CN107344727A - A kind of preparation method of hexagonal plate nano-sized magnesium hydroxide material - Google Patents
A kind of preparation method of hexagonal plate nano-sized magnesium hydroxide material Download PDFInfo
- Publication number
- CN107344727A CN107344727A CN201710431822.9A CN201710431822A CN107344727A CN 107344727 A CN107344727 A CN 107344727A CN 201710431822 A CN201710431822 A CN 201710431822A CN 107344727 A CN107344727 A CN 107344727A
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- nano
- magnesium hydroxide
- magnesia
- hexagonal plate
- sized magnesium
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Classifications
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a kind of preparation method of hexagonal plate nano-sized magnesium hydroxide material, magnesium raw material will be contained by hydrothermal synthesis method first and be prepared into nano-sized magnesium hydroxide precursor liquid, washing, centrifugation, again nano-sized magnesium hydroxide magma is prepared into through high energy ball mill, then the magma is made by powder by low temperature calcination, produces nano oxidized magnesium dust.The nano oxidized magnesium dust of preparation is passed through into the previously prepared highly concentrated nano magnesia aqueous solution of high frequency ultrasound, aqueous dispersion is added when its granularity reaches 300nm, continue milled processed using nano-level grinder, until granularity D90 is in below 100nm, so as to prepare the nano magnesia water paste of high concentration.Finally the nano magnesia water paste of preparation is placed in drying box and reacts suitable time, produces hexagonal plate nano-sized magnesium hydroxide slurry, the slurry is spray-dried again to produce hexagonal plate Magnesium Hydroxide Nano-particles material.
Description
Technical field
The present invention relates to a kind of preparation method of hexagonal plate nano-sized magnesium hydroxide material.
Background technology
Magnesium hydroxide is a kind of green, inexpensive and environment-friendly inorganic additive flame retardant, and it has heat endurance
The advantages that good, nontoxic, it can be added to extensively in plastics, rubber, coating Polymer material to improve its fire resistance.And grain
The polymolecularity hexagonal plate nano-sized magnesium hydroxide material that footpath is small, surface polarity is low has dispersiveness and nano active well；
In the case where having little influence on use intensity, the performance such as the fire-retardant of material, smoke elimination, antidrip, filling can be significantly improved.But advise
Then the synthesis technique of uniform nanometer hexagonal plate magnesium hydroxide is complex, at present, is prepared on a large scale and pattern is good six
Angle sheeted nanometer magnesium hydroxide is the difficult point of industry.
The original magnesium raw material of the present invention, by two-step method, original magnesium raw material is first synthesized into nanometer magnesia powder, then by receiving
Highly concentrated nano magnesium oxide powder is distributed to aqueous medium by rice dispersion technology, is formed high concentration slurry, is then passed through conjunction again
Nano magnesia slurry is prepared into a nanometer hexagonal plate magnesium hydroxide by suitable roasting stoving process.The nanometer six of this method synthesis
Angle flake magnesium hydroxide in high volume low cost can be prepared, and the lamella synthesized is uniformly dispersed, and overall difference is little, the property of powder
It can be significantly improved.
The content of the invention
It is an object of the invention to break through the magnesium hydroxide lamellar spacing heterogeneity prepared at present using conventional method, size
Inconsistent difficult point, synthetic method and technique are innovated, i.e., prepare the nanometer magnesia powder of size tunable first, then
Nano-sized magnesium hydroxide slurry and powder are prepared using nano-milled technology and special drying process.
To reach above-mentioned expected purpose, the present invention adopts the following technical scheme that：
A kind of preparation method of hexagonal plate nano-sized magnesium hydroxide material provided by the invention, can by preparing particle diameter first
The nanometer magnesia powder of control, nano-milled technology and special drying process is recycled to prepare nano-sized magnesium hydroxide slurry and powder
Body, the technique comprise the following steps：
A. composition mixed liquor is premixed in proportion by water, containing magnesium raw material, sodium carbonate, utilize autoclave in an oven 150
8~48 hours obtained nano-sized magnesium hydroxide precursor liquids of~200 DEG C of reactions；
B. nano-sized magnesium hydroxide precursor liquid made from step a is washed, centrifuged, then be prepared into and receive through high energy ball mill grinding
Rice magnesium hydroxide magma；
C. nano-sized magnesium hydroxide magma made from step b is subjected to 350~500 DEG C of low temperature calcinations, obtains nano magnesia
Powder；
D. nanometer magnesia powder made from step c is subjected to pre-dispersed processing, nano magnesia using high-frequency ultrasonic
Solid content is 5%~65%, until the granularity D90 of solid particle reaches 300nm in mixed solution；
E. dispersant is added in magnesia mixed solution made from step d, continues to grind using nano-level grinder
Processing, until the granularity D90 of solid particle reaches below 100nm in dispersion liquid, so as to which the oxidation of the water nano of high concentration be made
Magnesium water paste；
F. water nano magnesia water paste made from step e is placed on 100~200 DEG C of reactions suitable 4 in drying box
~48 hours, finely dispersed hexagonal plate nano-sized magnesium hydroxide slurry is produced, the slurry is spray-dried again to produce hexagonal piece
Shape Magnesium Hydroxide Nano-particles material.
In some embodiments, the water described in step a, the mass ratio containing magnesium raw material, sodium carbonate are 1:(0.1~
1.2)：(0.01~0.1), described containing magnesium raw material is magnesium chloride, magnesium sulfate, magnesia, one kind or its group in magnesium hydroxide
Close.
In some embodiments, in step e, described dispersant is BYK190, BYK106, BYK182, BYK184, moral
One kind or its combination in modest 904S, MOK5032, the wherein mass ratio of magnesia mixed solution and dispersant is 1:(0.05~
0.3)。
In some embodiments, in step e, the size of described nano-level grinder abrasive media zirconium pearl is 0.4mm,
0.2mm, 0.1mm or 0.05mm.
Compared with prior art, the preparation method of a kind of hexagonal plate nano-sized magnesium hydroxide material provided by the invention, its
Advantage is：Hexagonal plate nano-sized magnesium hydroxide material prepared by the present invention can keep the equal of yardstick and pattern in nanometer level
One property, particle agglomeration and pattern phenomenon not of uniform size are alleviated, also greatly improves hexagonal plate magnesium hydroxide material
Dispersiveness.
Embodiment
The details realized below by instantiation to the present invention is described, but protection scope of the present invention is not limited to
These embodiments.
Embodiment 1：
Water, magnesium chloride containing magnesium raw material, sodium carbonate are pressed 1:0.1:0.01 ratio premix composition mixed liquor, it is anti-using high pressure
Answer kettle 150 DEG C of reactions, 8 hours obtained nano-sized magnesium hydroxide precursor liquids in an oven；Obtained nano-sized magnesium hydroxide precursor liquid is washed
Wash, centrifuge, then nano-sized magnesium hydroxide magma is prepared into through high energy ball mill grinding；Obtained nano-sized magnesium hydroxide magma is carried out
350 DEG C of low temperature calcinations, obtain nanometer magnesia powder；Obtained nanometer magnesia powder is carried out pre-dispersed using high-frequency ultrasonic
Processing, the size of abrasive media zirconium pearl is 0.4mm, and nano magnesia solid content is 5%, until solid particle in mixed solution
Granularity D90 reaches 300nm；Dispersant B YK190 is added in magnesia mixed solution made from above step, ground using nanometer
Grinding machine continues milled processed, until the granularity D90 of solid particle reaches below 100nm in dispersion liquid, it is highly concentrated so as to be made
The water nano magnesia water paste of degree；Obtained water nano magnesia water paste is placed in drying box 100 DEG C
Reaction 4 hours, produces finely dispersed hexagonal plate nano-sized magnesium hydroxide slurry, the slurry is spray-dried again to produce hexagonal piece
Shape Magnesium Hydroxide Nano-particles material.
Embodiment 2：
Water, magnesium chloride containing magnesium raw material, sodium carbonate are pressed 1:0.6:0.06 ratio premix composition mixed liquor, it is anti-using high pressure
Answer kettle 180 DEG C of reactions, 8 hours obtained nano-sized magnesium hydroxide precursor liquids in an oven；Obtained nano-sized magnesium hydroxide precursor liquid is washed
Wash, centrifuge, then nano-sized magnesium hydroxide magma is prepared into through high energy ball mill grinding；Obtained nano-sized magnesium hydroxide magma is carried out
400 DEG C of low temperature calcinations, obtain nanometer magnesia powder；Obtained nanometer magnesia powder is carried out pre-dispersed using high-frequency ultrasonic
Processing, the size of abrasive media zirconium pearl is 0.2mm, and nano magnesia solid content is 30%, until solid particle in mixed solution
Granularity D90 reach 300nm；Dispersant B YK182 is added in magnesia mixed solution made from above step, utilizes nanometer
Grinder continues milled processed, until the granularity D90 of solid particle reaches below 100nm in dispersion liquid, so as to which height be made
The water nano magnesia water paste of concentration；Obtained water nano magnesia water paste is placed on 150 in drying box
DEG C reaction 24 hours, produce finely dispersed hexagonal plate nano-sized magnesium hydroxide slurry, the slurry is spray-dried again to produce six
Cornual plate shape Magnesium Hydroxide Nano-particles material.
Embodiment 3：
Water, magnesium chloride containing magnesium raw material, sodium carbonate are pressed 1:1.0:0.08 ratio premix composition mixed liquor, it is anti-using high pressure
Answer kettle 180 DEG C of reactions, 36 hours obtained nano-sized magnesium hydroxide precursor liquids in an oven；By obtained nano-sized magnesium hydroxide precursor liquid
Washing, centrifugation, then it is prepared into nano-sized magnesium hydroxide magma through high energy ball mill grinding；Obtained nano-sized magnesium hydroxide magma is entered
450 DEG C of low temperature calcinations of row, obtain nanometer magnesia powder；Obtained nanometer magnesia powder is divided in advance using high-frequency ultrasonic
Processing is dissipated, the size of abrasive media zirconium pearl is 0.1mm, and nano magnesia solid content is 45%, until solid in mixed solution
The granularity D90 of grain reaches 300nm；The modest 904S of dispersant moral is added in magnesia mixed solution made from above step, utilized
Nano-level grinder continues milled processed, until the granularity D90 of solid particle reaches below 100nm in dispersion liquid, so as to make
Obtain the water nano magnesia water paste of high concentration；Obtained water nano magnesia water paste is placed in drying box
180 DEG C are reacted 36 hours, produce finely dispersed hexagonal plate nano-sized magnesium hydroxide slurry, the slurry is spray-dried again to be produced
Hexagonal plate Magnesium Hydroxide Nano-particles material.
Embodiment 4：
Water, magnesium chloride containing magnesium raw material, sodium carbonate are pressed 1:1.2:0.1 ratio premix composition mixed liquor, it is anti-using high pressure
Answer kettle 200 DEG C of reactions, 48 hours obtained nano-sized magnesium hydroxide precursor liquids in an oven；By obtained nano-sized magnesium hydroxide precursor liquid
Washing, centrifugation, then it is prepared into nano-sized magnesium hydroxide magma through high energy ball mill grinding；Obtained nano-sized magnesium hydroxide magma is entered
500 DEG C of low temperature calcinations of row, obtain nanometer magnesia powder；Obtained nanometer magnesia powder is divided in advance using high-frequency ultrasonic
Processing is dissipated, the size of abrasive media zirconium pearl is 0.05mm, and nano magnesia solid content is 65%, until solid in mixed solution
The granularity D90 of grain reaches 300nm；Dispersant MOK5032 is added made from above step in magnesia mixed solution, using receiving
Rice grinder continues milled processed, until the granularity D90 of solid particle reaches below 100nm in dispersion liquid, so as to be made
The water nano magnesia water paste of high concentration；Obtained water nano magnesia water paste is placed in drying box
200 DEG C are reacted 48 hours, produce finely dispersed hexagonal plate nano-sized magnesium hydroxide slurry, the slurry is spray-dried again to be produced
Hexagonal plate Magnesium Hydroxide Nano-particles material.
The preferred embodiments of the present invention have shown and described in described above, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations, modification and
Environment, and can be changed in the scope of the invention is set forth herein by the technology or knowledge of above-mentioned teaching or association area
It is dynamic, and the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention, then all should be appended by the present invention
In scope of the claims.
Claims (4)
1. a kind of preparation method of hexagonal plate nano-sized magnesium hydroxide material, it is characterised in that by preparing size tunable first
Nanometer magnesia powder, recycle nano-milled technology and special drying process to prepare nano-sized magnesium hydroxide slurry and powder
Body, the technique comprise the following steps：
A. composition mixed liquor is premixed in proportion by water, containing magnesium raw material, sodium carbonate, utilize autoclave in an oven 150~200
DEG C reaction 8~48 hours obtained nano-sized magnesium hydroxide precursor liquids；
B. nano-sized magnesium hydroxide precursor liquid made from step a is washed, centrifuged, then a nanometer hydrogen is prepared into through high energy ball mill grinding
Magnesia magma；
C. nano-sized magnesium hydroxide magma made from step b is subjected to 350~500 DEG C of low temperature calcinations, obtains nanometer magnesia powder；
D. nanometer magnesia powder made from step c is subjected to pre-dispersed processing using high-frequency ultrasonic, nano magnesia contains admittedly
Measure as 5%~65%, until the granularity D90 of solid particle reaches 300nm in mixed solution；
E. dispersant is added in magnesia mixed solution made from step d, continues milled processed using nano-level grinder,
Until the granularity D90 of solid particle reaches below 100nm in dispersion liquid, it is water-based so as to which the water nano magnesia of high concentration be made
Slurry；
F. water nano magnesia water paste made from step e is placed on 100~200 DEG C of reactions suitable 4~48 in drying box
Hour, finely dispersed hexagonal plate nano-sized magnesium hydroxide slurry is produced, the slurry again receive by the spray-dried hexagonal plate that produces
Rice magnesium hydrate powder material.
2. the preparation method of hexagonal plate nano-sized magnesium hydroxide material according to claim 1, it is characterised in that step a
Described in water, mass ratio containing magnesium raw material, sodium carbonate be 1:(0.1~1.2):(0.01~0.1), it is described to be containing magnesium raw material
One kind or its combination in magnesium chloride, magnesium sulfate, magnesia, magnesium hydroxide.
3. the preparation method of hexagonal plate nano-sized magnesium hydroxide material according to claim 1, it is characterised in that step e
In, described dispersant is BYK190, BYK106, BYK182, BYK184, one kind or its group in moral modest 904S, MOK5032
Close, wherein the mass ratio of magnesia mixed solution and dispersant is 1:(0.05~0.3).
4. the preparation method of hexagonal plate nano-sized magnesium hydroxide material according to claim 1, it is characterised in that step e
In, the size of described nano-level grinder abrasive media zirconium pearl is 0.4mm, 0.2mm, 0.1mm or 0.05mm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793207A (en) * | 2018-08-09 | 2018-11-13 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of nano-silicon grade of steel magnesium oxide powder |
| CN109052439A (en) * | 2018-08-09 | 2018-12-21 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of high quality nano magnesium hydroxide aqueous slurry |
| CN109133123A (en) * | 2018-08-09 | 2019-01-04 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of high quality nano magnesium hydroxide powder |
| CN109233869A (en) * | 2018-08-09 | 2019-01-18 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of the high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide |
| CN110343860A (en) * | 2019-07-18 | 2019-10-18 | 北京科技大学 | A method of going demagging, fluorine ion from sulfuric acid solution |
| CN110357146A (en) * | 2019-07-26 | 2019-10-22 | 南京理工大学 | A kind of batch preparation of nanometer of cadmium hydroxide or nano oxygen cadmium |
| CN111547750A (en) * | 2020-05-15 | 2020-08-18 | 洛阳中超新材料股份有限公司 | Preparation method of hexagonal flaky magnesium hydroxide flame retardant with controllable particle size |
| CN112408439A (en) * | 2020-11-20 | 2021-02-26 | 洛阳中超新材料股份有限公司 | Method for preparing superfine magnesium hydroxide for flame retardant by using magnesium hydroxide coarse powder as raw material |
| CN113371739A (en) * | 2020-02-25 | 2021-09-10 | 中国科学院青海盐湖研究所 | Preparation method of hexagonal flaky magnesium hydroxide nanosheet |
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| CN102101684A (en) * | 2009-12-16 | 2011-06-22 | 中国科学院过程工程研究所 | Method for preparing submicron lamellar magnesium hydroxide by intensifying alkali |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793207A (en) * | 2018-08-09 | 2018-11-13 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of nano-silicon grade of steel magnesium oxide powder |
| CN109052439A (en) * | 2018-08-09 | 2018-12-21 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of high quality nano magnesium hydroxide aqueous slurry |
| CN109133123A (en) * | 2018-08-09 | 2019-01-04 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of high quality nano magnesium hydroxide powder |
| CN109233869A (en) * | 2018-08-09 | 2019-01-18 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of the high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide |
| CN110343860A (en) * | 2019-07-18 | 2019-10-18 | 北京科技大学 | A method of going demagging, fluorine ion from sulfuric acid solution |
| CN110357146A (en) * | 2019-07-26 | 2019-10-22 | 南京理工大学 | A kind of batch preparation of nanometer of cadmium hydroxide or nano oxygen cadmium |
| CN113371739A (en) * | 2020-02-25 | 2021-09-10 | 中国科学院青海盐湖研究所 | Preparation method of hexagonal flaky magnesium hydroxide nanosheet |
| CN111547750A (en) * | 2020-05-15 | 2020-08-18 | 洛阳中超新材料股份有限公司 | Preparation method of hexagonal flaky magnesium hydroxide flame retardant with controllable particle size |
| CN112408439A (en) * | 2020-11-20 | 2021-02-26 | 洛阳中超新材料股份有限公司 | Method for preparing superfine magnesium hydroxide for flame retardant by using magnesium hydroxide coarse powder as raw material |
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Address after: Suzhou City, Jiangsu province 215500 Changshou City Shanghu town yuanyangqiao industrial district Applicant after: SUZHOU ZEMEI NEW MATERIAL TECHNOLOGY CO., LTD. Address before: 215500 Jiangsu city of Changzhou province Changshou City Shanghu town yuanyangqiao industrial district Applicant before: SUZHOU ZEMEI NEW MATERIAL TECHNOLOGY CO., LTD. |
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