CN102491380A - Method for preparing flaky magnesium hydroxide - Google Patents
Method for preparing flaky magnesium hydroxide Download PDFInfo
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- CN102491380A CN102491380A CN2011104017173A CN201110401717A CN102491380A CN 102491380 A CN102491380 A CN 102491380A CN 2011104017173 A CN2011104017173 A CN 2011104017173A CN 201110401717 A CN201110401717 A CN 201110401717A CN 102491380 A CN102491380 A CN 102491380A
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Abstract
The invention relates to a method for preparing flaky magnesium hydroxide. The method comprises the following steps of: (1) roasting mineral resources of magnesium carbonate to obtain light-roasting magnesium oxide; (2) mixing the light-roasting magnesium oxide prepared in the step (1) with a grinding aid and water to obtain slurry; (3) performing mechanical ball-milling on the slurry prepared in the step (2); (4) aging the slurry processed in the step (3) at room temperature; and (5) performing solid-liquid separation on the slurry aged in the step (4), washing and drying to obtain flaky magnesium hydroxide granules. According to the method, alkali is not needed to be added, the production cost is saved, the requirement of equipment is reduced, and more important, hydro-thermal treatment is avoided in the process, so a process flow is shortened greatly, and the energy consumption of production and the investment of the equipment are reduced. The magnesium hydroxide prepared by the method can be widely applied in fields of materials, chemical industry, environment and the like.
Description
Technical field
The present invention relates to a kind of preparation method of Marinco H, relate in particular to a kind of mechanical ball milling legal system of utilizing and be equipped with flake magnesium hydroxide particulate method.
Background technology
Magnesite is the high-quality Mineral resources of China, and its output, reserves, export volume all occupy first place in the world.Domestic development and use to magnesite are main with primary products such as production light-burning magnesium powders still, are difficult to bring into play this resources advantage but at present.Therefore, the high-efficiency comprehensive utilization magnesite resource, the exploitation high value added product is the important directions of the magnesia utilization of resources of current China.
Marinco H is a kind of novel inorganic fire retardant newly developed in recent years, have that decomposition temperature is higher, Heat stability is good, nontoxic, smokelessly, do not produce characteristics such as corrosive gases.Flake magnesium hydroxide is more suitable for fire-retardant usefulness owing to having iris action.At present, the preparation method of flake magnesium hydroxide mainly contains: seawater, bittern and soluble magnesium salt alkaline precipitation; The Natural manganese dioxide hydrothermal crystallization method; Magnesium-containing ore or salt through roasting, add the buck method.
CN 1541943 A disclose a kind of preparation method of ultra-fine high dispersing magnesium hydrate; This method is that the aqueous solution with bittern or inorganic water-soluble magnesium salt is raw material; Under whipped state, add precipitation agent and the properties-correcting agent that is pre-mixed; Be reaction 10-60 minute under 20 ℃-90 ℃ the condition in temperature, with reacting liquid filtering, washing, drying, get product again.
CN 102101684 A disclose a kind of alkali and have strengthened the method for preparing the submicron flake magnesium hydroxide: Natural manganese dioxide, alkali, dispersion agent and water are mixed into slip by a certain percentage; Process crystallization through the mechanochemistry processing and use slip; Hydrothermal crystallizing; The product solid-liquid separation, solids wash, the dry submicron hydroxide flake magnesium dust that gets.
CN 1944260 A disclose a kind of method of utilizing preparing super fine magnesium hydroxide by wet method from brucite, and relating to the natural crystal is the method for feedstock production super fine magnesium hydroxide powder.Concrete steps are: (1) obtained magnesia powder with brucite powder in 1～3 hour 450 ℃～700 ℃ calcinings earlier; The fineness of brucite powder is 325 orders; (2) in the Natural manganese dioxide of 100 weight parts, add the trolamine of 1 weight part, the absolute ethyl alcohol ball milling of 200～300 weight parts 24 hours; (3) water that adds 100～200 weight parts continued ball milling 12 hours; (4) slurry is at 120 ℃ of convection dryings, pulverize median size in the Marinco H ultrafine powder of 370～500 nanometers.
Utilize the productive rate of seawater, bittern and soluble magnesium salt alkaline precipitation production Marinco H very low.Utilize the Natural manganese dioxide hydrothermal crystallization method to produce the raw materials cost height of Marinco H, complex process.Magnesite through calcining, adding the buck legal system, to be equipped with the method technology of flake magnesium hydroxide simple, but exogenously added alkali solution has increased production cost, and reaction process is difficult to control and will produces a large amount of coacervates.
Mechanochemical reaction (claiming high-energy ball milling again) is a kind of effective ways that prepare nano material commonly used in recent years; It is the different effects mode through the high-energy mechanical force; Like shearing, friction, compression and impact etc.; The physicochemical property of stressed material (solid, liquid or gas) are changed, thereby improve its reactive behavior, make the phenomenon of solid in material and the surrounding environment, liquid, gas generation chemical transformation.Mechanochemical reaction is simple because of its technology, efficient is high and adapt to suitability for industrialized production is widely used.
Summary of the invention
Deficiency to prior art; The present invention provides a kind of mechanical ball milling legal system of utilizing to be equipped with flake magnesium hydroxide particulate method, does not need the participation of alkali, has not only saved production cost but also has reduced equipment requirements; The present invention does not simultaneously need hydrothermal treatment consists; Therefore shortened technical process widely, reduced the energy consumption and the facility investment of producing, technology is simple, cost is low, be easy to the method for scale prodn to be one.
The method for preparing flake magnesium hydroxide provided by the present invention comprises the steps:
(1) mineral resources of roasting magnesiumcarbonate obtains light calcined magnesia;
(2) light calcined magnesia that step (1) is made and grinding aid, water mixed slurry;
(3) the slurry mechanical ball milling that step (2) is made is handled;
(4) with ageing under the slurry room temperature after step (3) processing;
(5) with the slurry solid-liquid separation after step (4) ageing, washing, the dry hydroxide flake magnesium granules that gets.
As optimal technical scheme, the mineral resources of magnesiumcarbonate is selected from a kind of or two or more at least mixture in rhombspar, magnesite, hydromagnesite or the huntite described in the step (1), preferred magnesite, MgCO in the further preferred magnesite
3Mass content is more than 90%.
The appropriate sources of magnesiumcarbonate comprises rhombspar, magnesite, hydromagnesite or huntite.Rhombspar is miemite (CaMg (CO
3)
2), magnesite is MgCO
3, hydromagnesite has chemical formula Mg
5(CO
3)
4(OH)
24H
2O, huntite have chemical formula CaMg
3(CO
3)
4It is thus clear that giobertite is one of magnesian main source, the preferred magnesite of the mineral resources of magnesiumcarbonate, MgCO in magnesite
3Mass content is 90% when above, the pattern of gained Marinco H rule, homogeneous, and productive rate is high.
As optimal technical scheme, the mineral resources of magnesiumcarbonate described in the step (1) is through pulverizing, and preferred powder is broken to mean particle size less than 500 μ m.Before roasting, the mineral resources of magnesiumcarbonate is pulverized, can be obtained the fine light calcined magnesia after the roasting like this.
As optimal technical scheme, the maturing temperature described in the step (1) is lower than 1000 ℃, preferred 400～800 ℃; Preferably, described roasting apparatus comprises down-draft kiln, tunnel, rotary kiln, retort furnace, shaft furnace or fluidized-bed.
Calcining temperature is that decision MgO is active, the key of dispersity.No matter be magnesite, dolomite mineral etc. are any to be that raw material decomposition reaction in roasting is thermo-negative reaction.Owing to decomposite CO
2And H
2O makes MgO form not densification product of porous crack crystalline structure, and when temperature was 400～800 ℃ of roastings, the MgO activity that roasting goes out was good, and dispersity is big, and when maturing temperature was higher than 1000 ℃, gained MgO crystal densification dispersity was little.Therefore, controlling the temperature of roasting well is the key that makes quality oxide magnesium.Roasting process can carry out in the suitable device that includes but not limited to like down-draft kiln, tunnel, rotary kiln, retort furnace, shaft furnace or fluidized-bed etc.
As optimal technical scheme, the grinding aid described in the step (2) is silane coupling agent or nonionogenic tenside, a kind of or two or more at least mixture in preferred polyoxyethylene glycol, Vinylpyrrolidone polymer, Z 150PH, the T 46155 amine.Grinding aid is a kind of additive that improves mill efficiency.Be generally surfactant, have the specific surface energy of reduction and the fissured effect of " wedging " particle.Material is in the fine grinding process, and particle is refinement progressively, and specific surface area increases, and its surface is charged because of scission of link, and particle adsorbs each other and occurs reuniting, and crush efficiency is descended.Add a small amount of grinding aid, can prevent particle aggregation, improve material fluidity, thereby improve grinding efficiency, shorten milling time.Select silane coupling agent, polyoxyethylene glycol, Vinylpyrrolidone polymer, Z 150PH or T 46155 amine as grinding aid among the present invention, can reach good ball milling effect.
As optimal technical scheme, the mass ratio of the light calcined magnesia described in the step (2), grinding aid, water is 1: 0.001～0.2: 5～40, and the mass ratio of preferred light calcined magnesia, grinding aid, water is 1: 0.01～0.1: 5～20.
As optimal technical scheme, the ball-milling processing time described in the step (3) is 15min～24h, preferred 1h～10h; Preferably, the ball-to-powder weight ratio during said ball-milling processing is 5～40, preferred 20～40.
As optimal technical scheme, the mechanical ball milling described in the step (3) is handled and is adopted intermittently ball milling or ball milling continuously.
Ball milling be shock action and the grinding element of the grinding element (like steel ball, pebbles etc.) that utilizes with the grinding of ball milling inwall with the material pulverizing and mix, be a kind of high efficiency mechanochemical reaction.Utilization ball milling at intermittence or continuous ball milling all can reach the effect of mechanical ball milling.
In general, the ball milling time is long more, and powder can be thin more, should prolong the ball milling time as much as possible, but ball milling can be introduced more impurity on the one hand for a long time, can reduce grinding efficiency on the other hand.Therefore in order to take into account efficient and ball milling quality, it is 15min～24h that the present invention selects the ball-milling processing time, preferred 1h～10h.The ball-to-powder weight ratio of ball mill is exactly the quality of grinding element in the mill and the ratio of quality of material.Its explanation under certain grinding element tonburden in the grinding process in the mill material stock amount how much, the uniform degree of feeding under ball mill normal operation situation also is described.Ball-to-powder weight ratio is too big, can increase between the grinding element and the idle work loss of impact friction between grinding element and the liner plate, and power consumption is increased, and output reduces; If ball-to-powder weight ratio is too little, explain that material stock is too much in the mill, will produce shock absorption, also can reduce mill efficiency.Therefore, the present invention is 5～40 through verification experimental verification selection ball-to-powder weight ratio.
As optimal technical scheme, the aged time described in the step (4) is 0.1h～100h, preferred 2h～30h, further preferred 5h～20h.After deposition is complete, let the deposition that just generates place for some time with mother liquor, this process is called " ageing ".The one side of its effect is to remove the impurity that contains in the deposition.Be to let the deposition crystal growth increase crystal particle diameter on the other hand, and make its size distribution more even.The present invention is 0.1h～100h in order to take into account efficient and aged time of ageing effect selection, preferred 2h～30h, further preferred 5h～20h.
As optimal technical scheme, it is characterized in that the solid-liquid separation described in the step (5) adopts press filtration or centrifugal.Preferably, described washing with washing, is washed with organic solvent earlier again; Preferably, said solvent is the less or non-polar organic solvent of polarity, further particular methanol or ethanol or acetone, or its mixture.Product after the washing makes that Marinco H is difficult for reuniting in the drying process like this.Solid-liquid separation of the present invention includes but not limited to press filtration or centrifugal, such as being separation modes such as sedimentation, filtration.
The present invention proposes to utilize the mechanical ball milling legal system to be equipped with the nano-sheet magnesium hydroxide particle; This technological advantage is following: (1) utilizes mechanical ball milling that the light calcined magnesia reactive behavior is increased; Realize that light calcined magnesia with water hydration reaction takes place apace under the situation of not adding alkaline solution, not only saved material cost of producing but also the requirement that has reduced the equipment resistance to acids and bases; (2) utilize mechanical ball milling can improve the dispersed characteristics of material, when hydration reaction carries out, improve the dispersing property of product; (3) slurry that obtains through mechanical ball milling only needs ageing for some time under the room temperature, does not need hydrothermal treatment consists just can obtain the nano-sheet magnesium hydroxide particle, thereby has reduced the energy consumption and the facility investment of producing.The magnesium hydroxide particle that makes with this technology is the hexagonal flake of rule, and primary particle size is about 200～300nm.Product of the present invention all can be used in a plurality of fields such as material, chemical industry and environment.
The invention solves the defective of traditional hydration prepared in reaction Marinco H, problems such as long like the reaction times, transformation efficiency is low, need hydrothermal treatment consists.Through making full use of mechanochemical treatment, reduced reactant magnesium oxide particle granularity, increase its surfactivity, and then impelled carrying out fast of magnesian hydration reaction.Do not need the participation of exogenously added alkali among the present invention, need not pass through the hydrothermal treatment consists process and just can prepare dispersiveness nano-sheet Marinco H preferably.This technology has been simplified the preparation process of nano-sheet Marinco H greatly, has shortened technical process, and greatly reduces production cost and energy consumption.Product of the present invention all can be used in a plurality of fields such as material, chemical industry and environment.
Description of drawings
Fig. 1 prepares the process flow sheet of flake magnesium hydroxide.
The XRD figure of the flake magnesium hydroxide of Fig. 2 embodiment of the invention 1 preparation.
The SEM figure of the flake magnesium hydroxide of Fig. 3 embodiment of the invention 1 preparation.
Embodiment
For ease of understanding the present invention, it is following that the present invention enumerates embodiment.Those skilled in the art should understand, and said embodiment only is used for helping to understand the present invention, should not be regarded as concrete restriction of the present invention.
Fig. 1 prepares the process flow sheet of flake magnesium hydroxide for the present invention.
Embodiment one
The Natural manganese dioxide that adopts is that (Haicheng City decorated archway magnesium ore deposit, Liaoning Province ltd provides by magnesite; The content of magnesiumcarbonate is 97.87wt%) obtain at 650 ℃ of calcining 3.5h, above-mentioned magnesium oxide powder 15.0g is mixed with 0.45g PEG 400 and 270ml deionized water; Transfer in the 500ml resin ball grinder, utilize zirconia balls (be ball-to-powder weight ratio be 20: 1) the mechanical ball milling 8h of 300g diameter for 3mm, rotating speed is 400r/min; With ageing 12h under the slurry room temperature of gained, suction filtration washs respectively 2 times with deionized water and absolute ethyl alcohol then, and dry 3h in 110 ℃ baking oven obtains the target Marinco H, and Fig. 2 and Fig. 3 are respectively its XRD figure and SEM figure.
Embodiment two
Getting the light calcined magnesia 3.0g that obtains among the embodiment one mixes with 0.154g silane coupling agent KH560 and 18ml deionized water; Transfer in the 500ml resin ball grinder, utilize zirconia balls (be ball-to-powder weight ratio be 30: 1) the mechanical ball milling 4h of 90g diameter for 3mm, rotating speed is 400r/min; With ageing 100h under the slurry room temperature of gained, suction filtration washs respectively 2 times with deionized water and absolute ethyl alcohol then, and dry 3h in 110 ℃ baking oven obtains the target Marinco H.
Embodiment three
Getting the light calcined magnesia 5.0g that obtains among the embodiment one mixes with 0.05g Vinylpyrrolidone polymer and 50ml deionized water; Transfer in the 500ml resin ball grinder, utilize zirconia balls (be ball-to-powder weight ratio be 40: 1) the mechanical ball milling 2h of 200g diameter for 3mm, rotating speed is 400r/min; With ageing 0.1h under the slurry room temperature of gained, suction filtration washs respectively 2 times with deionized water and absolute ethyl alcohol then, and dry 3h in 110 ℃ baking oven obtains the target Marinco H.
Applicant's statement; The present invention explains detailed process equipment of the present invention and technical process through the foregoing description; But the present invention is not limited to above-mentioned detailed process equipment and technical process, does not mean that promptly the present invention must rely on above-mentioned detailed process equipment and technical process could be implemented.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. the preparation method of a flake magnesium hydroxide comprises the steps:
(1) mineral resources of roasting magnesiumcarbonate obtains light calcined magnesia;
(2) light calcined magnesia that step (1) is made and grinding aid, water mixed slurry;
(3) the slurry mechanical ball milling that step (2) is made is handled;
(4) with ageing under the slurry room temperature after step (3) processing;
(5) with the slurry solid-liquid separation after step (4) ageing, washing, the dry hydroxide flake magnesium granules that gets.
2. the method for claim 1; It is characterized in that; The mineral resources of magnesiumcarbonate is selected from a kind of or two or more at least mixture in rhombspar, magnesite, hydromagnesite or the huntite described in the step (1), preferred magnesite, MgCO in the further preferred magnesite
3Mass content is more than 90%.
3. according to claim 1 or claim 2 method is characterized in that, the mineral resources of magnesiumcarbonate described in the step (1) is through pulverizing, and preferred powder is broken to mean particle size less than 500 μ m.
4. like each described method of claim 1～3, it is characterized in that the maturing temperature described in the step (1) is lower than 1000 ℃, preferred 400～800 ℃;
Preferably, described roasting apparatus comprises down-draft kiln, tunnel, rotary kiln, retort furnace, shaft furnace or fluidized-bed.
5. like each described method of claim 1～4; It is characterized in that; Grinding aid described in the step (2) is silane coupling agent or nonionogenic tenside, a kind of or two or more at least mixture in preferred polyoxyethylene glycol, Vinylpyrrolidone polymer, Z 150PH, the T 46155 amine.
6. like each described method of claim 1～5; It is characterized in that; The mass ratio of the light calcined magnesia described in the step (2), grinding aid, water is 1: 0.001～0.2: 5～40, and the mass ratio of preferred light calcined magnesia, grinding aid, water is 1: 0.01～0.1: 5～20.
7. like each described method of claim 1～6, it is characterized in that the ball-milling processing time described in the step (3) is 15min～24h, preferred 1h～10h;
Preferably, the ball-to-powder weight ratio during said ball-milling processing is 5～40, preferred 20～40.
8. like each described method of claim 1～7, it is characterized in that the mechanical ball milling described in the step (3) is handled and adopted intermittently ball milling or ball milling continuously.
9. like each described method of claim 1～8, it is characterized in that the aged time described in the step (4) is 0.1h～100h, preferred 2h～30h, further preferred 5h～20h.
10. like each described method of claim 1～9, it is characterized in that the solid-liquid separation described in the step (5) adopts press filtration or centrifugal;
Preferably, described washing with washing, is washed with organic solvent earlier again;
Preferably, said solvent is the less or non-polar organic solvent of polarity, further particular methanol or ethanol or acetone, or its mixture.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015051482A1 (en) * | 2013-10-11 | 2015-04-16 | 河北联合大学 | Method for manufacturing sheet monodisperse nano-magnesium hydroxide by using magnesite |
| CN106115748A (en) * | 2016-06-16 | 2016-11-16 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN106587119A (en) * | 2016-12-24 | 2017-04-26 | 天津大学 | Method for preparing hexagonal flake magnesium hydroxide with dominant growth on (001) crystal face |
| CN107344727A (en) * | 2017-06-09 | 2017-11-14 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of hexagonal plate nano-sized magnesium hydroxide material |
| CN107858747A (en) * | 2017-08-04 | 2018-03-30 | 华北理工大学 | A kind of method that magnesia hydro-thermal prepares hydroxide nanoparticle film |
| CN108706612A (en) * | 2018-07-04 | 2018-10-26 | 河南师范大学 | A kind of method that mechanical ball mill prepares nano-sized magnesium hydroxide |
| CN110342552A (en) * | 2019-08-16 | 2019-10-18 | 大连环球矿产股份有限公司 | A kind of method that chemical method prepares active micron/nanometer flame retardant of magnesium hydroxide |
| CN110357131A (en) * | 2019-08-08 | 2019-10-22 | 中国地质大学（北京） | A kind of nano-sized magnesium hydroxide slurry and its preparation method and application |
| CN110436598A (en) * | 2019-08-08 | 2019-11-12 | 中国地质大学（北京） | Application of the ammonium magnesium phosphate/nano-sized magnesium hydroxide in processing heavy metal-containing waste water |
| CN114394611A (en) * | 2022-01-21 | 2022-04-26 | 洛阳中超新材料股份有限公司 | Preparation method of high-aspect-ratio flaky magnesium hydroxide |
| CN115611298A (en) * | 2022-09-30 | 2023-01-17 | 中国科学院青海盐湖研究所 | Preparation method of battery-grade nano magnesium oxide |
| CN115924942A (en) * | 2022-12-30 | 2023-04-07 | 郑州大学 | Method for preparing high-purity flaky magnesium hydroxide by hydration of microcrystalline magnesite |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015051482A1 (en) * | 2013-10-11 | 2015-04-16 | 河北联合大学 | Method for manufacturing sheet monodisperse nano-magnesium hydroxide by using magnesite |
| CN104968605A (en) * | 2013-10-11 | 2015-10-07 | 华北理工大学 | Method for manufacturing sheet monodisperse nano-magnesium hydroxide by using magnesite |
| CN104968605B (en) * | 2013-10-11 | 2016-10-12 | 华北理工大学 | Magnesite prepares the method for lamellar dispersed nano magnesium hydroxide |
| CN106115748A (en) * | 2016-06-16 | 2016-11-16 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN106115748B (en) * | 2016-06-16 | 2018-01-09 | 东升新材料（山东）有限公司 | A kind of method of preparing super fine magnesium hydroxide by wet method slurry |
| CN106587119A (en) * | 2016-12-24 | 2017-04-26 | 天津大学 | Method for preparing hexagonal flake magnesium hydroxide with dominant growth on (001) crystal face |
| CN107344727A (en) * | 2017-06-09 | 2017-11-14 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of hexagonal plate nano-sized magnesium hydroxide material |
| CN107858747B (en) * | 2017-08-04 | 2019-12-10 | 华北理工大学 | Method for preparing magnesium hydroxide nano film by magnesium oxide hydrothermal method |
| CN107858747A (en) * | 2017-08-04 | 2018-03-30 | 华北理工大学 | A kind of method that magnesia hydro-thermal prepares hydroxide nanoparticle film |
| CN108706612A (en) * | 2018-07-04 | 2018-10-26 | 河南师范大学 | A kind of method that mechanical ball mill prepares nano-sized magnesium hydroxide |
| CN110357131A (en) * | 2019-08-08 | 2019-10-22 | 中国地质大学（北京） | A kind of nano-sized magnesium hydroxide slurry and its preparation method and application |
| CN110436598A (en) * | 2019-08-08 | 2019-11-12 | 中国地质大学（北京） | Application of the ammonium magnesium phosphate/nano-sized magnesium hydroxide in processing heavy metal-containing waste water |
| CN110342552A (en) * | 2019-08-16 | 2019-10-18 | 大连环球矿产股份有限公司 | A kind of method that chemical method prepares active micron/nanometer flame retardant of magnesium hydroxide |
| CN110342552B (en) * | 2019-08-16 | 2021-12-10 | 大连环球矿产股份有限公司 | Method for preparing active micro-nano magnesium hydroxide flame retardant by chemical method |
| CN114394611A (en) * | 2022-01-21 | 2022-04-26 | 洛阳中超新材料股份有限公司 | Preparation method of high-aspect-ratio flaky magnesium hydroxide |
| CN115611298A (en) * | 2022-09-30 | 2023-01-17 | 中国科学院青海盐湖研究所 | Preparation method of battery-grade nano magnesium oxide |
| CN115924942A (en) * | 2022-12-30 | 2023-04-07 | 郑州大学 | Method for preparing high-purity flaky magnesium hydroxide by hydration of microcrystalline magnesite |
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Application publication date: 20120613 |