CN103789819A - Preparation method of fibrous alkali magnesium sulfate whisker - Google Patents
Preparation method of fibrous alkali magnesium sulfate whisker Download PDFInfo
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- CN103789819A CN103789819A CN201410056427.3A CN201410056427A CN103789819A CN 103789819 A CN103789819 A CN 103789819A CN 201410056427 A CN201410056427 A CN 201410056427A CN 103789819 A CN103789819 A CN 103789819A
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Abstract
The invention relates to the preparation field of chemical industrial materials, and particularly relates to a preparation method of a fibrous alkali magnesium sulfate whisker. The preparation method of the fibrous alkali magnesium sulfate whisker comprises the following steps: (1) preparing a magnesium sulfate solution by using MgSO4.7H2O, stirring and adding NaOH granular caustic soda, aging for 2-24 hours at the temperature of 25 to 100 DEG C to obtain a slurry; (2) transferring the slurry obtained in the step (1) into a hydrothermal reactor, wherein the filling degree is 50-80 percent, adding 0.5-5 percent of seed crystal according to the mass of the NaOH granular caustic soda, uniformly stirring, and reacting the slurry for 2-12 hours at the temperature of 130-180 DEG C; (3) cooling after finishing the reaction of the step (2), filtering, washing and drying a obtained white turbid liquid to obtain the fibrous alkali magnesium sulfate whisker. According to the preparation method, the seed crystal is added into the reaction slurry, alkali magnesium sulfate is easily subjected to nucleus formation growth, and the preparation concentration of the reaction slurry can be relatively high; the whisker nucleation time is reduced, and the whisker growth time also can be shortened.
Description
Technical field
The present invention relates to chemical materials preparation field, particularly, the present invention relates to a kind of preparation method of fibrous alkali magnesium sulfate crystal whisker.
Background technology
Alkali magnesium sulfate crystal whisker also claims magnesium oxysulfide whisker (being called for short MOS whisker), and chemical formula is MgSO
45Mg (OH)
23H
2o or MgSO
45Mg (OH)
22H
2o, outward appearance is white powder, is single needle-like or fan-shaped crystal under microscope, has the feature of high strength, low density and high elastic coefficient, can be used as the packing material of plastics, rubber, resin and ceramic and other composite material, improves the mechanical property of matrix.MOS, as a kind of whisker of functional type, can not only strengthen, and fire-retardant, is the fire-retardant strongthener of high-performance inorganic.Sum up, the preparation method of alkali magnesium sulfate crystal whisker mainly contains following several according to the difference of raw material: (1) activated magnesia and Adlerika or sulphuric acid soln are made slip and carried out hydro-thermal reaction; (2) magnesium hydroxide and Adlerika are made hydro-thermal reaction after slip; (3) precipitation agent such as water-soluble magnesium salt and sodium hydroxide generates magnesium hydrate precipitate, after filtration washing, carries out hydro-thermal reaction again with the solution such as magnesium sulfate or sodium sulfate; (4) Adlerika and sodium hydroxide solution are made the laggard row hydro-thermal reaction of slip.(1) in (2) two kinds of methods, activated magnesia and different, the prepared alkali magnesium sulfate crystal whisker difficult quality control of magnesium hydroxide because of raw material batch activity, particle diameter and degree of crystallinity.In method (3), magnesium salts reacts with sodium hydroxide and generates magnesium hydrate precipitate, and degree of crystallinity is poor, and magnesium hydroxide filtration washing is an industrial difficult problem always.The employing such as Yue Tao, Yi Zanquan method (4) is prepared alkali magnesium sulfate crystal whisker, easily obtains fan-shaped alkali magnesium sulfate crystal whisker, and these fan-shaped whiskers make an addition in matrix as strongthener, and whisker is difficult to disperse, and causes composite materials property to decline.Therefore, in MOS technology of preparing, just need to avoid the growth of fan-shaped whisker.Xiang Lan etc. add the agent of chelating type morphology control to suppress the growth of fan-shaped whisker at reaction slurry.Chinese patent CN101319378A discloses a kind of preparation method of alkali magnesium sulfate crystal whisker, and the method is difficult to suppress fan-shaped whisker growth.Lu Huigang is by optimizing the method control synthon shape alkali magnesium sulfate crystal whisker of hydrothermal reaction condition and interpolation EDTA, and Reaction conditions range is narrow, and when industrialization operation, quality product is difficult to control; Hydro-thermal reaction time length, single yield poorly, and add EDTA to cause the problems such as Recycling Mother Solution difficulty.
In a word, forefathers are doing a large amount of work aspect fibrous alkali magnesium sulfate crystal whisker, but exist complex technical process and the unequal problem of whisker morphology, have limited the further industrial application of correlation technique.
Summary of the invention
To the object of the invention is, to provide a kind of novel method of preparing fibrous alkali magnesium sulfate crystal whisker in order addressing the above problem.The method technique is simple, with low cost, and added value of product is high, and the crystal whisker products length-to-diameter ratio of preparation is larger thus, has solved fan-shaped whisker problem.
The preparation method of fibrous alkali magnesium sulfate crystal whisker of the present invention, comprises the following steps:
1) by MgSO
47H
2o is mixed with Adlerika, stirs and adds NaOH grain alkali, and at 25 ℃～100 ℃, ageing obtains slip for 2～24 hours;
2) slip that step 1) obtained moves in hydrothermal reaction kettle, and compactedness is 50%～80%, adds 0.5%～5% crystal seed of NaOH grain alkali quality, stirs; Slip reacts 2～12 hours at 130 ℃～180 ℃;
3) step 2) reaction naturally cools to the white suspension liquid that room temperature obtains after finishing, after filtration, washing, obtain fibrous alkali magnesium sulfate crystal whisker after drying.
Preparation in accordance with the present invention, wherein, in Adlerika, magnesium sulfate concentration is 1.0～1.5mol/L described in step 1).
Preparation in accordance with the present invention, wherein, the mol ratio of magnesium sulfate and sodium hydroxide is (0.65～1.00) described in step 1): 1.
Preparation in accordance with the present invention, wherein, step 2) described crystal seed makes by alkali magnesium sulfate crystal whisker ball milling, and preferable particle size is between 0.2～2.0 μ m.Preparing above-mentioned crystal seed alkali magnesium sulfate crystal whisker used is the existing alkali magnesium sulfate crystal whisker of selling on the market, for example, and 153 or 152 type alkali magnesium sulfate crystal whiskers.
In prior art, the employing magnesium sulfate such as Xiang Lan and sodium hydroxide hydro-thermal reaction are prepared alkali magnesium sulfate crystal whisker, and first Adlerika reacts and obtains nanometric magnesium hydroxide with sodium hydroxide solution, then filter, wash magnesium hydroxide.Nano level material filtering washs in industrial more difficult realization.Add the fan-shaped whisker of chelating type morphology control agent control, increased mother liquor composition, bring difficulty to the recycle of mother liquor.
And in the preparation method of fibrous alkali magnesium sulfate crystal whisker of the present invention:
1) MgSO
47H
2o is mixed with certain density solution, stirs and adds a certain amount of granular NaOH, is conducive to the raising of magnesium hydroxide degree of crystallinity, and then ageing slip further improves the degree of crystallinity of magnesium hydroxide.The preparation of industrial slip can be carried out in dissolving tank or material-compound tank, is easy to industrial design.
Magnesium hydroxide degree of crystallinity increases, and reduces the dissolution rate of magnesium hydroxide in reaction process, controls the lower degree of supersaturation of alkali magnesium sulfate, promotes the growth of high length-diameter ratio whisker; And magnesium hydroxide degree of crystallinity increases, magnesium hydroxide lattice imperfection reduces, and the nucleation site on magnesium hydroxide platelet reduces, thereby has reduced the growth of fan-shaped alkali magnesium sulfate crystal whisker.
2) in slip, add crystal seed, increase the generating rate of alkali magnesium sulfate nucleus, suppress the growth (the most of reason of growth of fan-shaped whisker be that nucleus is less cause) of fan-shaped whisker.
3) because added crystal seed in reaction slurry, alkali magnesium sulfate is easy to nucleating growth, and the concentration that reaction slurry can be prepared is larger; And reduced whisker nucleation time, the time of whisker growth also can shorten.So whisker output increases, the reaction times reduces, and industrial cost can reduce.
Further, the present invention has the following advantages and high-lighting effect:
1. after Adlerika reacts with sodium hydrate solid, the for some time of ageing at a certain temperature, increases generated magnesium hydroxide degree of crystallinity, has reduced the dissolution rate of magnesium hydroxide in reaction process, control the lower degree of supersaturation of alkali magnesium sulfate, promote the growth of high length-diameter ratio whisker; And by slip ageing, the sheet-like magnesium hydroxide crystal degree of crystallinity generating increases, magnesium hydroxide lattice imperfection reduces, and the nucleation site on magnesium hydroxide platelet reduces, thereby has suppressed the growth of fan-shaped alkali magnesium sulfate crystal whisker.
2. in reaction slurry, add the alkali magnesium sulfate crystal seed of ball milling, can increase the nucleation rate of alkali magnesium sulfate crystal whisker, reduce the growth of fan-shaped whisker.
3. the concentration of magnesium sulfate of the present invention is 1.0～1.5mol/L, and the mol ratio of magnesium sulfate and sodium hydroxide is (0.65～1.00): 1, and pulp density is higher, and whisker output is larger; The mol ratio of magnesium sulfate and sodium hydroxide is lower, and magnesium sulfate utilization ratio is higher, and raw materials cost reduces, and mother liquor is easy to circular treatment.
4. technique of the present invention is simple, and production cost is low, is easy to realize large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is technological process schematic diagram of the present invention.
Fig. 2 is the SEM photo of the alkali magnesium sulfate crystal whisker prepared of the embodiment of the present invention 1.
Fig. 3 is the SEM photo of the alkali magnesium sulfate crystal whisker prepared of comparative example 2 of the present invention
Fig. 4 is the XRD figure spectrum of the alkali magnesium sulfate crystal whisker prepared of the embodiment of the present invention 3.
Embodiment
The method of fibrous alkali magnesium sulfate crystal whisker of the present invention, is elaborated by following examples.
Embodiment 1
Preparation 1.0mol/L MgSO
47H
21.6 liters of O solution add the NaOH(MgSO of 98.5 gram particle shapes under agitation condition
4with NaOH mol ratio be 0.65:1), ageing 2 hours at 25 ℃.The slip that obtains is moved in 2 liters of reactors, and compactedness is 80%, and (particle diameter 0.2～2.0 μ m), stirs to add the crystal seed of 0.55 gram.Slip reacts 2 hours at 130 ℃.After finishing, reaction naturally cools to room temperature.After being filtered, wash, dried, the white suspension liquid obtaining after hydro-thermal reaction obtains length 30～50 μ m, diameter 0.2～0.5 μ m, 152 fiber type shape alkali magnesium sulfate crystal whiskers of length-to-diameter ratio 60～200, main content 98.0%.
Embodiment 2
Preparation 1.0mol/L MgSO
47H
21.6 liters of O solution add the NaOH(MgSO of 60.0 gram particle shapes under agitation condition
4with NaOH mol ratio be 1:1), ageing 24 hours at 60 ℃.The slip that obtains is moved in 2 liters of reactors, and compactedness is 75%, and (particle diameter 0.2～2.0 μ m), stirs to add the crystal seed of 3.5 grams.Slip reacts 12 hours at 180 ℃.After finishing, reaction naturally cools to room temperature.After being filtered, wash, dried, the white suspension liquid obtaining after hydro-thermal reaction obtains length 50～200 μ m, diameter 0.5～1.0 μ m, 152 fiber type shape alkali magnesium sulfate crystal whiskers of length-to-diameter ratio 50～400, main content 98.7%.
Embodiment 3
Preparation 1.5mol/L MgSO
47H
21.0 liters of O solution add the NaOH(MgSO of 92.3 gram particle shapes under agitation condition
4with NaOH mol ratio be 0.65:1), ageing 24 hours at 100 ℃.The slip that obtains is moved in 2 liters of reactors, and compactedness is 50%, and (particle diameter 0.2～2.0 μ m), stirs to add the crystal seed of 4.0 grams.Slip reacts 12 hours at 130 ℃.After finishing, reaction naturally cools to room temperature.After being filtered, wash, dried, the white suspension liquid obtaining after hydro-thermal reaction obtains length 50～200 μ m, diameter 0.2～0.5 μ m, 152 fiber type shape alkali magnesium sulfate crystal whiskers of length-to-diameter ratio 100～1000, main content 98.9%.
Embodiment 4
Preparation 1.5mol/L MgSO
47H
21.5 liters of O solution add the NaOH(MgSO of 90.0 gram particle shapes under agitation condition
4with NaOH mol ratio be 1:1), ageing 24 hours at 80 ℃.The slip that obtains is moved in 2 liters of reactors, and compactedness is 75%, and (particle diameter 0.2～2.0 μ m), stirs to add the crystal seed of 0.5 gram.Slip reacts 12 hours at 150 ℃.After finishing, reaction naturally cools to room temperature.After being filtered, wash, dried, the white suspension liquid obtaining after hydro-thermal reaction obtains length 30～100 μ m, diameter 0.2～0.8 μ m, 152 fiber type shape alkali magnesium sulfate crystal whiskers of length-to-diameter ratio 50～500, main content 99.2%.
Embodiment 5
Preparation 1.2mol/L MgSO
47H
21.5 liters of O solution add the NaOH(MgSO of 90.0 gram particle shapes under agitation condition
4with NaOH mol ratio be 0.8:1), ageing 12 hours at 80 ℃.The slip that obtains is moved in 2 liters of reactors, and compactedness is 75%, and (particle diameter 0.2～2.0 μ m), stirs to add the crystal seed of 2.5 grams.Slip reacts 6 hours at 150 ℃.After finishing, reaction naturally cools to room temperature.After being filtered, wash, dried, the white suspension liquid obtaining after hydro-thermal reaction obtains length 30～60 μ m, diameter 0.2～0.6 μ m, 152 fiber type shape alkali magnesium sulfate crystal whiskers of length-to-diameter ratio 50～300, main content 98.9%.
Embodiment 6
Preparation 1.3mol/L MgSO
47H
21.5 liters of O solution add the NaOH(MgSO of 86.6 gram particle shapes under agitation condition
4with NaOH mol ratio be 0.9:1), ageing 12 hours at 80 ℃.The slip that obtains is moved in 2 liters of reactors, and compactedness is 75%, and (particle diameter 0.2～2.0 μ m), stirs to add the crystal seed of 2.5 grams.Slip reacts 8 hours at 160 ℃.After finishing, reaction naturally cools to room temperature.After being filtered, wash, dried, the white suspension liquid obtaining after hydro-thermal reaction obtains length 30～80 μ m, diameter 0.3～0.6 μ m, 152 fiber type shape alkali magnesium sulfate crystal whiskers of length-to-diameter ratio 50～300, main content 98.7%.
Comparative example 1
Preparation 1.0mol/L MgSO
47H
21.6 liters of O solution add the NaOH(MgSO of 98.5 gram particle shapes under agitation condition
4with NaOH mol ratio be 0.65:1).The slip obtaining is moved in 2 liters of reactors, and compactedness is 80%.Slip reacts 2 hours at 130 ℃.After finishing, reaction naturally cools to room temperature.After the white suspension liquid obtaining after hydro-thermal reaction is filtered, washs, dried, obtain product, product is examined under a microscope, and has a small amount of tiny fan-shaped whisker to produce, and most of raw material does not react.
Comparative example 2
Preparation 1.0mol/L MgSO
47H
21.5 liters of O solution add the NaOH(MgSO of 60.0 gram particle shapes under agitation condition
4with NaOH mol ratio be 1:1).The slip obtaining is moved in 2 liters of reactors, and compactedness is 75%.Slip reacts 12 hours at 180 ℃.After finishing, reaction naturally cools to room temperature.After being filtered, wash, dried, the white suspension liquid obtaining after hydro-thermal reaction obtains 152 type alkali magnesium sulfate crystal whiskers, alkali magnesium sulfate crystal whisker is all unidirectional or two-way fan-shaped whisker, long 50～150 μ m of fan-shaped fibrous bundle, fan root diameter 5.0～10.0 μ m, fantail radiation diameter.See Fig. 3.
In above-described embodiment 1～6 and comparative example, water magnesium sulfate and sodium hydroxide are analytical reagent; Conversion unit adopts GSH-2/20 type lift magnetic force reactor, Weihai Yuan Cheng petrochemical equipment company limited.
Claims (4)
1. a preparation method for fibrous alkali magnesium sulfate crystal whisker, comprises the following steps:
1) by MgSO
47H
2o is mixed with Adlerika, stirs and adds NaOH grain alkali, and at 25 ℃～100 ℃, ageing obtains slip for 2～24 hours;
2) slip that step 1) obtained moves in hydrothermal reaction kettle, and compactedness is 50%～80%, adds 0.5%～5% crystal seed of NaOH grain alkali quality, stirs; Slip reacts 2～12 hours at 130 ℃～180 ℃;
3) step 2) reaction finish rear cooling, the white suspension liquid obtaining after filtration, washing, dry after obtain fibrous alkali magnesium sulfate crystal whisker.
2. preparation method according to claim 1, is characterized in that, in Adlerika, magnesium sulfate concentration is 1.0～1.5mol/L described in step 1).
3. preparation method according to claim 1 and 2, is characterized in that, the mol ratio of magnesium sulfate and sodium hydroxide is (0.65～1.00) described in step 1): 1.
4. preparation method according to claim 1, is characterized in that step 2) described crystal seed makes by alkali magnesium sulfate crystal whisker ball milling.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988576A (en) * | 2015-07-14 | 2015-10-21 | 中国科学院青海盐湖研究所 | Preparation method of basic magnesium sulfate whiskers |
| CN105603504A (en) * | 2014-11-21 | 2016-05-25 | 合肥杰事杰新材料股份有限公司 | Method for preparing needle-like basic magnesium sulfate whiskers by ultrasonic assistance |
| CN107201542A (en) * | 2017-06-08 | 2017-09-26 | 青海大学 | A kind of preparation method of alkali magnesium sulfate crystal whisker |
| CN108034991A (en) * | 2017-12-08 | 2018-05-15 | 中国科学院青海盐湖研究所 | The preparation method of 311 type alkali magnesium sulfate crystal whiskers |
| CN108166062A (en) * | 2017-12-25 | 2018-06-15 | 岭南师范学院 | It is a kind of using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker |
| CN115558996A (en) * | 2022-09-09 | 2023-01-03 | 中国科学院青海盐湖研究所 | Method for preparing 517 type basic magnesium sulfate whisker under mild condition |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319378A (en) * | 2008-05-09 | 2008-12-10 | 中国科学院青海盐湖研究所 | Preparation method of alkali type magnesium sulfate crystal whisker |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319378A (en) * | 2008-05-09 | 2008-12-10 | 中国科学院青海盐湖研究所 | Preparation method of alkali type magnesium sulfate crystal whisker |
Non-Patent Citations (2)
| Title |
|---|
| 卢会刚等: "控制合成纤维状碱式硫酸镁晶须的研究", 《盐湖研究》, vol. 19, no. 3, 30 September 2011 (2011-09-30) * |
| 姜玉芝等: "碱式硫酸镁晶须制备技术研究", 《有色矿冶》, vol. 22, 31 August 2006 (2006-08-31) * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105603504A (en) * | 2014-11-21 | 2016-05-25 | 合肥杰事杰新材料股份有限公司 | Method for preparing needle-like basic magnesium sulfate whiskers by ultrasonic assistance |
| CN104988576A (en) * | 2015-07-14 | 2015-10-21 | 中国科学院青海盐湖研究所 | Preparation method of basic magnesium sulfate whiskers |
| CN104988576B (en) * | 2015-07-14 | 2018-01-16 | 中国科学院青海盐湖研究所 | The preparation method of alkali magnesium sulfate crystal whisker |
| CN107201542A (en) * | 2017-06-08 | 2017-09-26 | 青海大学 | A kind of preparation method of alkali magnesium sulfate crystal whisker |
| CN108034991A (en) * | 2017-12-08 | 2018-05-15 | 中国科学院青海盐湖研究所 | The preparation method of 311 type alkali magnesium sulfate crystal whiskers |
| CN108166062A (en) * | 2017-12-25 | 2018-06-15 | 岭南师范学院 | It is a kind of using Hoh Yanhu making from brine for the method for alkali magnesium sulfate crystal whisker |
| CN115558996A (en) * | 2022-09-09 | 2023-01-03 | 中国科学院青海盐湖研究所 | Method for preparing 517 type basic magnesium sulfate whisker under mild condition |
| CN115558996B (en) * | 2022-09-09 | 2024-04-12 | 中国科学院青海盐湖研究所 | Method for preparing 517 type basic magnesium sulfate whisker under mild condition |
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