CN1458066A - Process for preparing magnesium hydroxide whisker - Google Patents
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- CN1458066A CN1458066A CN 02109685 CN02109685A CN1458066A CN 1458066 A CN1458066 A CN 1458066A CN 02109685 CN02109685 CN 02109685 CN 02109685 A CN02109685 A CN 02109685A CN 1458066 A CN1458066 A CN 1458066A
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Abstract
The process of preparing magnesium hydroxide whisker features that the material magnesium salt whisker MgSO4.5Mg(OH)2.3H2O is made to react with the water solution of hydroxide of ammonia, alkali metal or alkali earth metal to obtain magnesium hydroxide whisker. The preparation process uses rich and low cost magnesite resource and prepares magnesium hydroxide whisker from magnesium salt whisker, resulting in short production period, high production efficiency and no serious corrosion of apparatus by chloride. In addition, the preparation process has simple process, low cost and no environmental pollution and is suitable for industrial production.
Description
Technical field:
The present invention relates to the preparation method of Preparation of Whiskers technology, particularly magnesium hydroxide crystal whisker.
Technical background:
Magnesium hydroxide can be widely used in every field: can make it have flame retardant resistance as adding thermoplastic resin.But magnesium hydroxide commonly used is the powder shape, when utilizing it to obtain flame retardant effect, but can obviously reduce the physicals and the mechanical property of material, makes resin flow and forming property variation, forming efficiency and molding degraded appearance.Analyze its reason, be because magnesium hydroxide crystallization particle diameter is little, specific surface is bigger, the polarity of crystal surface is bigger, the normal secondary aggregation structure that forms water content in the crystallization, even residual and the water molecules and the air work in-process that are adsorbed in this aggregate, also be difficult to remove by drying, thereby can cause with the affinity of thermoplastic resin poor, have a strong impact on dispersiveness to resin, form the gap between resin and magnesium hydroxide particles interface easily, make physicals particularly shock strength and unit elongation decline.Simultaneously, water molecules that exists in the secondary agglomeration and air are emitted when being shaped, and can form burr influences products appearance, and the high proportion of secondary agglomeration is little, and when resin extruded shaping, reinforced operational difficulty is difficult for homodisperse.
In technology in the past, for addressing the above problem, once new texture was made in trial, (particle diameter is at 800A-10000A, and specific surface is at 1-20M for large-size crystalline magnesium hydroxide
2/ g.), so that its secondary aggegation reduces, dispersiveness improves, method as the clear 52-115799 of patent JP is with magnesium chloride or magnesium nitrate and alkaline matter, in the water-based medium, amount (concentration), particularly alkali number by regulating magnesium chloride or magnesium nitrate and its ratio equivalent (0.5～0.95) carry out the hydro-thermal compressive reaction and generate basic magnesium chloride or magnesium nitrate: Mg (OH)
2-xA
x.mH
2(in the formula, A is C1 or NO to O
3, 0＜x＜1, m=0～6), then in the water-based medium heating (150～250 ℃), the pressurization (pressure is at 5Kg/cm
2More than, 5～30Kg/cm according to appointment
2) under, the Mg (OH) of generation new texture
2But this method has used the aqueous chloride solution of high density to make raw material, and the technological operation heating and pressurizing is very serious to the reactor equipment corrosion.And for example the flat 4-362012 of patent JP has adopted ultrasonic generator to mix device in order to obtain the magnesium hydroxide of polymolecularity, use to pulverize, specific surface is at 3～20M
2The light calcined magnesia adding of/g contains the solution of certain density organic acid and/or its magnesium salts, and maintains the temperature at more than 50 ℃, the limit ultrasonic stirring, and specific surface is filtered and got to the limit hydration reaction at 2～10M with the gained magnesium hydroxide slurries
2The magnesium hydroxide powdery crystallization of/g.But the magnesium hydroxide that above-mentioned all methods obtain all is granular, and when when improving flame retardant resistance and join in the resin large usage quantity, the mechanical property of material still can not get guaranteeing.In clear 54-112400 of patent JP and the clear 58-130248 of JP, also once introduced the method for making fibrous magnesium hydroxide, be to utilize the alkaline magnesium chloride that is similar to the resulting needle crystal of the clear 52-115799 method of patent JP, do not losing under its acicular condition, drying makes it slough partial crystallization water, again with this drying treatment thing, in the water liquid of this compound (or do not dissolve), contact and generate with alkali.And emphasize under the situation that crystal water is sloughed fully or do not sloughed fully, can not generate desired fibrous magnesium hydroxide.The problem of this method is: the problem of this method is: 1. used the high concentration cl compound big to the synthesis reaction vessel equipment corrosion; 2. must the thermal treatment drying slough partial crystallization water before contacting alkali; 3. to form the alkaline magnesium chloride intermediate necessary " slaking " of needle crystal earlier, required time long (more than at least 18 hours), and the needle crystal instability that forms, very easily revert to granular crystal, be difficult to obtain fibrous magnesium hydroxide stable, that length-to-diameter ratio is big.
Summary of the invention:
The object of the present invention is to provide a kind of magnesium hydroxide crystal whisker and preparation method thereof, magnesium hydroxide crystal whisker with this method preparation easily disperses in the course of processing of resin material, when improving the Flame Retardancy energy, can also improve the mechanical property of material, and the preparation method is easy, with low cost, non-environmental-pollution is applicable to industrial mass manufacture.
The invention provides a kind of preparation method of magnesium hydroxide crystal whisker, it is characterized in that: with magnesium salt whisker MgSO
4.5Mg (OH)
2.3H
2O is a raw material, reacts by the hydroxide aqueous solution with ammonia, basic metal or alkaline-earth metal, obtains magnesium hydroxide crystal whisker.
Among the preparation method of magnesium hydroxide crystal whisker of the present invention, used alkali preferably is selected from sodium hydroxide, potassium hydroxide or Qing Yangization : add alkali molar equivalent by normal 1～4 times of equivalent of the contained anion sulfate acid root of magnesium salt whisker, be preferably 1.2～2 times of equivalents.
Among the preparation method of magnesium hydroxide crystal whisker of the present invention, temperature of reaction is preferably in 40～100 ℃ in room temperature～200 ℃.
Among the preparation method of magnesium hydroxide crystal whisker of the present invention, reaction process need add stirring, and speed per minute 10～120 changes, and preferably per minute 20～80 changes.
Among the preparation method of magnesium hydroxide crystal whisker of the present invention, described magnesium salt whisker MgSO
4.5Mg (OH)
2.3H
2O obtains (CN99113254.8) by sparry magnesite and sal epsom or sulfuric acid hydro-thermal reaction, and in MgO, when adding sal epsom, its mol ratio is 1～5, and when adding sulfuric acid, mol ratio is 2～6; 100～250 ℃ of temperature of reaction, generated time 30 minutes～10 hours.
In the preparation method of above-mentioned magnesium salt whisker, sparry magnesite should be re-used as the raw material of hydro-thermal reaction after 750～1000 ℃ of calcination, the alkali magnesium sulfate crystal seed that can also add 0.1～4wt% during hydro-thermal reaction is done promotor.
The inventor finds in the making processes of research magnesium salt whisker (CN99113254.8): this single crystal fiber is made easily, and length-to-diameter ratio is big and very stable.The contriver further to magnesium salt whisker research, adds suitable normal alkali lye, and under proper temperature, agitation condition, displaces the whole sulfate radicals in the magnesium salt whisker, has made stable whiskers fiber---magnesium hydroxide crystal whisker, thereby has finished the present invention.
The new texture whiskers fiber magnesium hydroxide crystal whisker that the inventive method provided, zero defect almost in the lattice, have higher physicals and mechanical property, the surface is nonpolarity, does not produce the secondary aggegation, easily disperse, high proportion is bigger, and when cooperating thermoplastic resin, processing performance is good, when guaranteeing flame retardant properties, can also improve the mechanical property of material.And be easy to suitability for industrialized production, help using.Be the good toughener of plastics, fire retardant, the tackifier of coating, good filtering material and auxiliary agent etc.Can be widely used in fields such as automobile, electric, mechanical, chemical industry and building.
Preparation method's of the present invention advantage is: 1. synthesis material has used the abundant ore source magnesite of China, and it is with low cost; 2. after adopting the generation magnesium salt whisker, add alkaline matter, control adds the method for alkali number (mol ratio), concentration, temperature, stirring velocity and prepares magnesium hydroxide crystal whisker; 3. need not spend long-time " slaking " to form alkaline magnesium chloride needle crystal, also not be used in to heat-treat before the alkaline purification and take off crystal water and change crystalline structure, shorten the production cycle, improve production efficiency; 4. avoided the heavy corrosion that in the past brought to equipment with the high concentration chloride method.Preparation technology provided by the invention in addition, method is easy, with low cost, and non-environmental-pollution is applicable to industrial mass manufacture.
Description of drawings:
Fig. 1. the magnesium salt whisker stereoscan photograph;
Fig. 2. the magnesium hydroxide crystal whisker stereoscan photograph;
Fig. 3. prepare magnesium hydroxide crystal whisker x-ray diffraction pattern comparison diagram by magnesium salt whisker.
Embodiment:
1. with China the Northeast special product sparry magnesite through 750～1000 ℃ of calcination, pulverizing, its product (MgO content is more than 90%) adds the slurries that water mill becomes, and removes throw out and impurity, makes raw material with it;
2. solutes content in content of magnesia and the magnesium sulfate solution (or aqueous sulfuric acid) joins in the reactor with suitable mol ratio dosage in the slurries that 1. are prepared into set by step, mixes;
3. the alkali magnesium sulfate crystal seed that adds 0.1～4wt.% in reactor is done promotor;
4. under 100～250 ℃ of temperature and hydrostaticpressure, synthesized 30 minutes～10 hours;
5. washing is filtered.Get magnesium salt whisker MgSO
4.5Mg (OH)
2.3H
2O.
In 1.～5. step, it is to be noted especially: the A. raw material adopts sparry magnesite (proportion is 2.9～3.1), and calcining is pulverized at 750～1000 ℃.As be higher than 1200 ℃ of calcinings, should not be as the slurries raw material; B. dispersive MgO concentration can not be greater than 30wt.% in magnesium sulfate solution or aqueous sulfuric acid for raw slurry, not so, and because of the mixed solution thickness that can become in synthetic influences whisker growth; C. will control proportion of raw materials well, to adding the raw slurry in the magnesium sulfate solution, its mol ratio is 1～5 better, and 2～4 is good; To adding the slurries of aqueous sulfuric acid, mol ratio is 2～6 better, and 3～5 is good.Mol ratio has remaining particle greater than the specified upper limit after the building-up reactions, be difficult to remove, and influences the whisker quality; And mol ratio is less than specified lower limit, has too much sal epsom can not participate in reaction and causes wastage of material, and yield is reduced; D. (0.1～4wt.%), to promote whisker growth, the reduction synthesis temperature improves whisker quality and yield preferably will to add an amount of nucleus promotor in mixed solution; E. synthesis reaction temperature is advisable at 100～250 ℃.Be lower than 100 ℃, be unfavorable for whisker growth, the reaction times is long, and effect is bad, is higher than 250 ℃, and reacting kettle inner pressure is big, and equipment configuration is required height, and energy consumption is big, is unfavorable for producing.
6. the magnesium salt whisker of gained is put into reactive tank, add alkali lye by suitable mol ratio;
7. under proper temperature and stirring velocity, reacted 30 minutes～10 hours;
8. drying is filtered in washing.
In 6., 7. step was operated, used alkali had alkaline aqueous solutions such as ammonia, ammonium hydroxide, calcium hydroxide, sodium hydroxide, potassium hydroxide.Preferably utilize facile liquid caustic soda such as ammonium hydroxide, sodium hydroxide, potassium hydroxide.Add alkali lye concentration be not particularly limited, but had better not cross rare or overrich, can be preferably between 1～10mol/L in 0.2～20mol/L scope.The molar equivalent that adds alkali by normal about 1～4 times of equivalent of the contained anion sulfate acid root of magnesium salt whisker for well, add one times of equivalent of less than, can not generate the magnesium hydroxide crystal whisker of new texture fully, add and surpass 4 times of equivalents, can not obtain better effect, also can cause the waste of alkali number, be preferably 1.2～2 times of equivalents; Temperature of reaction can be in room temperature, but needs the long period, is preferably in more than 40 ℃, carries out below 100 ℃.Add stirring and can improve speed of response, shorten the reaction times.But the length-to-diameter ratio of stirring and to damage whisker too soon, destroying fiber; Stirred slowly and also can influence reaction efficiency.Generally transfer to suitablely, better change at per minute 20～80 with per minute 10～120.Visual response device size is suitably selected.
Embodiment 1:
Select China the Northeast special product sparry magnesite for use,, pulverize through 750～1000 ℃ of calcinings 1～10 hour.Crushed material contains magnesium oxide amount＞95% by analysis.Get this magnesia powder 484 grams (12mol), add 8 liters in water, grind into slurries (removing throw out and impurity), put into reactor; 3 liters of aqueous sulfuric acids that add 1mol/L concentration while stirring add alkali magnesium sulfate nucleus promotor 10 grams again, make its thorough mixing even; 150 ℃ of heating, pressure 0.45Mpa reacted 2 hours down; After the cooling, resultant of reaction taken out to be put in to soak in the water blend; Filter to dry and remove moisture, take out small amount of sample and put into the electric oven drying.Dry thing is fibrous crystallization through scanning electron microscopic observation.Diameter is 02～1 μ m, and length is at 20～100 μ m, and quality is even, its electron micrograph such as Fig. 1.X-ray diffraction is analyzed, and the structural chemistry formula is MgSO
4.5MgO.8H
2O or MgSO
4.5Mg (OH)
2.3H
2O (seeing Fig. 3-1) is single crystal fiber magnesium salt whisker.The above-mentioned remaining magnesium salts crystalline substance that dries is put into reactor, add 8 liters in water, add 1.4 liters of the aqueous sodium hydroxide solutions of 4mol/L concentration while stirring, make its thorough mixing even.Then, under 60 ℃, 60 rev/mins stirring velocity, reacted 2 hours.After the cooling, the resultant of reaction taking-up is put in soaking and stirring dispersion in the water; After filtration, dry to remove moisture, it is dry to put into electric oven; Receive to such an extent that white needles thing 626 restrains, calculating number turnover is 100%.Reaction product is fibrous crystallization through scanning electron microscopic observation.Diameter is 0.2～1 μ m, and length is at 10～80 μ m, and quality is even, its electron micrograph such as Fig. 2.X-ray diffraction is analyzed, and all is magnesium hydroxide, Mg (OH)
2(seeing Fig. 3-2).
Embodiment 2:
Preparation magnesium sulfate solution:, add 8 liters of dissolvings of water with 863 gram magnesium sulfate heptahydrates (3.5mol).With calcined magnesite powder 423 grams (10.5mol), add 8 liters in water, grind into slurries (removing throw out and impurity).Two kinds of liquid material of above method preparation are put into reactor, add alkali magnesium sulfate nucleus promotor 15 grams again, mix.Then, 150 ℃ of heating, pressure 0.45MPa reacted 2 hours down.After the cooling, reaction product taken out to be put in to soak in the water blend; Refilter removal moisture, it is dry in electric oven to get sample segment, scanning electron microscopic observation and X-ray diffraction analysis, and the result is identical with embodiment 1, is single crystal fiber magnesium salt whisker.The magnesium salt whisker that above-mentioned rest part dries is put into reactor, add 9 liters in water, add 1.3 liters of the potassium hydroxide aqueous solutions of 5mol/L concentration while stirring, make its thorough mixing even.Then, under 70 ℃, 40 rev/mins stirring velocity, reacted 2 hours.After the cooling, the resultant of reaction taking-up is put in soaking and stirring dispersion in the water; After filtration, dry to remove moisture, it is dry to put into electric oven; Receive to such an extent that white needles thing 730 restrains, calculating number turnover is 100%.Reaction product is fibrous crystallization through scanning electron microscopic observation.Diameter is 0.2～1 μ m, and length is at 15～80 μ m, and quality is even, the same Fig. 2 of its electron micrograph.X-ray diffraction is analyzed, and all is magnesium hydroxide, Mg (OH)
2(same Fig. 3-2).
Embodiment 3:
Magnesium salt whisker with embodiment 1 method preparation is put into reactor, adds 8 liters in water, adds 1.5 liters of the ammonium hydroxide aqueous solutions of 4mol/L concentration while stirring, makes its thorough mixing even.Then, under 60 ℃, 80 rev/mins stirring velocity, reacted 2 hours.After the cooling, the resultant of reaction taking-up is put in soaking and stirring dispersion in the water; After filtration, dry to remove moisture, it is dry to put into electric oven; Receive to such an extent that white needles thing 625 restrains, calculating number turnover is 100%.Reaction product is fibrous crystallization through scanning electron microscopic observation.Diameter is 0.2～1 μ m, and length is at 10～60 μ m, and quality is even, the same Fig. 2 of its electron micrograph.X-ray diffraction is analyzed, and all is magnesium hydroxide, Mg (OH)
2(same Fig. 3-2).
Embodiment 4:
Magnesium salt whisker with embodiment 2 methods preparations is put into reactor, adds 8 liters in water, puts into reactor, stirs, and adds 1.2 liters of the aqueous sodium hydroxide solutions of 4mol/L concentration while stirring, makes its thorough mixing even.Then, 60 ℃, 12 rev/mins of following reactions 2 hours of stirring velocity.After the cooling, the resultant of reaction taking-up is put in soaking and stirring dispersion in the water; Dry after filtration and remove moisture, it is dry to put into electric oven; Receive to such an extent that white needles thing 745 restrains, calculating number turnover is 96%.Reaction product is fibrous crystallization through scanning electron microscopic observation.Diameter is 0.4～1 μ m, and length is at 20～80 μ m, and quality is even, the same Fig. 2 of its electron micrograph.X-ray diffraction is analyzed, and is mainly magnesium hydroxide Mg (OH)
2Spectral line, but minimal residue alkali magnesium sulfate spectral line is arranged.(seeing Fig. 3-3).
Comparative example 1:
Magnesium salt whisker with embodiment 2 methods preparations is put into reactor, stirs, and adds 1 liter of the aqueous sodium hydroxide solution of 4mol/L concentration while stirring, makes its thorough mixing even.Then, 30 ℃, 12 rev/mins of following reactions 2 hours of stirring velocity.After the cooling, the resultant of reaction taking-up is put in soaking and stirring dispersion in the water; Get rid of after filtration in removing moisture, it is dry to put into electric oven; Receive to such an extent that white needles thing 842 restrains, calculating number turnover is 58%.Reaction product is fibrous crystallization through scanning electron microscopic observation.Diameter is 0.4～1 μ m, and length is at 20～80 μ m.X-ray diffraction is analyzed, and is mainly magnesium hydroxide Mg (OH)
2Spectral line, but obviously residual alkali magnesium sulfate spectral line (seeing Fig. 3-4) is arranged.
Comparative example 2:
In the 0.8L stainless steel cauldron, add 150 ml waters and magnesium chloride (MgCl
2.6H
2O) 81.5g (0.4mol) stirs and makes its dissolving.Slowly add and contain calcium hydroxide 14.8g (0.2mol) emulsion, the limit edged stirs.Left standstill 8 hours in room temperature (about 15 ℃) then, microscopic examination is done in sampling, finds no needle crystal and occurs.Reactor is put into 80 ℃ baking oven, and after 5 hours, sampling is observed, and finds that mixed solution top has rectangular crystal to occur, wide＜1 micron, and long 5-25 micron, but the rectangular crystal of mixed solution lower floor is seldom.After again reactor being placed 5 hours in 120 ℃ baking oven, sampling is observed, and the strip crystal length is not found to increase to some extent, and rectangular crystalline density reduces greatly, this may be since needle-like crystal that generates and unstable institute extremely.The washing of taking-up small amount of sample, acetone is washed, and in drying at room temperature, this rectangular crystal of X-diffraction analysis is Mg
3(OH)
5C1.4H
2O.In the mixed solution of reactor remainder, slowly add 150 milliliters of 2mol/L aqueous sodium hydroxide solutions (0.3mol) while stirring, 80 ℃ of reactions 6 hours.Open reactor, find that the stainless steel cauldron inwall gets rusty seriously corroded.Reaction product is filtered drying through washing.Through the X-ray diffraction analysis, be mainly magnesium hydroxide Mg (OH)
2Spectral line, the microscopic examination fiber is not sufficiently complete, and the crystal length-to-diameter ratio is less than 10, and major part is very broken.
Claims (8)
1, a kind of preparation method of magnesium hydroxide crystal whisker is characterized in that: with magnesium salt whisker MgSO
4.5Mg (OH)
2.3H
2O is a raw material, reacts by the hydroxide aqueous solution with ammonia, basic metal or alkaline-earth metal, obtains magnesium hydroxide crystal whisker.
2, by the preparation method of the described magnesium hydroxide crystal whisker of claim 1, it is characterized in that:described alkali is sodium hydroxide, potassium hydroxide or Qing Yangization .
3, by the preparation method of the described magnesium hydroxide crystal whisker of claim 1, it is characterized in that: add the molar equivalent of alkali by normal 1～4 times of equivalent of the contained anion sulfate acid root of magnesium salt whisker.
4, by the preparation method of the described magnesium hydroxide crystal whisker of claim 1, it is characterized in that: temperature of reaction is in room temperature～200 ℃.
5, by the preparation method of the described magnesium hydroxide crystal whisker of claim 1, it is characterized in that: reaction process adds stirring, and per minute 10～120 changes.
6, by the preparation method of the described magnesium hydroxide crystal whisker of claim 1, it is characterized in that described magnesium salt whisker MgSO
4.5Mg (OH)
2.3H
2O is obtained by sparry magnesite and sal epsom or sulfuric acid hydro-thermal reaction, and in MgO, when adding sal epsom, its mol ratio is 1～5, and when adding sulfuric acid, mol ratio is 2～6; 100～250 ℃ of temperature of reaction, generated time 30 minutes～10 hours.
7,, it is characterized in that sparry magnesite is re-used as the raw material of hydro-thermal reaction after 750～1000 ℃ of calcination by the preparation method of the described magnesium hydroxide crystal whisker of claim 6.
8, by the preparation method of the described magnesium hydroxide crystal whisker of claim 6, the alkali magnesium sulfate crystal seed that adds 0.1～4wt.% when it is characterized in that hydro-thermal reaction is done promotor.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358808C (en) * | 2005-11-10 | 2008-01-02 | 赵兴利 | Method of producing high purity magnesium hydroxide by whisker selection method |
| CN100393919C (en) * | 2006-05-31 | 2008-06-11 | 东北大学 | Method for magnesium hydroxide whisker using giobertite as material |
| CN101880912A (en) * | 2010-03-18 | 2010-11-10 | 中国人民解放军第二炮兵工程学院 | Aluminum hydroxide/magnesium-based hydrotalcite multiphase-based material and preparation method for crystal whiskers thereof |
| CN102046534A (en) * | 2008-03-28 | 2011-05-04 | 宇部材料工业株式会社 | Process for continuous production of fibrous basic magnesium sulfate particle |
| CN102877115A (en) * | 2012-10-10 | 2013-01-16 | 中国科学院福建物质结构研究所 | Preparation method of whisker-shaped magnesium hydroxide |
| CN102046535B (en) * | 2008-03-31 | 2013-11-20 | 宇部材料工业株式会社 | Basic magnesium sulfate granule and process for production thereof |
| CN103849924A (en) * | 2014-02-12 | 2014-06-11 | 沈阳理工大学 | Method for preparing nano-magnesium hydroxide whisker by using magnesium hydroxide whisker |
| CN103922368A (en) * | 2014-04-23 | 2014-07-16 | 中北大学 | Preparation method of nano-sheet-based flower-shaped level substructure magnesium hydroxide powder body |
| CN104153002A (en) * | 2014-08-22 | 2014-11-19 | 瓮福（集团）有限责任公司 | Method for preparing magnesium hydroxide crystal whiskers by utilizing magnesium-containing waste liquid |
| CN107500961A (en) * | 2017-08-17 | 2017-12-22 | 南通奥新电子科技有限公司 | The method and its alkaline matrix of inexpensive potassium titanate crystal whisker coated nano calcium carbonate |
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| JP4778111B1 (en) * | 2010-06-29 | 2011-09-21 | 貴夫 舩田 | Magnesium hydroxide and method for producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358808C (en) * | 2005-11-10 | 2008-01-02 | 赵兴利 | Method of producing high purity magnesium hydroxide by whisker selection method |
| CN100393919C (en) * | 2006-05-31 | 2008-06-11 | 东北大学 | Method for magnesium hydroxide whisker using giobertite as material |
| CN102046534B (en) * | 2008-03-28 | 2013-11-20 | 宇部材料工业株式会社 | Process for continuous production of fibrous basic magnesium sulfate particle |
| CN102046534A (en) * | 2008-03-28 | 2011-05-04 | 宇部材料工业株式会社 | Process for continuous production of fibrous basic magnesium sulfate particle |
| CN102046535B (en) * | 2008-03-31 | 2013-11-20 | 宇部材料工业株式会社 | Basic magnesium sulfate granule and process for production thereof |
| CN101880912B (en) * | 2010-03-18 | 2012-11-07 | 中国人民解放军第二炮兵工程学院 | Aluminum hydroxide/magnesium-based hydrotalcite multiphase-based material and preparation method for crystal whiskers thereof |
| CN101880912A (en) * | 2010-03-18 | 2010-11-10 | 中国人民解放军第二炮兵工程学院 | Aluminum hydroxide/magnesium-based hydrotalcite multiphase-based material and preparation method for crystal whiskers thereof |
| CN102877115A (en) * | 2012-10-10 | 2013-01-16 | 中国科学院福建物质结构研究所 | Preparation method of whisker-shaped magnesium hydroxide |
| CN102877115B (en) * | 2012-10-10 | 2015-10-07 | 中国科学院福建物质结构研究所 | A kind of preparation method of crystal whisker-shaped magnesium hydroxide |
| CN103849924A (en) * | 2014-02-12 | 2014-06-11 | 沈阳理工大学 | Method for preparing nano-magnesium hydroxide whisker by using magnesium hydroxide whisker |
| CN103849924B (en) * | 2014-02-12 | 2016-06-29 | 沈阳理工大学 | A kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker |
| CN103922368A (en) * | 2014-04-23 | 2014-07-16 | 中北大学 | Preparation method of nano-sheet-based flower-shaped level substructure magnesium hydroxide powder body |
| CN103922368B (en) * | 2014-04-23 | 2016-01-20 | 中北大学 | The colored form class aggregated(particle) structure magnesium hydrate powder preparation method of nanometer sheet base |
| CN104153002A (en) * | 2014-08-22 | 2014-11-19 | 瓮福（集团）有限责任公司 | Method for preparing magnesium hydroxide crystal whiskers by utilizing magnesium-containing waste liquid |
| CN107500961A (en) * | 2017-08-17 | 2017-12-22 | 南通奥新电子科技有限公司 | The method and its alkaline matrix of inexpensive potassium titanate crystal whisker coated nano calcium carbonate |
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