CN110002478A - The device and method of flake magnesium hydroxide and spherical magnesia is prepared with rear magnesia - Google Patents
The device and method of flake magnesium hydroxide and spherical magnesia is prepared with rear magnesia Download PDFInfo
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- CN110002478A CN110002478A CN201810009905.3A CN201810009905A CN110002478A CN 110002478 A CN110002478 A CN 110002478A CN 201810009905 A CN201810009905 A CN 201810009905A CN 110002478 A CN110002478 A CN 110002478A
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- magnesia
- magnesium
- magnesium hydroxide
- spherical
- round
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- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 64
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 30
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 27
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000007246 mechanism Effects 0.000 claims abstract description 54
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000011777 magnesium Substances 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 17
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000004448 titration Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 11
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 15
- 238000003760 magnetic stirring Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 8
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims 1
- 229910000976 Electrical steel Inorganic materials 0.000 abstract description 11
- 229910000831 Steel Inorganic materials 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 4
- 239000010959 steel Substances 0.000 abstract description 4
- -1 supporting mechanism Chemical compound 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000004064 recycling Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 150000002680 magnesium Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon 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
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
- C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
-
- 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
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
- C01P2006/12—Surface area
Abstract
The present invention proposes a kind of device that flake magnesium hydroxide and spherical magnesia are prepared with rear magnesia, including supporting mechanism, titrate mechanism, rabbling mechanism and heating mechanism, titration mechanism and rabbling mechanism are installed on supporting mechanism, titrating has the space for accommodating ammonium hydroxide and the magnesium chloride liquid formed with rear magnesia through the molten removal of impurities processing of acid in mechanism, anti- drop operation is carried out by titration mechanism and forms magnesium hydrate precipitate, magnesium hydrate precipitate is heated by heating mechanism to obtain flake magnesium hydroxide solid, and continue to obtain spherical magnesia to magnesium hydroxide solid heating and calcining.Using the device and method, to silicon-steel grade magnesium oxide, remaining black powder during producing grain-oriented Si steel sheet is recycled, and after, removal of impurities molten by acid, precipitating, washing, drying and calcining and other processes, prepares ultra-fine sheet Mg (OH)2With coccoid MgO product, generation heat is focused with convex lens, reaction is heated, directly using sunlight as the energy, do not consume other energy, process is environmentally protective.
Description
Technical field
The present invention relates to magnesia production technology more particularly to a kind of flake magnesium hydroxide and spherical is prepared with rear magnesia
The device and method of magnesia.
Background technique
Silicon-steel magnesium oxide has very important purposes during manufacturing grain-oriented Si steel sheet, therefore industrially makes to it
Dosage demand is also very big.In industrial production orientating type silicon steel sheet, silicon-steel grade magnesium oxide and water are mixed by a certain percentage first
Jelly is synthesized, silicon steel sheet surface is then coated on, is finally calcined under bell-type furnace high-temperature, silicon steel sheet obtained in this way
Just there is good insulating properties and electromagnetism intensity.Coil of strip can fall off lower a large amount of black powders during uncoiling after cooling, this
The content rich in elements, especially magnesium such as magnesium, silicon, iron is very high in kind black powder, and black is deposited in the form of magnesia
In powder.A few big steel enterprises in China will produce nearly million tons of orientating type silicon steel sheets every year, thus to silicon-steel grade magnesium oxide
Demand is also up to nearly ten thousand tons, then just remained a large amount of this black oxidation magnesium dust in production process, they are much
It is unable to reach silicon-steel grade magnesium oxide standard, cannot be utilized again.These powder were all directly left unused or were buried in the past, no longer heavy
Utilization newly developed, had not only caused a kind of waste of resource in this way, but also affected to environment and ecology.Therefore how by this
Magnesium recycling and reusing in black powder, economically both reduces cost in this way, and the recycling of resource is also one big in environmental protection
Contribution.At present to the enterprises and institutions studied with the recycling and reusing of rear magnesia also almost without Baosteel and Wuhan Iron and Steel Plant etc.
Large enterprise it is also noted that resource recycling necessity, entrust some research units to rear magnesia recycling and reusing into
Row discusses and research, this is also at one urgent problem to be solved of current electrical sheet manufacturing enterprise.
Summary of the invention
The object of the present invention is to provide it is a kind of with rear magnesia prepare flake magnesium hydroxide and spherical magnesia device and
Method is recycled to rear magnesia.
The present invention is that technical solution used by solving its technical problem is:
It prepares the device of flake magnesium hydroxide and spherical magnesia with rear magnesia, including supporting mechanism, titration mechanism, stirs
Mechanism and heating mechanism are mixed, titration mechanism and rabbling mechanism are installed on supporting mechanism, and titrating in mechanism has receiving ammonium hydroxide
And the space of the magnesium chloride liquid formed with rear magnesia through the molten removal of impurities processing of acid, it is dripped by titration mechanism and heating mechanism are counter
Operation forms magnesium hydrate precipitate, carries out heating, drying to magnesium hydrate precipitate by heating mechanism after washing and obtains hydroxide flake
Magnesium solid, and continue to obtain spherical magnesia to magnesium hydroxide solid heating and calcining.
Supporting mechanism includes pedestal, and column is fixed on pedestal, and column is fixed with outstanding to stretching above pedestal, top
Bar, hanging stick end have positioning ring；
Titrating mechanism includes the separatory funnel that can accommodate ammonium hydroxide, which is placed in positioning ring, below separatory funnel
Equipped with the round-bottomed flask that can accommodate magnesium chloride liquid, which is placed on pedestal, and the down tube of separatory funnel protrudes into round bottom burning
In bottle；
Rabbling mechanism includes magnetic stirring apparatus, and magnetic stirring apparatus is placed between pedestal and round-bottomed flask, is put in round-bottomed flask
It is equipped with the stirrer being adapted to magnetic stirring apparatus, the liquid in round-bottomed flask is stirred by magnetic stirring apparatus driving stirrer
It mixes；
Heating mechanism includes one group of convex lens and calcining furnace, and convex lens is provided with 12~20, and convex lens surrounds round bottom
Flask arrangement, light focusing point are located in round-bottomed flask solution everywhere.
Flake magnesium hydroxide and spherical method of magnesium oxide are prepared with rear magnesia, comprising the following steps:
(1) prepare containing B, S, Fe, Al with rear MgO raw material, B, S therein are removed by high-temperature process；
(2) the molten processing of acid is carried out to the MgO raw material formed after step (1) processing using HCl, formation contains MgCl2、Fe2+、
Al3+Liquid；
(3) H is used2O2Oxidation processes are carried out to the liquid formed after step (2) processing, by Fe2+It is converted to Fe3+, then will
Fe3+Conversion forms Fe (OH)3It precipitates and filters；
(4) liquid formed after step (3) processing is handled, by Al3+Conversion forms Al (OH)3It precipitates and filters；
(5) liquid formed after being handled as precipitating reagent step (4) using ammonium hydroxide is counter to be dripped, reaction process MgCl2+
NH3·H2O→Mg(OH)2Precipitating+2NH4Cl uses convex lens focal heat in titration process, is filtered, washed, is dried and ground
Sheet Mg (OH) is obtained after broken2Solid powder；
(6) the sheet Mg (OH) that step (5) are formed2It is calcined, by sheet Mg (OH)2Admittedly glomeration MgO is converted,
Reaction process is Mg (OH)2→MgO+H2O。
In step (5), material reaction ratio NH3·H2O:MgCl2It is 3.0~8.0, the reaction time is in 40~80min, drying
Temperature is 80~130 DEG C, and drying time is 100~150min.
In step (6), calcination temperature is 800~1000 DEG C, and calcination time is 90~150min.
The present invention has the advantages that
(1) using the device and method to silicon-steel grade magnesium oxide remaining black powder during producing grain-oriented Si steel sheet
It is recycled, solves the problems, such as that silicon steel manufacturing enterprise waste material is idle, waste recovery is recycled to being economical and environmentally friendly also one big
Contribution.
(2) optical principle is utilized, heat cooperation back titration is generated with the convex lens type of focusing, reaction is heated, directly
It connects using sunlight as the energy, does not consume other energy, process is environmentally protective, and sunlight is easy to get, high financial profit.
(3) molten by acid, clean, precipitate, being filtered, washed, after the processes such as drying and calcination, prepared ultra-fine sheet
Mg(OH)2With coccoid MgO product, particle size is small, large specific surface area, and the rate of recovery is up to 92%~98%, product form knot
Structure is stablized.
(4) raw material used in the present invention is easy to get, at low cost, and production principle and simple process, and instrument and equipment requirement is low, easily
It is industrialized in realizing.
Detailed description of the invention
Fig. 1 is that the structure of the device proposed by the present invention that flake magnesium hydroxide and spherical magnesia are prepared with rear magnesia is shown
It is intended to.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Diagram and specific embodiment are closed, the present invention is further explained.
As shown in Figure 1, the device packet proposed by the present invention for preparing flake magnesium hydroxide and spherical magnesia with rear magnesia
Supporting mechanism, titration mechanism, rabbling mechanism and heating mechanism, titration mechanism and rabbling mechanism is included to be installed on supporting mechanism,
Titrating has the space for accommodating ammonium hydroxide and the magnesium chloride liquid formed with rear magnesia through the molten removal of impurities processing of acid in mechanism, by titrating
Mechanism and heating mechanism carry out anti-drop operation and form magnesium hydrate precipitate, are carried out by heating mechanism to magnesium hydrate precipitate after washing
Heating, drying obtains flake magnesium hydroxide solid, and continues to obtain spherical magnesia to magnesium hydroxide solid heating and calcining.Support
Mechanism includes pedestal 1, and column 2 is fixed on pedestal, and column is fixed with hanging stick 3, hanging stick end to stretching above pedestal, top
With positioning ring 4；Titrating mechanism includes the separatory funnel 5 that can accommodate ammonium hydroxide, which is placed in positioning ring, separatory funnel
Lower section is equipped with the round-bottomed flask 6 that can accommodate magnesium chloride liquid, which is placed on pedestal, and the down tube 7 of separatory funnel protrudes into
In round-bottomed flask；Rabbling mechanism includes magnetic stirring apparatus 8, and magnetic stirring apparatus is placed between pedestal and round-bottomed flask, round-bottomed flask
Inside be placed with the stirrer 9 being adapted to magnetic stirring apparatus, by magnetic stirring apparatus driving stirrer to the liquid in round-bottomed flask into
Row stirring；Heating mechanism includes one group of convex lens 10 and calcining furnace, and convex lens is provided with 12~20, and convex lens surrounds round bottom
Flask arrangement, light focusing point are located in round-bottomed flask solution everywhere.
Flake magnesium hydroxide and spherical method of magnesium oxide are prepared with rear magnesia, comprising the following steps:
(1) prepare containing B, S, Fe, Al with rear MgO raw material, B, S therein are removed by high-temperature process；
(2) the molten processing of acid is carried out to the MgO raw material formed after step (1) processing using HCl, formation contains MgCl2、Fe2+、
Al3+Liquid；
(3) H is used2O2Oxidation processes are carried out to the liquid formed after step (2) processing, by Fe2+It is converted to Fe3+, then will
Fe3+Conversion forms Fe (OH)3It precipitates and filters；
(4) liquid formed after step (3) processing is handled, by Al3+Conversion forms Al (OH)3It precipitates and filters；
(5) liquid formed after being handled as precipitating reagent step (4) using ammonium hydroxide is counter to be dripped, reaction process MgCl2+
NH3·H2O→Mg(OH)2Precipitating+2NH4Cl uses convex lens focal heat in titration process, is filtered, washed, is dried and ground
Sheet Mg (OH) is obtained after broken2Solid powder；
(6) the sheet Mg (OH) that step (5) are formed2It is calcined, by sheet Mg (OH)2Admittedly glomeration MgO is converted,
Reaction process is Mg (OH)2→MgO+H2O。
In step (5), material reaction ratio NH3·H2O:MgCl2It is 3.0~8.0, the reaction time is in 40~80min, drying
Temperature is 80~130 DEG C, and drying time is 100~150min.
In step (6), calcination temperature is 800~1000 DEG C, and calcination time is 90~150min.
This method is, as raw material, after, removal of impurities molten through peracid, using ammonium hydroxide as precipitating reagent, to pass through control material with rear magnesia
NH is compared in reaction3·H2O:MgCl2When being 3.0~8.0, number of lenses is 12~20, and the reaction time is in 40~80min, drying temperature
It is 80~130 DEG C, drying time is 100~150min, prepares middle partial size (D50) in 1 μm of sheet Mg (OH) below2,
Wherein D50 is only 0.45~0.75 μm the smallest, and specific surface area is up to 3.50~5.50m2/ g, the rate of recovery are also up to
92%~98%, and the crystalline structure of product is stablized, it is impure less.When calcination temperature is 800~1000 DEG C, calcination time is
When 90~150min, sheet Mg (OH)2It will become spherical magnesia.
Embodiment of above only technical concepts and features to illustrate the invention, its object is to allow those skilled in the art
Member understands the contents of the present invention and is implemented, and it is not intended to limit the scope of the present invention, all spiritual according to the present invention
The equivalent change or modification that essence is done, should be covered by the scope of protection of the present invention.
Claims (5)
1. preparing the device of flake magnesium hydroxide and spherical magnesia with rear magnesia, it is characterised in that:
Support machine is installed in including supporting mechanism, titration mechanism, rabbling mechanism and heating mechanism, titration mechanism and rabbling mechanism
On structure, titrating has the space for accommodating ammonium hydroxide and the magnesium chloride liquid formed with rear magnesia through the molten removal of impurities processing of acid in mechanism,
Anti- drop operation is carried out by titration mechanism and heating mechanism and forms magnesium hydrate precipitate, is sunk by heating mechanism to magnesium hydroxide after washing
The progress heating, drying that forms sediment obtains flake magnesium hydroxide solid, and continues to obtain spherical oxidation to magnesium hydroxide solid heating and calcining
Magnesium.
2. the device according to claim 1 for preparing flake magnesium hydroxide and spherical magnesia with rear magnesia, feature
It is:
Supporting mechanism includes pedestal, and column is fixed on pedestal, and column is fixed with hanging stick to stretching above pedestal, top, hangs
Bar end has positioning ring；
Titrating mechanism includes the separatory funnel that can accommodate ammonium hydroxide, which is placed in positioning ring, is equipped with below separatory funnel
The round-bottomed flask of magnesium chloride liquid can be accommodated, which is placed on pedestal, and the down tube of separatory funnel protrudes into round-bottomed flask；
Rabbling mechanism includes magnetic stirring apparatus, and magnetic stirring apparatus is placed between pedestal and round-bottomed flask, is placed in round-bottomed flask
The stirrer being adapted to magnetic stirring apparatus is stirred the liquid in round-bottomed flask by magnetic stirring apparatus driving stirrer；
Heating mechanism includes one group of convex lens and calcining furnace, and convex lens is provided with 12~20, and convex lens surrounds round-bottomed flask
Arrangement, light focusing point are located in round-bottomed flask solution everywhere.
3. preparing flake magnesium hydroxide and spherical method of magnesium oxide with rear magnesia, which comprises the following steps:
(1) prepare containing B, S, Fe, Al with rear MgO raw material, B, S therein are removed by high-temperature process；
(2) the molten processing of acid is carried out to the MgO raw material formed after step (1) processing using HCl, formation contains MgCl2、Fe2+、Al3+
Liquid；
(3) H is used2O2Oxidation processes are carried out to the liquid formed after step (2) processing, by Fe2+It is converted to Fe3+, then by Fe3+Turn
Change forms Fe (OH)3It precipitates and filters；
(4) liquid formed after step (3) processing is handled, by Al3+Conversion forms Al (OH)3It precipitates and filters；
(5) liquid formed after being handled as precipitating reagent step (4) using ammonium hydroxide is counter to be dripped, reaction process MgCl2+NH3·
H2O→Mg(OH)2Precipitating+2NH4Cl uses convex lens focal heat in titration process, after being filtered, washed, dried and being ground
Obtain sheet Mg (OH)2Solid powder；
(6) the sheet Mg (OH) that step (5) are formed2It is calcined, by sheet Mg (OH)2Admittedly converting glomeration MgO, reaction
Process is Mg (OH)2→MgO+H2O。
4. according to claim 3 prepare flake magnesium hydroxide and spherical method of magnesium oxide, feature with rear magnesia
It is:
In step (5), material reaction ratio NH3·H2O:MgCl2It is 3.0~8.0, the reaction time is in 40~80min, drying temperature
It is 80~130 DEG C, drying time is 100~150min.
5. according to claim 3 prepare flake magnesium hydroxide and spherical method of magnesium oxide, feature with rear magnesia
It is:
In step (6), calcination temperature is 800~1000 DEG C, and calcination time is 90~150min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113620323A (en) * | 2021-08-17 | 2021-11-09 | 上海应用技术大学 | Preparation method of flame retardant magnesium hydroxide |
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| CN113620323A (en) * | 2021-08-17 | 2021-11-09 | 上海应用技术大学 | Preparation method of flame retardant magnesium hydroxide |
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Application publication date: 20190712 |