CN106587119A - Method for preparing hexagonal flake magnesium hydroxide with dominant growth on (001) crystal face - Google Patents
Method for preparing hexagonal flake magnesium hydroxide with dominant growth on (001) crystal face Download PDFInfo
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- CN106587119A CN106587119A CN201611213912.2A CN201611213912A CN106587119A CN 106587119 A CN106587119 A CN 106587119A CN 201611213912 A CN201611213912 A CN 201611213912A CN 106587119 A CN106587119 A CN 106587119A
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- magnesium hydroxide
- polyethylene
- crystal face
- slurry
- hexagonal flake
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
Abstract
The invention provides a method for preparing hexagonal flake magnesium hydroxide with dominant growth on a (001) crystal face. The method comprises the following steps: dispersing a magnesium hydroxide raw material into a sodium hydroxide solution in a ball milling manner, and performing ball-milling so as to prepare slurry with the solid content of 5-30%; adding the ground magnesium hydroxide slurry into a hydrothermal reactor lined with polytetrafluoroethylene, and performing hydrothermal treatment in a temperature range from 120 DEG C to 200 DEG C; and cooling, filtering and washing the product after the reaction is completed, and drying the product in a drying oven. The hexagonal flake magnesium hydroxide is added into polyethylene, so that the oxygen index of the polyethylene can be improved from 19.2% to 22.6% by virtue of the magnesium hydroxide, and the flame retardant property is enhanced. The polyethylene material added with the hexagonal flake magnesium hydroxide is of a meshed structure, the tensile strength of the polyethylene is improved, while the elongation at break is reduced along with increase of the addition amount. The modified magnesium hydroxide and the polyethylene material have high compatibility, and the mechanical property of the polyethylene can be maintained.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry is related to a kind of preparation of flame retardant of magnesium hydroxide, and in particular to a kind of
(001) preparation technology of the hexagonal plate magnesium hydroxide fire retardant of crystal face dominant growth.
Background technology
With the progress of society, macromolecular material has also obtained the macromolecule materials such as swift and violent development, plastics, rubber, fiber
Material is also widely used for the fields such as chemical industry, Aero-Space, automobile, building trade.Be indispensable life in people's life,
The producer goods.But most of macromolecule product easily burns, and the product of dense smoke and toxic gas is generally entailed in combustion process
Raw, this life and property safety to the mankind constitutes grave danger, while also severe contamination can be caused to environment.The fire for taking place frequently
Calamity forces people to put forward higher requirement the fire resistance of various materials.
Magnesium hydroxide is a kind of thermally-stabilised good, nontoxic, suppression cigarette inorganic additive flame retardant.Generate in combustion
Water and magnesium oxide are not polluted to air, and are also had in neutralization combustion process while corrosive gas is not produced
The acidity and corrosive gas function of generation, is a kind of fire retardant of environmental protection, and the heat decomposition temperature of magnesium hydroxide is higher,
About 140 DEG C are higher by than aluminium hydroxide, fire proofing can be made to bear higher processing temperature, beneficial to extrusion molding speed is accelerated, shortened
Molding cycle.It is the inorganic combustion inhibitor kind very with development prospect.
Magnesium hydroxide although have the advantages that it is many, but there is also some defects, the flame retarding efficiency of magnesium hydroxide is relatively low, hydrogen
Magnesium oxide will reach the addition of flame retardant effect than larger, and run-of-the-mill fraction reaches 60%, due to the big magnesium hydroxide of addition
Poor with the compatibility of macromolecular material, this can be damaged to the mechanical performance and processing characteristics of polymer composite.
So using hydro-thermal method in magnesium hydroxide after dissolve-repreparation herein so that the weaker crystal face of its polarity fully appears, therefore
With lower surface polarity, while dispersibility is improved, mean diameter reaches 11 μm or so of hexagonal plate magnesium hydroxide.
The content of the invention
It is an object of the invention to provide a kind of preparation method of hexagonal plate magnesium hydroxide, obtain that surface polarity is low, dispersion
The good, mean diameter of property is 1 μm or so of hexagonal plate magnesium hydroxide.
The preparation method of the hexagonal plate magnesium hydroxide of one kind (001) crystal face dominant growth of the invention, its step is as follows:
(1) raw material magnesium hydroxide is distributed in sodium hydroxide solution in the way of ball milling, ball milling is configured to solid content and is
5%~30% slurry.
(2) ground magnesium hydroxide slurry is added in the water heating kettle of inner liner polytetrafluoroethylene, temperature be 120~
Hydrothermal treatment consists are carried out in the range of 200 DEG C.
(3) product will be cooled down after the completion of reaction, is filtered, washing is put into oven drying.
The concentration of sodium hydroxide is 4~8mol/L in described step (1).
Ball-milling Time described in described step (1) is 8~12h.
The time of hydrothermal treatment consists is 4~10h in described step (2).
The time being dried in described step (3) is 8~12h.
The present invention is prepared for the hexagonal plate magnesium hydroxide fire retardant of (001) crystal face dominant growth.By the hydrogen of certain mass
Magnesium oxide and sodium hydroxide solution are poured in screw socket bottle carries out ball milling dispersion, and then scattered serosity is added in water heating kettle
Dissolving-recrystallization is carried out in the range of 120~200 DEG C of temperature.Filter after cooling, wash, be dried.By magnesium hydroxide dissolving-
After recrystallization, it is completely homogeneous to have obtained crystal morphology, and corner angle are clearly demarcated, edge clear, the hexagonal plate magnesium hydroxide in rule.And
And the weaker crystal face ((001) crystal face) of its polarity of the hexagonal plate magnesium hydroxide of preparation is appeared so that the polarity drop of crystal
It is low, reunite and reduce.Simultaneously dispersibility is improved, and mean diameter reaches 11 μm or so.The magnesium hydroxide tool of crystal pattern
There is the different shape characteristic of common crystal pattern, so because their special appearance is to height when they are added in macromolecular material
Molecule plays different effects, and the particle diameter of hexagonal plate magnesium hydroxide is less with thickness ratio, easily with resin mixing, to macromolecule
The physical and mechanical propertiess of polymer affect little.
The magnesium hydroxide of hexagonal plate is added to into result in polyethylene and finds that magnesium hydroxide can refer to the oxygen of polyethylene
Number brings up to 22.6% from 19.2%, enhances its fire resistance.The polythene material of addition hexagonal plate magnesium hydroxide is in net
Shape structure, improves the tensile strength of polyethylene, but elongation at break is then reduced with the increase of addition, and modified
Magnesium hydroxide preferably, is able to maintain that the mechanical property of polyethylene with the polythene material compatibility.
Description of the drawings
Fig. 1 is the SEM figures of the magnesium hydroxide of the hexagonal plate that the present invention prepares (001) crystal face dominant growth.
Fig. 2 is the XRD figure of the magnesium hydroxide of the hexagonal plate that the present invention prepares (001) crystal face dominant growth.
Specific embodiment
For a better understanding of the present invention, now specific embodiment is listed below, embodiment can be done into one to the present invention
The explanation and explanation of step, but the present invention is not limited to Examples below.
Embodiment 1:
A kind of preparation technology circuit of hexagonal plate magnesium hydroxide:14.44g magnesium hydroxide is weighed, by the hydroxide for weighing
Magnesium and 57.75g molar concentrations pour screw socket bottle into for 4mol/L sodium hydroxide solutions, and the solid content that ball milling disperses after 8~12h is
The slurry of 20wt.% is added in water heating kettle hydrothermal treatment consists 8h at 200 DEG C, and question response terminates.Will cooling after, filter, washing,
The siccative of 14.22g is dried to obtain, its yield is 98.50%, and scanned electron-microscope scanning, product is hexagonal plate magnesium hydroxide.
Embodiment 2:
14.44g magnesium hydroxide is weighed, is 6mol/L sodium hydroxide by the magnesium hydroxide for weighing and 274.36g molar concentrations
Solution pours screw socket bottle into, and ball milling disperses 8~12h.Slurry of the solid content after ball milling for 5wt.% is added in water heating kettle
Hydrothermal treatment consists 4h at 200 DEG C, question response cools down, filters, washing, being dried to obtain the siccative of 13.86g after terminating, its yield is
95.98%, scanned electron-microscope scanning, product is hexagonal plate magnesium hydroxide.
Embodiment 3:
14.44g magnesium hydroxide is weighed, is that 4mol/L sodium hydroxide is molten by the magnesium hydroxide for weighing and 57.75g molar concentrations
Liquid pours screw socket bottle into, and ball milling disperses 8~12h.Slurry of the solid content after ball milling for 30wt.% is added in water heating kettle
Hydrothermal treatment consists 10h at 120 DEG C, question response cools down, filters, washing, being dried to obtain the siccative of 14.28g after terminating, its yield is
98.89%, scanned electron-microscope scanning, product is hexagonal plate magnesium hydroxide
Embodiment 4:
14.44g magnesium hydroxide is weighed, is 8mol/L sodium hydroxide by the magnesium hydroxide for weighing and 129.96g molar concentrations
Solution pours screw socket bottle into, and ball milling disperses 8~12h.Slurry of the solid content after ball milling for 10wt.% is added in water heating kettle
Hydrothermal treatment consists 8h at 160 DEG C, question response cools down, filters, washing, being dried to obtain the siccative of 14.10g after terminating, its yield is
97.66%, scanned electron-microscope scanning, product is hexagonal plate magnesium hydroxide.
Embodiment 5:
14.44g magnesium hydroxide is weighed, is that 4mol/L sodium hydroxide is molten by the magnesium hydroxide for weighing and 43.32g molar concentrations
Liquid pours screw socket bottle into, and ball milling disperses 8~12h.Slurry of the solid content after ball milling for 25wt.% is added in water heating kettle
Hydrothermal treatment consists 8h at 140 DEG C, question response cools down, filters, washing, being dried to obtain the siccative of 14.30g after terminating, its yield is
99.03%, scanned electron-microscope scanning, product is hexagonal plate magnesium hydroxide.‘
Embodiment 6:
14.44g magnesium hydroxide is weighed, is that 4mol/L sodium hydroxide is molten by the magnesium hydroxide for weighing and 57.75g molar concentrations
Liquid pours screw socket bottle into, and ball milling disperses 8~12h.Slurry of the solid content after ball milling for 20wt.% is added in water heating kettle
Hydrothermal treatment consists 8h at 180 DEG C, question response cools down, filters, washing, being dried to obtain the siccative of 13.80g after terminating, its yield is
95.57%, scanned electron-microscope scanning, product is hexagonal plate magnesium hydroxide.
Claims (5)
1. a kind of preparation method of the hexagonal plate magnesium hydroxide of (001) crystal face dominant growth, it is characterised in that step is as follows:
(1) raw material magnesium hydroxide is distributed in sodium hydroxide solution in the way of ball milling, ball milling be configured to solid content for 5%~
30% slurry.
(2) ground magnesium hydroxide slurry is added in the water heating kettle of inner liner polytetrafluoroethylene, is 120~200 DEG C in temperature
In the range of carry out hydrothermal treatment consists.
(3) product will be cooled down after the completion of reaction, is filtered, washing is put into oven drying.
2. method according to claim 1, it is characterised in that:The concentration of sodium hydroxide is 4~8mol/L in step (1).
3. method according to claim 1, it is characterised in that:Ball-milling Time described in step (1) is 8~12h.
4. method according to claim 1, it is characterised in that:The time of hydrothermal treatment consists is 4~10h in step (2).
5. method according to claim 1, its feature in:The time dry in an oven is 8~12h in step (3).
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN111410786A (en) * | 2020-03-25 | 2020-07-14 | 深圳市沃尔核材股份有限公司 | Halogen-free high-flame-retardant oil-resistant thermal shrinkage identification tube and production method thereof |
CN112239222A (en) * | 2019-07-18 | 2021-01-19 | 自然资源部天津海水淡化与综合利用研究所 | Equipment and method for continuous hydrothermal production of magnesium hydroxide |
CN113582209A (en) * | 2021-08-26 | 2021-11-02 | 上海应用技术大学 | Preparation method and application of hexagonal flaky magnesium hydroxide |
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CN102502726A (en) * | 2011-10-28 | 2012-06-20 | 南京工业大学 | Preparation method for hexagonal sheet magnesium hydroxide |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN112239222A (en) * | 2019-07-18 | 2021-01-19 | 自然资源部天津海水淡化与综合利用研究所 | Equipment and method for continuous hydrothermal production of magnesium hydroxide |
CN111410786A (en) * | 2020-03-25 | 2020-07-14 | 深圳市沃尔核材股份有限公司 | Halogen-free high-flame-retardant oil-resistant thermal shrinkage identification tube and production method thereof |
CN111410786B (en) * | 2020-03-25 | 2023-07-07 | 深圳市沃尔核材股份有限公司 | Halogen-free high-flame-retardant oil-resistant heat-shrinkable identification tube and production method thereof |
CN113582209A (en) * | 2021-08-26 | 2021-11-02 | 上海应用技术大学 | Preparation method and application of hexagonal flaky magnesium hydroxide |
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Application publication date: 20170426 |