deposit magnesium and utilizes the bischofite to produce magnesium hydroxide products. In order to develop the application market of magnesium hydroxide, a process for preparing high-purity light magnesium oxide by circulating and dynamic carbonizing magnesium hydroxide mother liquor is researched, and the process can greatly improve the product value and has great economic benefits.
The light magnesium oxide is white powder with small bulk density and loose particles, the purity requirement is more than or equal to 92 percent, and the apparent specific volume is more than or equal to 4mL/g. It is mainly applied to the industries of plastics, tires, wires and cables, medicines, coatings, adhesives, leather making and the like. Magnesium resources in China are rich, but products with high added values are few.
The existing dolomite carbonization method is a main way for preparing light magnesium oxide domestically, such as patent 201910080552.0; the preparation process has the defects of high energy consumption, difficult control of impurity content, high fixed asset investment and the like. The production of light magnesium oxide from salt lake magnesium resources mainly uses ammonium bicarbonate as a carbonizing agent, mother liquor is not recycled, and waste water and waste residues are generated. Meanwhile, the light magnesium oxide product prepared from ammonium bicarbonate has high apparent specific volume, the appearance is not easy to control, the composition of the mother liquor carbide is not monitored in real time, and the requirement of dynamically regulating and controlling the apparent specific volume according to requirements cannot be met.
The prior magnesium oxide preparation method does not introduce the mother liquor circulation-dynamic carbonization, and also does not report that sodium bicarbonate, ammonium bicarbonate and carbon dioxide are utilized to regulate the carbide component in the mother liquor step by step and magnesium oxide with different apparent specific volumes is produced as required.
Disclosure of Invention
Aiming at the defects of the preparation process of light magnesium oxide in the prior art, the invention aims to provide the process for preparing high-purity light magnesium oxide by using the magnesium hydroxide of a salt lake product as a raw material and utilizing mother liquor circulation-dynamic carbonization, wherein the process forms a green closed loop, the mother liquor is recycled, and no wastewater or waste residue is discharged; monitoring the composition of the mother liquor carbide in real time, and dynamically carbonizing to accurately control the apparent specific volume; the pain point of the prior light magnesium oxide process is solved; the prepared light magnesium oxide has stable quality, adjustable specific volume and high production efficiency, and meets the requirements of industrial production.
The invention discloses a process for preparing high-purity light magnesium oxide from magnesium hydroxide, which comprises the following steps:
(1) Adding magnesium hydroxide into the carbonization liquid for carbonization and aging, and filtering to obtain basic magnesium carbonate solid and mother liquor;
(2) And washing, drying and calcining the basic magnesium carbonate to obtain the high-purity light magnesium oxide.
(3) Detecting the composition of the mother liquor carbide in real time, and adding the carbide into the mother liquor to prepare a carbonization liquid in a circulating manner when the composition of the mother liquor carbide is less than a threshold value; when the carbide component in the mother liquor is larger than a threshold value, using a reserved carbonization liquid; the mother liquor enters magnesium removal and carbon dioxide carbonization processes for carbonization, and the carbide components of the mother liquor are adjusted and then return to the carbonization liquid.
The process for preparing high-purity light magnesium oxide from magnesium hydroxide further comprises the following preferred scheme:
preferably, as in step (1), the carbonization reaction temperature is 30 to 95 ℃ and the carbonization time is 1 to 4 hours. The aging reaction time is 1-6h.
When magnesium hydroxide is added into the carbonization liquid for carbonization, the addition amount of the bicarbonate radical is 0.5 to 0.9 time of the theoretical molar weight of the carbonization reaction. Preferably 0.6 to 0.8 times. The theoretical molar amount of carbonation in the present invention means the molar amount of bicarbonate required for complete conversion of magnesium hydroxide to basic magnesium carbonate.
The purity of the magnesium hydroxide used in the invention is more than or equal to 99 percent. The D50 is less than 74 microns.
Preferably, as shown in step (2), the washed and dried filter residue is placed in a furnace, and calcined by raising the temperature to 800-1150 ℃ at a temperature raising rate of 6-10 ℃/min. A further preferred calcination temperature is 850-1150 ℃.
Preferably, as step (3), the molar ratio of carbonate to bicarbonate in the mother liquor is detected in real time, and the ratio interval is 20-45. Namely, the selectable range of the threshold value is 20-45; in industrial applications, 45 is preferred. The determination of the value is favorable for obtaining the magnesium oxide product with high quality.
Preferably, as in step (3), when the molar ratio of carbonate to bicarbonate in the mother liquor is less than 45, the carbide is added to the mother liquor to prepare the carbonization liquid. In industrial application, when the molar ratio of carbonate to bicarbonate in the mother liquor is less than 45, the carbonate is added to adjust the bicarbonate content in the mother liquor, which is beneficial to realizing the cyclic utilization of the mother liquor on the premise of ensuring the controllable morphology and yield of the light magnesium oxide.
Preferably, as in step (3), when the molar ratio of carbonate to bicarbonate in the mother liquor is greater than 45, a stock carbonation solution is used; the mother liquor enters into a magnesium and CO removing device 2 And a carbonization procedure is carried out to prepare carbonization liquid. CO 2 2 The stirring speed in the carbonization procedure is 150-350r/min, and the flow of the introduced carbon dioxide is 300-800ml/min. The composition of the stored carbonization liquid is consistent with that of the carbonization liquid in the step (1).
Preferably, as in step (3), ammonium bicarbonate in the carbide: and (b) the mass ratio of A =0-10, wherein A is bicarbonate which can be dissolved in water besides ammonium bicarbonate.
Preferably, as in step (3), the bicarbonate is one or more of sodium bicarbonate and potassium bicarbonate, and the sodium bicarbonate or potassium bicarbonate has a wide source and a proper price, and is beneficial to controlling the morphology and the apparent specific volume of the magnesium oxide.
Preferably, as step (3), the molar ratio of carbonate to bicarbonate in the carbonization liquid is detected and controlled in real time and is less than or equal to 2.1. As a further preference, as in step (3), a molar ratio of carbonate to bicarbonate in the carbonized liquid detected and controlled in real time is preferably 0.5 or less, for example, 0 to 0.3, 0.1 to 0.25, 0.30 to 0.45. When the molar ratio of carbonate to bicarbonate in the carbonization liquid is more than 2.1, the carbonization efficiency is low, and the appearance and the apparent specific volume are not controllable.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1. the mother solution of the invention is circulated, no waste water and waste residue are discharged, and the green closed-loop preparation of the high-purity light magnesium oxide is realized.
2. The real-time monitoring of the invention determines whether to add carbide to prepare the carbonization liquid or use the stored carbonization liquid according to the carbide components in the mother liquid, and the mother liquid enters the magnesium removal and carbon dioxide carbonization procedures, thereby realizing the closed loop of the process and improving the production efficiency.
3. The dynamic carbonization of the invention dynamically adjusts the components of the carbonization liquid according to the requirements of users on specific volume, realizes the accurate dynamic control on the specific volume and achieves the balance of cost and quality by combining with the circulation of the mother liquid.
4. The carbide prepared carbonization liquid of the invention makes up the disadvantage of slower carbonization rate of carbon dioxide at normal temperature and normal pressure, and realizes the balance and matching of the production speed of magnesium oxide and the carbonization speed of carbon dioxide.
5. The mother liquor can be circularly prepared into carbonization liquid, the carbonate component in the mother liquor is adjusted by dynamic carbonization of sodium bicarbonate, ammonium bicarbonate and carbon dioxide, high-purity light magnesium oxide with different specific volumes is produced according to needs, and zero discharge of waste residue and waste water is realized. Meanwhile, the magnesium oxide prepared by the method has the advantages of controllable specific volume and appearance, stable product quality, low cost, environmental friendliness and high production efficiency, and meets the requirements of industrial production.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is an SEM photograph of the light magnesium oxide obtained in example 3
FIG. 3 is an SEM photograph of light magnesium oxide obtained in comparative example 4
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present disclosure is further described in conjunction with the following examples, it is emphasized that the following description is intended to be illustrative only, and is not intended to limit the scope and application of the present disclosure.
Example 1
Step (1): magnesium hydroxide (purity 99.4%, D50=45 μm) was added to the carbonation vessel at a rate of 0.2L/h of ammonium bicarbonate and sodium bicarbonate solution, a mass ratio of ammonium bicarbonate to sodium bicarbonate of 10, and bicarbonate was added in an amount of 0.8 times the theoretical molar amount of carbonation (the theoretical molar amount of carbonation being the molar amount of bicarbonate required for complete conversion of magnesium hydroxide to basic magnesium carbonate). The carbonization reaction temperature is 70 ℃, and the carbonization time is 2h. The aging reaction time is 2h, and the stirring speed is 100r/min. Filtering with a plate filter press.
Step (2): drying by a flash evaporation dryer, wherein the air inlet temperature of the dryer is 240 ℃, the mixing temperature is 110 ℃, and the air outlet temperature is 110 ℃. And (3) putting the washed and dried filter residue into a furnace, and heating to 1000 ℃ at the heating rate of 8 ℃/min for calcining. The purity of the magnesium oxide obtained by the first calcination was 99.5wt%, and the apparent specific volume was 8.7ml/g.
And (3): the filtrate obtained by filtering in the step (1) is mother liquor (the molar ratio of carbonate to bicarbonate in the mother liquor is 21), ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 10; completing the first cyclic utilization of the mother liquor;
repeating the steps (1) and (2) for the first time, and defining the steps as cycle 1; the purity of the magnesium oxide obtained by calcination in cycle 1 was 99.5% by weight, depending on the specific volume, 8.6ml/g. And by parity of reasoning, cycle 2, cycle 3, cycle 4, cycle 5, cycle 6, 8230, 8230are formed; at each specific cycle, the condition parameters and controls are as follows:
in the circulation 2, the molar ratio of carbonate radicals to bicarbonate radicals in the mother liquor is 28, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 10: 20), and the steps (1) and (2) are repeated; the mother liquor is recycled; the purity of the magnesium oxide obtained by calcination in cycle 2 was 99.4wt%, depending on the specific volume 8.4ml/g.
When the step 3 is circulated, the molar ratio of carbonate to bicarbonate in the mother liquor is 35, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 10); the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 3 was 99.5% by weight, depending on the specific volume, 8.0ml/g.
In the circulation 4, the molar ratio of carbonate to bicarbonate in the mother liquor is 40, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 10: 20), and the steps (1) and (2) are repeated; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 4 was 99.3% by weight, depending on the specific volume, 7.5ml/g.
When circulation 5 is carried out, the molar ratio of carbonate radicals to bicarbonate radicals in the mother liquor is 45, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 10; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 5 was 99.4% by weight, depending on the specific volume, 7.1ml/g.
In the cycle 6, the molar ratio of carbonate radicals to bicarbonate radicals in the mother liquor is 49; the mother liquor can not be recycled, and at the moment, a reserve carbonization liquid is used, and the molar ratio of carbonate to bicarbonate in the carbonization liquid is 0. The steps (1) and (2) were repeated, and the calcined magnesium oxide had a purity of 99.5wt% and a specific volume of 8.6ml/g. Removing magnesium ions from the mother liquor by using SCD-120 resin; the mother liquor enters CO after magnesium removal 2 A carbonization procedure, wherein the stirring speed is 150r/min, and the flow rate of carbon dioxide is 200ml/min; the carbonization time is 12h, the mother liquor is added into the carbonization liquid after the carbonization is finished, and the molar ratio of carbonate radical to bicarbonate radical in the mother liquor after the carbonization is finished is 0.6; at which point use can continue.
The storage carbonization liquid consists of ammonium bicarbonate and sodium bicarbonate according to the mass ratio of 10: the amount of bicarbonate added is 0.8 times the theoretical molar amount of carbonation (the theoretical molar amount of carbonation is the molar amount of bicarbonate required for complete conversion of magnesium hydroxide to basic magnesium carbonate).
Example 2
Step (1): magnesium hydroxide (purity 99.4%, D50=5 μm) was added to the carbonation vessel, the rate of addition of ammonium bicarbonate and sodium bicarbonate solution was 0.3L/h, the mass ratio of ammonium bicarbonate to sodium bicarbonate was 3, and the amount of bicarbonate added was 0.5 times the theoretical molar amount of carbonation reaction. The carbonization reaction temperature is 80 ℃, and the carbonization time is 1.5h. The aging reaction time is 2h, and the stirring speed is 150r/min. Filtering with a plate filter press.
Step (2): and drying by adopting a flash dryer, wherein the air inlet temperature of the dryer is 240 ℃, the mixing temperature is 115 ℃, and the air outlet temperature is 110 ℃. The filter residue after washing and drying is put into a furnace, and is heated to 1100 ℃ at the heating rate of 10 ℃/min for calcination. The purity of the magnesium oxide obtained by the first calcination was 99.5wt%, and the apparent specific volume was 7.8ml/g.
And (3): the filtrate obtained by filtering in the step (1) is mother liquor (the molar ratio of carbonate to bicarbonate in the mother liquor is 21), ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 3; the first recycling of the mother liquor is completed;
repeating the steps (1) and (2) for the first time, and defining the steps as cycle 1; the purity of the magnesium oxide obtained by calcination in cycle 1 was 99.5% by weight, depending on the specific volume, 7.5ml/g. The process is repeated to form a cycle 2, a cycle 3, a cycle 4, a cycle 5 and a cycle 6 of 82308230; at each specific cycle, the condition parameters and controls are as follows:
when the process 2 is circulated, the molar ratio of carbonate to bicarbonate in the mother liquor is 26, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 3; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 2 was 99.4% by weight, depending on the specific volume, 7.4ml/g.
When the step 3 is circulated, the molar ratio of carbonate radicals to bicarbonate radicals in the mother liquor is 36, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of the ammonium bicarbonate to the sodium bicarbonate is 3; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 3 was 99.5% by weight, depending on the specific volume, 7.2ml/g.
When the circulation is 4, the molar ratio of carbonate to bicarbonate in the mother liquor is 39, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 3; the mother liquor is recycled again; cycle 4 calcination gave magnesium oxide with a purity of 99.4wt% and a specific volume of 6.9ml/g.
In the circulation 5, the molar ratio of carbonate to bicarbonate in the mother liquor is 44, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 3; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 5 was 99.4wt%, depending on the specific volume 6.6ml/g.
When circulating 6, the molar ratio of carbonate radicals to bicarbonate radicals in the mother solution is 50; the mother liquor can not be recycled, a stock carbonization liquid is used, the molar ratio of carbonate to bicarbonate in the carbonization liquid is 0, the steps (1) and (2) are repeated, and the purity of the magnesium oxide obtained by calcination is 99.5wt%, and the apparent specific volume is 7.6ml/g. Removing magnesium ions from the mother liquor by using SCD-120 resin; the mother liquor enters CO after magnesium removal 2 A carbonization procedure, wherein the stirring speed is 150r/min, and the flow rate of carbon dioxide is 300ml/min; the carbonization time is 14h, the mother liquor is added into the carbonization liquid after the carbonization, and the molar ratio of carbonate radical to bicarbonate radical in the mother liquor after the carbonization is 0.5; use can continue at this point. The storage carbonization liquid consists of ammonium bicarbonate and sodium bicarbonate according to the mass ratio of 3: the amount of bicarbonate added is 0.5 times the theoretical molar amount of carbonation (the theoretical molar amount of carbonation is the molar amount of bicarbonate required for complete conversion of magnesium hydroxide into basic magnesium carbonate).
Example 3
Step (1): magnesium hydroxide (purity 99.6%, D50=47 μm) was added to the carbonation vessel at a rate of 0.25L/h of ammonium bicarbonate and sodium bicarbonate solution, a mass ratio of ammonium bicarbonate to sodium bicarbonate of 0.20, and bicarbonate was added in an amount of 0.6 times the theoretical molar amount of carbonation reaction. The carbonization reaction temperature is 90 ℃, and the carbonization time is 2h. The aging reaction time is 3h, and the stirring speed is 300r/min. Filtering with a plate filter press.
Step (2): drying by a flash evaporation dryer, wherein the inlet air temperature of the dryer is 240 ℃, the mixing temperature is 115 ℃, and the outlet air temperature is 110 ℃. And (3) putting the washed and dried filter slag into a furnace, and heating to 900 ℃ at the heating rate of 8 ℃/min for calcining. The purity of the magnesium oxide obtained by the first calcination was 99.6wt%, and the apparent specific volume was 5.2ml/g.
And (3): step 1, filtering to obtain a filtrate which is a mother liquor (the molar ratio of carbonate to bicarbonate in the mother liquor is 20), adding ammonium bicarbonate and sodium bicarbonate into the mother liquor to prepare a carbonization solution (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 0; the first recycling of the mother liquor is completed;
repeating the steps (1) and (2) for the first time, and defining the steps as cycle 1; the purity of the magnesium oxide obtained by calcination in cycle 1 was 99.6% by weight, depending on the specific volume, 5.1ml/g. The process is repeated to form a cycle 2, a cycle 3, a cycle 4, a cycle 5 and a cycle 6 of 82308230; at each specific cycle, the condition parameters and controls are as follows:
in the circulation 2, the molar ratio of carbonate radicals to bicarbonate radicals in the mother liquor is 24, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 0; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 2 was 99.4% by weight, depending on the specific volume, 5.1ml/g.
When the step 3 is circulated, the molar ratio of carbonate to bicarbonate in the mother liquor is 34, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 0; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 3 was 99.4wt%, depending on the specific volume 4.8ml/g.
When the circulation is 4, the molar ratio of carbonate to bicarbonate in the mother liquor is 41, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 0: 20), and the steps (1) and (2) are repeated; the mother liquor is recycled again; calcination in cycle 4 gave a magnesia purity of 99.4wt% with a specific volume of 4.6ml/g.
When circulating 5, the molar ratio of carbonate to bicarbonate in the mother liquor is 45, adding ammonium bicarbonate and sodium bicarbonate into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 0; the mother liquor is recycled; the purity of the magnesium oxide obtained by calcination in cycle 5 was 99.4% by weight, depending on the specific volume 4.4ml/g. The SEM image is shown in FIG. 2.
In the circulation 6, the molar ratio of carbonate to bicarbonate in the mother liquor is 51; the mother liquor can not be recycled, the stored carbonization liquid is used, and the carbonate and bicarbonate radicals in the carbonization liquid are usedThe molar ratio was 0, and the steps (1) and (2) were repeated, and the calcined magnesium oxide had a purity of 99.5% by weight and a specific volume of 5.2ml/g. Removing magnesium ions from the mother liquor by using SCD-120 resin; the mother liquor enters CO after magnesium removal 2 A carbonization procedure, wherein the stirring speed is 150r/min, and the flow rate of carbon dioxide is 400ml/min; the carbonization time is 8h, the mother liquor is added into the carbonization liquid after the carbonization, and the molar ratio of carbonate radical to bicarbonate radical in the mother liquor after the carbonization is 1.2; use can continue at this point.
The storage carbonization liquid is sodium bicarbonate solution, and the dosage standard is as follows: the amount of bicarbonate added is 0.6 times the theoretical molar amount of carbonation (the theoretical molar amount of carbonation is the molar amount of bicarbonate required for complete conversion of magnesium hydroxide to basic magnesium carbonate).
Comparative example 1
Magnesium hydroxide (99.4% pure, D50=45 μm) was placed in a furnace and calcined by heating to 900 ℃ at a rate of 8 ℃/min. The purity of the magnesium oxide obtained by calcination was 99.4% by weight, depending on the specific volume, 2ml/g.
Comparative example 2
And (3) putting magnesium hydroxide into a reaction kettle, wherein the adding amount of ammonium bicarbonate is 1.2 times of the theoretical molar amount of the carbonization reaction, the concentration of the ammonium bicarbonate is 1.3mol/l, the reaction temperature is 60 ℃, and the reaction time is 1.5H. The calcining temperature is 950 ℃, the heating rate is 6 ℃/min, and the calcining time is 1.5H. The light magnesium oxide with a purity of 99.1% is obtained, the apparent specific volume is 10ml/g. The theoretical molar amount of carbonization reaction refers to the molar amount of bicarbonate required for complete conversion of magnesium hydroxide into basic magnesium carbonate.
Comparative example 3
And (3) putting magnesium hydroxide into a reaction kettle, wherein the adding amount of ammonium bicarbonate is 1.1 times of the theoretical molar amount of the carbonization reaction, the concentration of the ammonium bicarbonate is 1.1mol/l, the reaction temperature is 70 ℃, and the reaction time is 2H. The calcination temperature is 900 ℃, the heating speed is 6 ℃/min, and the calcination time is 1.5H. The purity of the obtained magnesium oxide product is 98.9 percent, and the apparent specific volume reaches 9ml/g. The theoretical molar amount of carbonization reaction refers to the molar amount of bicarbonate required for complete conversion of magnesium hydroxide into basic magnesium carbonate.
Comparative example 4
And (3) putting magnesium hydroxide into a reaction kettle, wherein the adding amount of ammonium bicarbonate is 1.3 times of the theoretical molar amount of the carbonization reaction, the concentration of the ammonium bicarbonate is 1.5mol/l, the reaction temperature is 65 ℃, and the reaction time is 2H. The calcination temperature is 930 ℃, the heating speed is 6 ℃/min, and the calcination time is 2H. The purity of the obtained magnesium oxide product is 99.2 percent, and the apparent specific volume reaches 11ml/g. The SEM image is shown in FIG. 3. The theoretical molar amount of carbonization reaction refers to the molar amount of bicarbonate required for complete conversion of magnesium hydroxide into basic magnesium carbonate.
Comparative example 5
Other conditions were the same as in example 3; the difference lies in that:
in the circulation 6, the molar ratio of carbonate to bicarbonate in the mother liquor is 51; the mother liquor is continuously recycled, namely ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of the ammonium bicarbonate to the sodium bicarbonate is 0; the mother liquor is recycled; the purity of the magnesium oxide obtained by calcination in cycle 6 was 99.4% by weight, depending on the specific volume, 3.9ml/g. At this time, the carbonization rate is slow, and the quality of the product is poor. This results in the mother liquor not being able to be recycled.
Comparative example 6
Step (1): magnesium hydroxide (purity 99.3%, D50=43 μm) was added to the carbonation kettle at a rate of 0.32L/h of ammonium bicarbonate and sodium bicarbonate solution, with a mass ratio of ammonium bicarbonate to sodium bicarbonate of 1 to 20, and bicarbonate was added in an amount of 0.6 times the theoretical molar amount of the carbonation reaction. The carbonization reaction temperature is 90 ℃, and the carbonization time is 2h. The aging reaction time is 3h, and the stirring speed is 200r/min. Filtering with a plate filter press.
Step (2): drying by a flash evaporation dryer, wherein the inlet air temperature of the dryer is 240 ℃, the mixing temperature is 115 ℃, and the outlet air temperature is 105 ℃. And (3) putting the washed and dried filter residue into a furnace, and heating to 900 ℃ at a heating rate of 10 ℃/min for calcining. The purity of the magnesium oxide obtained by the first calcination was 99.6wt%, and the specific volume was 5.8ml/g.
And (3): filtering in the step (1) to obtain a filtrate which is a mother solution (the molar ratio of carbonate to bicarbonate in the mother solution is 20), adding ammonium bicarbonate and sodium bicarbonate to prepare a carbonization solution (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 1; completing the first cyclic utilization of the mother liquor;
repeating the steps (1) and (2) for the first time, and defining the steps as cycle 1; the purity of the magnesium oxide obtained by calcination in cycle 1 was 99.6% by weight, depending on the specific volume 5.7ml/g.
When the step 2 is circulated, the molar ratio of carbonate to bicarbonate in the mother liquor is 24, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 1 to 20), and the steps (1) and (2) are repeated; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 2 was 99.4wt%, depending on the specific volume 5.6ml/g.
When the step 3 is circulated, the molar ratio of carbonate to bicarbonate in the mother liquor is 36, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 1 to 20), and the steps (1) and (2) are repeated; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 3 was 99.4% by weight, depending on the specific volume, 5.2ml/g.
In the circulation 4, the molar ratio of carbonate radicals to bicarbonate radicals in the mother liquor is 40, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of the ammonium bicarbonate to the sodium bicarbonate is 1; the mother liquor is recycled again; cycle 4 calcination gave magnesium oxide with a purity of 99.4wt% and a specific volume of 4.9ml/g.
When circulation 5 is carried out, the molar ratio of carbonate radicals to bicarbonate radicals in the mother liquor is 45, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 1; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 5 was 99.4% by weight, depending on the specific volume 4.4ml/g.
When the circulation is carried out for 6, the molar ratio of carbonate to bicarbonate in the mother liquor is 50, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 1; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 6 was 99.4% by weight, depending on the specific volume, 3.9ml/g.
When 7 is circulated, the molar ratio of carbonate radicals to bicarbonate radicals in the mother liquor is 54, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 1; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 7 was 99.4% by weight, depending on the specific volume 3.1ml/g.
When the circulation is carried out for 8, the molar ratio of carbonate to bicarbonate in the mother liquor is 58, ammonium bicarbonate and sodium bicarbonate are added into the mother liquor to prepare a carbonization liquid (the mass ratio of ammonium bicarbonate to sodium bicarbonate is 1; the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 8 was 99.4% by weight, depending on the specific volume, 2.6ml/g.
Comparative example 7
Step (1): magnesium hydroxide (purity 99.3%, D50=44 μm) was added to the carbonation kettle at a rate of 0.32L/h of ammonium bicarbonate and sodium bicarbonate solution, a mass ratio of ammonium bicarbonate to sodium bicarbonate of 0.20, and bicarbonate was added in an amount of 0.6 times the theoretical molar amount of the carbonation reaction. The carbonization reaction temperature is 90 ℃, and the carbonization time is 2h. The aging reaction time is 3h, and the stirring speed is 200r/min. Filtering with a plate filter press.
Step (2): drying by a flash dryer, wherein the inlet air temperature of the dryer is 240 ℃, the mixing temperature is 115 ℃, and the outlet air temperature is 105 ℃. The filter residue after washing and drying is put into a furnace, and is heated to 1000 ℃ at the heating rate of 10 ℃/min for calcination. The purity of the magnesium oxide obtained by the first calcination was 99.6wt%, and the specific volume was 5.8ml/g.
And (3): the filtrate obtained by filtering in the step (1) is mother liquor (the molar ratio of carbonate to bicarbonate in the mother liquor is 20), carbon dioxide is introduced into the mother liquor for 6 hours, the flow rate of the carbon dioxide is 300ml/min, and the molar ratio of the carbonate to the bicarbonate in the mother liquor after reaction is 1.4; repeating the steps (1) and (2); the mother liquor is recycled; the purity of the magnesium oxide obtained by calcination in cycle 1 was 99.6wt%, depending on the specific volume, 5.2ml/g.
During circulation 2, the molar ratio of carbonate to bicarbonate in the mother liquor is 24, carbon dioxide is introduced into the mother liquor for 10 hours, the flow rate of the carbon dioxide is 400ml/min, and the molar ratio of the carbonate to the bicarbonate in the mother liquor after reaction is 1.0; repeating the steps (1) and (2); the mother liquor is recycled again; the purity of the magnesium oxide obtained by calcination in cycle 2 was 99.4% by weight, depending on the specific volume, 5.1ml/g.
When the solution is circulated for 3 times, the molar ratio of carbonate to bicarbonate in the mother solution is 23, carbon dioxide is introduced into the mother solution for 20 hours, the flow rate of the carbon dioxide is 350ml/min, and the molar ratio of the carbonate to the bicarbonate in the mother solution after the reaction is 0.3; repeating the steps (1) and (2); the mother liquor is recycled; the purity of the magnesium oxide obtained by calcination in cycle 2 was 99.4wt%, depending on the specific volume, 5.2ml/g. The biggest problems reflected by this comparative example are: the reaction period is long and the production efficiency is low.
The background section of the present invention may contain background information related to the problem or environment of the present invention and does not necessarily describe prior art. Accordingly, the inclusion in the background section is not an admission of prior art by the applicant.
The foregoing is a more detailed description of the present invention with reference to specific embodiments thereof, and it is not intended to limit the invention to the specific embodiments thereof. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and these substitutions and modifications should be considered to fall within the scope of the invention. In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Various embodiments or examples and features of various embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction. Although embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the scope of the claims.
Claims (10)
1. A green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization is characterized by comprising the following steps:
(1) Adding magnesium hydroxide into the carbonization liquid for carbonization and aging, and filtering to obtain basic magnesium carbonate solid and mother liquor;
(2) Washing and drying basic magnesium carbonate, and calcining to obtain high-purity light magnesium oxide;
(3) Detecting the composition of the mother liquor carbide in real time, and adding the carbide to prepare a carbonized liquid circularly when the carbonized composition of the mother liquor is less than a threshold value; when the mother liquor carbonization component is larger than the threshold value, using a reserved carbonization liquid; the mother liquor enters magnesium removal and carbon dioxide carbonization procedures for carbonization, the carbide component in the mother liquor is adjusted and then added into the carbonization liquor, and the threshold value is the mole ratio of carbonate radical and bicarbonate radical of the mother liquor; the threshold value ranges from 20 to 45.
2. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization as claimed in claim 1, wherein: the carbonization reaction temperature in the step (1) is 25-100 ℃, the carbonization time is 1-5h, and the aging reaction time is 1-7h.
3. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization as claimed in claim 1, wherein: in the step (2), the filter residue after washing and drying is placed in a furnace, and the temperature is raised to 800-1150 ℃ at the temperature raising rate of 6-10 ℃/min for calcination.
4. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization as claimed in claim 1, characterized in that: and (3) detecting the mole ratio of carbonate and bicarbonate of the mother liquor in real time, wherein the ratio interval is 20-45, namely the value range of the threshold is 20-45.
5. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization as claimed in claim 4, characterized in that: in the step (3), the threshold value of the carbonized component in the mother liquor is that the molar ratio of carbonate to bicarbonate is 45.
6. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization as claimed in claim 4, wherein: in the step (3), when the molar ratio of carbonate to bicarbonate in the mother liquor is less than 45, adding a carbide into the mother liquor to prepare a carbonization liquid, wherein ammonium bicarbonate in the carbide: bicarbonate mass ratio = 0-10.
7. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization as claimed in claim 6, wherein: in the step (3), the bicarbonate is one or more of sodium bicarbonate and potassium bicarbonate.
8. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization as claimed in claim 4, characterized in that: in the step (3), when the molar ratio of carbonate to bicarbonate in the mother solution is greater than 45, using a stored carbonization solution; the mother liquor enters into a magnesium and CO removing device 2 And a carbonization procedure is carried out to prepare carbonization liquid.
9. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization according to claim 8, characterized in that: in step (3), CO 2 The stirring speed in the carbonization procedure is 150-350r/min, and the flow of the introduced carbon dioxide is 300-800ml/min.
10. The green method for preparing high-purity light magnesium oxide by mother liquor circulation-dynamic carbonization as claimed in claim 4, characterized in that: and (3) detecting and controlling the mole ratio of carbonate to bicarbonate of the carbonization liquid in real time to be less than or equal to 2.1.
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| CN101353176A (en) * | 2007-07-26 | 2009-01-28 | 郑州大学 | Novel method for preparing nano-magnesia |
| CN104495881A (en) * | 2014-12-19 | 2015-04-08 | 中南大学 | Process for preparing high-purity silicon steel magnesium oxide from magnesium hydroxide |
| CN104591234A (en) * | 2015-01-09 | 2015-05-06 | 中南大学 | Process for preparing light magnesium carbonate from industrial magnesium hydroxide |
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| CN101353176A (en) * | 2007-07-26 | 2009-01-28 | 郑州大学 | Novel method for preparing nano-magnesia |
| CN104495881A (en) * | 2014-12-19 | 2015-04-08 | 中南大学 | Process for preparing high-purity silicon steel magnesium oxide from magnesium hydroxide |
| CN104591234A (en) * | 2015-01-09 | 2015-05-06 | 中南大学 | Process for preparing light magnesium carbonate from industrial magnesium hydroxide |
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| 程俊峰: ""高纯氢氧化镁制备硅钢级氧化镁工艺研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑（电子期刊）》, pages 2 - 5 * |
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