CN101679058A - Magnesium hydroxide powder and preparation method thereof - Google Patents
Magnesium hydroxide powder and preparation method thereof Download PDFInfo
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- CN101679058A CN101679058A CN200880018158A CN200880018158A CN101679058A CN 101679058 A CN101679058 A CN 101679058A CN 200880018158 A CN200880018158 A CN 200880018158A CN 200880018158 A CN200880018158 A CN 200880018158A CN 101679058 A CN101679058 A CN 101679058A
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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
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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- 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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/016—Flame-proofing or flame-retarding additives
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- 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
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- C08K9/04—Ingredients treated with organic substances
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/12—Surface area
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- C01P2006/14—Pore volume
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- 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
Abstract
Containing spherical offspring, the BET specific surface area that the median size that is formed by lepidiod primary particle is 1.0～4.8 μ m is 1～10m
2The magnesium hydroxide powder water absorbability of/g is low, is suitable for use as the fire retardant of resin.
Description
Technical field
The present invention relates to magnesium hydroxide powder of low BET specific surface area and preparation method thereof.
Background technology
Magnesium hydroxide powder is used for various uses, and one of its purposes has as resin, in particular as the purposes of the fire retardant of the resin combination of the coating material of electric wire or cable.As the resin of fire-retardantization object, polyolefine such as polyethylene, polypropylene, ethylene-propylene rubber (EPM), ethylene-propylene-diene terpolymer title complex (EPDM), ethylene-ethyl acrylate copolymer (EEA), vinyl-vinyl acetate copolymer are arranged.
Industrial production process as magnesium hydroxide powder, usual method is as follows: drop into alkali sources such as milk of lime in seawater, make magnesium ion and alkali source reaction in the seawater, obtain being dispersed with the magnesium hydroxide slurries of the spherical offspring that forms by lepidiod primary particle thus, then this magnesium hydroxide slurries is washed, after dehydration etc. handles, carries out drying formation powder.This use seawater as the preparation method of the magnesium hydroxide powder in magnesium source (below be sometimes referred to as the seawater method) in advantageous method aspect the preparation cost.But the magnesium hydroxide powder that is obtained by this seawater method is the spherical offspring of 1.0～4.8 μ m owing to contain the median size that is formed by lepidiod primary particle usually, BET specific surface area height, is 11～50m
2Therefore/g exists the high trend of absorptivity.If the magnesium hydroxide powder of moisture absorption is used for the fire retardant of resin combination of the coating material etc. of electric wire or cable, then because the heat during with resin mixing, the moisture evaporation of magnesium hydroxide powder moisture absorption and foaming might cause damaging the outward appearance of the resin combination that obtains.Therefore, developing water absorbability low is the low magnesium hydroxide powder of specific surface area.
The specific surface area that discloses the median size that contains flakey magnesium hydroxide primary particle cohesion and form in the patent documentation 1 and be the spherical offspring of 5～500 μ m is 10m
2The magnesium hydroxide powder that/g is following.According to this patent documentation 1, above-mentioned magnesium hydroxide powder can be 500kg/m at the crystallization load of magnesium hydroxide by making the aqueous solution and the ammonia that contain water soluble magnesium
3Magnesium hydroxide slurries concentration in the following and crystallization device of h is to react under the condition of 1～60wt% to prepare.
The BET specific surface area is disclosed in the patent documentation 2 less than about 10m
2/ g, median size is about 0.5～10.0 micron, and the particle that surpasses 10 microns is less than about 0.5%, and most crystallizations have the roughly flame retardant resistance magnesium hydroxide powder in the cross section of ovum type.According to this patent documentation 2, above-mentioned magnesium hydroxide powder can add excess of ammonia raw material on the molecular weight by being included in the magnesium chloride solution, form the precipitation of magnesium hydroxide, and the method for magnesium hydroxide with the step of hot water recrystallization prepared.
Patent documentation 1: Japanese kokai publication sho 61-168522 communique
Patent documentation 2: Japanese Unexamined Patent Application Publication 2001-508015 communique
Summary of the invention
It is spherical or avette disclosing particle shape in above-mentioned patent documentation 1 and the patent documentation 2, and the BET specific surface area is 10m
2The magnesium hydroxide powder that/g is following.Wherein, the magnesium hydroxide powder of record in the patent documentation 1 because the median size of offspring is big, during as fire retardant, the resin combination that obtains except outward appearance become coarse, stress is easily concentrated, intensity has the trend that dies down.In addition, though the magnesium hydroxide powder of record is fine in the patent documentation 2, not spherical, therefore existing problems of the dispersiveness in resin, during this external its preparation, essential hot-water cure, preparation process is miscellaneous and preparation cost has the trend of increase.
Therefore, the objective of the invention is to, the magnesium hydroxide powder that comprises fine spherical particle of the low BET specific surface area of the fire retardant that particularly is suitable for use as resin is provided.
The inventor finds, the magnesium hydroxide slurries that will in the seawater method, obtain or this magnesium hydroxide slurries is carried out the water ratio that processed obtains is the moisture magnesium hydroxide solids of 10～50 quality % as intermediate product, dry lentamente under the drying conditions that until water ratio is the time of 5 quality % needs more than 2 hours, after the formation water ratio is the moisture magnesium hydroxide powder of 1～5 quality %, being dried to water ratio is below the 0.5 quality %, obtain thus the BET specific surface area low, be 1～10m
2/ g and be shaped as the globular magnesium hydroxide powder.In addition, the inventor finds that making the BET specific surface area that obtains by the seawater method is 11～50m
2The magnesium hydroxide powder of/g (water ratio: 0.5 quality % is following) contacts with water vapour under the moisture absorption condition that until water ratio is the time of 1 quality % needs more than 30 minutes, the water ratio that makes magnesium hydroxide powder lentamente be 1 quality % above after, being dried to water ratio is below the 0.5 quality %, obtain thus the BET specific surface area low, be 1～10m
2/ g and be shaped as the globular magnesium hydroxide powder.
Therefore, the present invention is that to comprise spherical offspring, the BET specific surface area that the median size that is formed by lepidiod primary particle is 1.0～4.8 μ m be 1～10m
2The magnesium hydroxide powder of/g.
The optimal way of magnesium hydroxide powder of the present invention is as described below.
(1) spherical offspring, the length of longest diameter is 1 o'clock in the diameter of three mutually orthogonal directions, the length of other two diameters is respectively 0.6～1.
(2) aperture is that the maximum value of logarithmic differentiation pore volume in the hole of 3～5nm is 0.001～0.14cm
3/ g.
(3) handle with lipid acid, fatty acid soaps or silane coupling agent on the surface.
(4), contain above-mentioned lipid acid, fatty acid soaps or silane coupling agent 0.1～10 mass parts with respect to magnesium hydroxide 100 mass parts.
Magnesium hydroxide powder of the present invention can particularly advantageously be used as the fire retardant of resin.Therefore, the present invention is the resin combination that is mixed with the magnesium hydroxide powder of the invention described above.
In addition, the present invention is the preparation method of the magnesium hydroxide powder of the invention described above, this method comprises the magnesium hydroxide slurries that is dispersed with the spherical offspring that is formed by lepidiod primary particle by the reaction of magnesium ion in the seawater and alkali source is obtained, or this magnesium hydroxide slurries is carried out the water ratio that processed obtains is the moisture magnesium hydroxide solids of 10～50 quality %, dry under the drying conditions that until water ratio is the time of 5 quality % needs more than 2 hours, obtaining water ratio is the moisture magnesium hydroxide powder of 1～5 quality %, and then should moisture magnesium hydroxide powder being dried to water ratio is below the 0.5 quality %.
Among the preparation method of the magnesium hydroxide powder of the invention described above, it is that 50～100 ℃, relative humidity are the condition of 50～85%RH that the drying conditions of magnesium hydroxide slurries or moisture magnesium hydroxide solids is preferably temperature.
Further, the present invention is the preparation method of the magnesium hydroxide powder of the invention described above, and this method comprises: make by magnesium hydroxide slurries preparation to contain spherical offspring, the BET specific surface area that the median size that is formed by lepidiod primary particle is 1.0～4.8 μ m be 11～50m
2/ g, water ratio are the following magnesium hydroxide powder of 0.5 quality %, under the moisture absorption condition that until water ratio is the time of 1 quality % needs more than 30 minutes, contact with water vapour, obtain water ratio and be the moisture magnesium hydroxide powder of 1 quality % above (particularly 5 quality % are following), then should moisture magnesium hydroxide powder being dried to water ratio is below the 0.5 quality %.The magnesium hydroxide slurries that be dispersed with the spherical offspring that by lepidiod primary particle form of wherein said magnesium hydroxide slurries for obtaining by magnesium ion in the seawater and alkali source reaction.
Among the preparation method of the magnesium hydroxide powder of the invention described above, the moisture absorption condition optimization of magnesium hydroxide powder is that temperature is that 10～100 ℃, relative humidity are the condition of 50～98%RH.
Magnesium hydroxide powder of the present invention is because the BET specific surface area is low, water absorbability is low, and long-term moisture absorption is few and stable, owing to be made of fine spherical offspring, therefore the dispersiveness in resin is high in addition.Therefore, magnesium hydroxide powder of the present invention is specially suitable as the fire retardant of resin.
In addition, by utilizing preparation method of the present invention, can use the magnesium hydroxide slurries that obtains as intermediate product in the magnesium hydroxide powder, seawater method of the seawater method preparation by industrial cheapness or moisture magnesium hydroxide solids as raw material, the magnesium hydroxide powder that the BET specific surface area of fire retardant that preparation is suitable for use as resin is low, contain fine spherical offspring.
Embodiment
Magnesium hydroxide powder of the present invention contains the spherical offspring that the median size that is formed by lepidiod primary particle is 1.0～4.8 μ m, and the BET specific surface area is 1～10m
2/ g.The median size of spherical offspring is preferably 1.0～4.5 μ m, is preferably 1.2～4.0 μ m especially.The BET specific surface area is preferably 2～9m
2/ g.
In the magnesium hydroxide powder of the present invention, the offspring of magnesium hydroxide is spherical referring to, and the length of longest diameter is 1 o'clock in the diameter of three mutually orthogonal directions of offspring, and the length of other two diameters is respectively 0.6～1, is preferably 0.8～1.
Magnesium hydroxide powder of the present invention for example can be by the method preparation of following (1) or (2).
(1) comprises the magnesium hydroxide slurries that is dispersed with the spherical offspring that forms by lepidiod primary particle that to obtain as intermediate product in the seawater method or this magnesium hydroxide slurries is carried out the water ratio that processed obtains is the moisture magnesium hydroxide solids of 10～50 quality %, dry under the drying conditions that until water ratio is the time of 5 quality % needs more than 2 hours, obtaining water ratio is the moisture magnesium hydroxide of 1～5 quality %, and then will this moisture magnesium hydroxide powder being dried to water ratio is the following method of 0.5 quality %.
(2) comprise make by seawater method preparation to contain spherical offspring, the BET specific surface area that the median size that is formed by lepidiod primary particle is 1.0～4.8 μ m be 11～50m
2/ g is following, water ratio is the following magnesium hydroxide powder of 0.5 quality %, under the moisture absorption condition that until water ratio is the time of 1 quality % needs more than 30 minutes, contact with water vapour, obtain water ratio and be the moisture magnesium hydroxide powder of 1 quality % above (particularly 5 quality % are following), then will this moisture magnesium hydroxide powder be dried to water ratio and be the method below the 0.5 quality %.
In the method for above-mentioned (1), at first prepare the mixed solution of seawater and alkali source, make magnesium ion and alkali source reaction in the seawater, the flakey primary particle of magnesium hydroxide is separated out.The flakey primary particle of separating out is circulated in mixed solution, make the cohesion of flakey primary particle, be grown to the globular offspring, can obtain being dispersed with the magnesium hydroxide slurries of spherical offspring thus.
As the seawater in magnesium source, preferably carry out decarbonate in advance and handle, making dissolved carbonic acid ionic concn is 20 quality ppm following (being scaled carbonic acid gas).As the decarbonate treatment process, can use in seawater, add milk of lime (calcium hydroxide slurry), with the form fixed method of carbonic acid ion with lime carbonate, or acidic solutions such as hydrochloric acid, sulfuric acid are added in the seawater, make the pH of seawater is back below 4, seawater is carried out aeration handles the method for thus the carbonic acid ion being removed with the form of carbon dioxide.And the decarbonate treatment process of the former use milk of lime reduces its content owing to silicon or aluminium component in the adsorbing seawater on the lime carbonate that generates, is preferred method therefore.
As with the alkali source of sea water mixing, can use milk of lime.
The mixture ratio of seawater and alkali source, be preferably with seawater in the reactivity (molar percentage of the magnesium ion in the seawater of separating out as magnesium hydroxide particles with alkali source reaction) of magnesium ion be 50～110% ratio, be preferably 70～90% ratio especially.If reactivity is crossed low then from the yield aspect consideration of magnesium hydroxide powder, is disadvantageous economically.
In the method for above-mentioned (1), with the magnesium hydroxide slurries of so preparation directly or filter etc. after common processed forms water ratio and be the moisture magnesium hydroxide solids of 10～50 quality %, join in the drying installation, until water ratio be that 5 quality needed more than 2 hours, dry under the drying conditions of preferred more than 4 hours, time of more preferably 24 hours～200 hours, obtaining water ratio is the moisture magnesium hydroxide powder of 1～5 quality %.Until water ratio is that time of 5 quality % can be by temperature and the relative humidity adjustment in the drying installation.Temperature in the drying installation is generally 50～100 ℃, is preferably 60～90 ℃, and relative humidity is generally 50～85%RH.The concentration of the magnesium hydroxide slurries before dry is generally 10～45 quality %.With directly the magnesium hydroxide slurries drying is compared, carry out drying after being preferably formed moisture magnesium hydroxide solids.
With the water ratio that as above obtains is the moisture magnesium hydroxide powder of 1～5 quality %, then join in the common drying installation such as hot-air drier (for example box-shaped moisture eliminator, pneumatic dryer, exhaust pass ventilation moisture eliminator, fluidized bed dryer, rotatory drier) and heat transfer by conduction moisture eliminator (for example drum dryer, disk dryer), being dried to water ratio is below the 0.5 quality %.Drying temperature is generally more than 100 ℃, is preferably 110～150 ℃.To not limiting especially time of drying, still be generally 0.01～2 hour.
In the method for above-mentioned (2), use the magnesium hydroxide powder by the preparation of seawater method, promptly containing spherical offspring, the BET specific surface area that the median size that is formed by lepidiod primary particle is 1.0～4.8 μ m is 11～50m
2/ g, water ratio are that the following magnesium hydroxide powder of 0.5 quality % is as starting raw material.
As the magnesium hydroxide powder that becomes raw material, can preferably use with the method for above-mentioned (1) similarly, react the flakey primary particle cohesion of the magnesium hydroxide of separating out by magnesium ion in the seawater and alkali source, be grown to spherical offspring, obtain magnesium hydroxide slurries, it is washed, processing such as dehydration, after the formation water ratio is the moisture magnesium hydroxide solids of 10～50 quality %, join in the common drying installation such as hot-air drier and heat transfer by conduction moisture eliminator, more than 100 ℃, drying is 0.01～2 hour under preferred 110～150 ℃ temperature, and making water ratio thus is the following magnesium hydroxide powder of 0.5 quality %.
In the method for above-mentioned (2), the magnesium hydroxide powder (water ratio: 0.5 quality % following) that makes raw material until water ratio is being that 1 quality % needed more than 30 minutes, contact with water vapour under the moisture absorption condition of preferred more than 2 hours, time of more preferably 24 hours～200 hours, obtains water ratio and be that 1 quality % is above, preferred 2 quality % are above, the more preferably moisture magnesium hydroxide powder below the 5 quality %.Specifically, the magnesium hydroxide powder of raw material is contacted with the gas that contains water vapour with state, fluidised bed or the static condition that swims in air-flow, obtaining water ratio thus is the above moisture magnesium hydroxide powder of 1 quality %.Until water ratio is relative humidity or the temperature adjustment of time by the steam-laden gas (being generally air) that contacts with magnesium hydroxide more than the 1 quality %.Condition when making the magnesium hydroxide powder moisture absorption is that temperature is generally 10～100 ℃, preferred 50～90 ℃, and relative humidity is generally 50～98%RH.
With the water ratio that as above obtains is moisture magnesium hydroxide powder more than the 1 quality %, joins in the common drying installation such as hot-air drier and heat transfer by conduction moisture eliminator after then, and being dried to water ratio is below the 0.5 quality %.Drying temperature is generally more than 100 ℃, is preferably 110～150 ℃.To not limiting especially time of drying, still be generally 0.01～2 hour.
The magnesium hydroxide powder of the present invention that obtains by aforesaid method and is compared by the magnesium hydroxide powder of common seawater method preparation, and the aperture is that the maximum value of logarithmic differentiation pore volume in the hole of 3～5nm shows as low value.The aperture is the hole of 3～5nm, owing to be equivalent to be formed on the hole between the primary particle of magnesium hydroxide, think magnesium hydroxide powder of the present invention with compare by the magnesium hydroxide powder of common seawater method preparation, fine pore volume between the primary particle is little, therefore the BET specific surface area is low, and water absorbability is low.Magnesium hydroxide powder of the present invention, aperture are that the maximum value of logarithmic differentiation pore volume in the hole of 3～5nm is generally 0.001～0.14cm
3/ g is preferably 0.005～0.10cm
3/ g.
Magnesium hydroxide powder of the present invention, itself is compared separately with by the magnesium hydroxide powder of common seawater method preparation, have the low characteristic of water absorbability,, can handle by lipid acid, fatty acid soaps or silane coupling agent the surface in order further to reduce its water absorbability.The content of lipid acid, fatty acid soaps and silane coupling agent with respect to magnesium hydroxide 100 mass parts, is preferably 0.1～10 mass parts.As the example of lipid acid, can enumerate stearic acid and oleic acid.Fatty acid soaps is preferably sodium salt or sylvite.
The fire retardant of the resin combination that magnesium hydroxide powder of the present invention can be advantageously used for resin, particularly use as the coating material of electric wire or cable.As the resin of fire-retardantization object, polyolefine such as polyethylene, polypropylene, ethylene-propylene rubber (EPM), ethylene-propylene-diene terpolymer title complex (EPDM), ethylene-ethyl acrylate copolymer (EEA), vinyl-vinyl acetate copolymer are arranged.The use level of the magnesium hydroxide powder in these resins with respect to resin 100 mass parts, is generally 10～150 mass parts, is preferably 30～100 mass parts.
The resin combination that contains magnesium hydroxide powder of the present invention can be by using common mixing rolls such as Banbury mixer, rotary drum, pressurization kneading machine, mixing extruder, biaxial extruder, with resin and magnesium hydroxide powder is mixing prepares.The resin combination that contains magnesium hydroxide powder of the present invention can contain inorganic filling materials such as talcum as required, lubricant such as silicone oil or lipid acid, tensio-active agent such as silane coupling agent or fatty acid soaps, and then the various additives that use in the common resin combination such as softening agent, tenderizer, antiaging agent, tinting material, antioxidant, UV light absorber, stabilization agent, linking agent.
Embodiment
In the present embodiment, the maximum value and the moisture-absorption characteristics of the logarithmic differentiation pore volume in the sphericity of water ratio, average aggregate particle size, offspring, the hole that the aperture is 3～5nm are measured by following method.
[water ratio]
Sample 5g is joined in the moisture meter (MX-50, (strain) worker one-ァ Application De-デ ィ system), and in 180 ℃ of heating down of temperature, the rate of mass reduction when the quality minimizing is reached balance is calculated as water ratio.
[average aggregate particle size]
Sample 0.5g is put among the ethanol 50mL, use ultrasonic homogenizer under the condition of output 200 μ A, to carry out 2 minutes dispersion treatment, the preparation magnesium magma.Use laser diffraction and scattering method size-grade distribution meter (マ ィ Network ロ ト ラ Star Network particle size distribution device 9320HRA (X-100), day machine dress (strain) system) to measure the median size of the volume reference of the magnesium hydroxide particles that contains in this magnesium magma then.
[sphericity of offspring]
The sample table angle that makes scanning electron microscope (SEM) is 0 degree (level), takes the magnesium hydroxide offspring, determines the diameter of offspring, measures its length.Making the direction of measuring this diameter is turning axle, and the sample table angle from inclined+45 degree, is taken the magnesium hydroxide offspring, the diameter of the offspring of the direction of mensuration and rotating shaft direct cross.Then, the sample table angle from inclined-45 degree, is taken the magnesium hydroxide offspring, the diameter of the offspring of the direction of mensuration and rotating shaft direct cross.Make sample table angle 0 degree ,+diameter of the magnesium hydroxide offspring that 45 degree ,-45 degree are measured in the length of longest diameter be X=1, with the length Y of the second long diameter, will be the shortest the length Z of diameter calculate as relative value.
[maximum value of logarithmic differentiation pore volume]
Use Quantachrome (strain) system, full-automatic gas adsorptive capacity determinator (Autosorb-3B), measure desorption isotherm by the nitrogen adsorption method, data by this desorption isotherm are passed through the BJH method, calculating with the specific surface area is that the aperture of benchmark is the logarithmic differentiation pore volume in the hole of 3～5nm, tries to achieve its maximum value.
[moisture-absorption characteristics]
Magnesium hydroxide powder is put in the controlled thermohygrostat that is set at 30 ℃ of temperature, relative humidity 80%RH, drop into the back and measured the quality of magnesium hydroxide powder until 180 minutes in per 30 minutes, measured the quality of magnesium hydroxide powder, its quality increment rate is calculated as the moisture rate of moisture absorption in per then 60 minutes.
[embodiment 1]
(1) preparation of moisture magnesium hydroxide solids
To being scaled the seawater of 80 quality ppm according to carbonic acid gas in, dissolved carbon acid ion concentration adds milk of lime, the dissolved carbon acid ion is separated out as lime carbonate, after making dissolved carbon acid ion concentration be reduced to 10 quality ppm, filter, remove lime carbonate with sand filter according to the carbonic acid gas conversion.In the seawater that the content of dissolved carbon acid ion reduces, be that 80% ratio adds milk of lime and prepares mixed solution with the magnesium hydroxide ionic reactivity that contains in this seawater, this mixed solution is put in the thickener.By thickener the flakey primary particle of the magnesium hydroxide of separating out is circulated, make the cohesion of flakey primary particle, be grown to spherical offspring, obtain being dispersed with the magnesium hydroxide slurries of spherical offspring.This magnesium hydroxide slurries is derived from the thickener bottom, wash with water remove salt residues after, use the Nutsche suction strainer, obtaining water ratio is the moisture magnesium hydroxide solids of 33.5 quality %.
(2) preparation of magnesium hydroxide powder
Moisture magnesium hydroxide solids joined in the controlled thermohygrostat that is set at 85 ℃ of temperature, relative humidity 65%RH left standstill 48 hours, obtain water ratio and be the moisture magnesium hydroxide powder (is time of 5 quality % to be about 30 hours until water ratio) of 1.1 quality %.Then moisture magnesium hydroxide powder was joined in the box-shaped moisture eliminator that is set at 120 ℃ of temperature dry 2 hours.The water ratio of the magnesium hydroxide powder that obtains is below the 0.5 quality %.
Use scanning electron microscope (SEM) to observe to the particle shape of the magnesium hydroxide powder that obtains.Figure 1 shows that the SEM photo.Photo by Fig. 1 confirms that magnesium hydroxide powder is made of the spherical offspring that lepidiod primary particle cohesion forms.
The chemical ingredients of the magnesium hydroxide powder that obtains, BET specific surface area, average aggregate particle size, aperture are that the sphericity of the maximum value of logarithmic differentiation pore volume in hole of 3～5nm and offspring is as shown in table 1.The measurement result of the moisture-absorption characteristics of magnesium hydroxide powder as shown in Figure 2.
[embodiment 2]
The water ratio that to use the method preparation identical with embodiment 1 (1) is that the moisture magnesium hydroxide solids of 33.5 quality % joins temperature and is set in 120 ℃ the box-shaped moisture eliminator dry 1 hour, and forming water ratio is the following magnesium hydroxide powder of 0.5 quality %.This magnesium hydroxide powder joined in the controlled thermohygrostat that is set at 85 ℃ of temperature, relative humidity 80%RH left standstill 24 hours, the magnesium hydroxide powder after leaving standstill is that water ratio is the moisture magnesium hydroxide powder of 2.1 quality %.Then, moisture magnesium hydroxide powder is joined temperature and be set in 120 ℃ the box-shaped moisture eliminator dry 2 hours.The water ratio of the magnesium hydroxide powder that obtains is below the 0.5 quality %.
Use scanning electron microscope (SEM) to observe to the particle shape of the magnesium hydroxide powder that obtains, results verification forms the spherical offspring that lepidiod primary particle cohesion forms.
The chemical ingredients of the magnesium hydroxide powder that obtains, BET specific surface area, average aggregate particle size, aperture are that the sphericity of the maximum value of logarithmic differentiation pore volume in hole of 3～5nm and offspring is as shown in table 1.In addition, the measurement result of the moisture-absorption characteristics of magnesium hydroxide powder as shown in Figure 2.
[comparative example 1]
(1) preparation of moisture magnesium hydroxide solids
Be reduced in the seawater of 10 quality ppm to dissolved carbon acid ion concentration is converted according to carbonic acid gas with embodiment 1 (1), with the magnesium hydroxide ionic reactivity that contains in this seawater is that 90% ratio adds milk of lime and prepares mixed solution, and this mixed solution is put in the thickener.In thickener, make the flakey primary particle circulation of the magnesium hydroxide of separating out, make the cohesion of flakey primary particle, be grown to spherical offspring, obtain being dispersed with the magnesium hydroxide slurries of spherical offspring.This magnesium hydroxide slurries is derived from the thickener bottom, wash with water remove salt residues after, use the Nutsche suction strainer, obtaining water ratio is the moisture magnesium hydroxide solids of 38.5 quality %.
(2) preparation of magnesium hydroxide powder
Moisture magnesium hydroxide solids is joined temperature be set in 120 ℃ the box-shaped moisture eliminator dry 1 hour.The water ratio of the magnesium hydroxide powder that obtains is below the 0.5 quality %.
Use scanning electron microscope (SEM) to observe to the particle shape of the magnesium hydroxide powder that obtains, results verification forms the spherical offspring that lepidiod primary particle cohesion forms.
The chemical ingredients of the magnesium hydroxide powder that obtains, BET specific surface area, average aggregate particle size, aperture are that the sphericity of the maximum value of logarithmic differentiation pore volume in hole of 3～5nm and offspring is as shown in table 1.In addition, the measurement result of the moisture-absorption characteristics of magnesium hydroxide powder as shown in Figure 2.
[table 1]
Table 1
By the result of Fig. 2 as can be known, the BET specific surface area is low in the water absorbability of the magnesium hydroxide powder of scope of the present invention.
[embodiment 3]
In the glass beaker of capacity 3L, add pure water 2000g, be heated to 70 ℃ after, add count the sodium stearate as finish materials (Japanese grease (strain) system, ノ Application サ one Le SN-15) of 2.5g with solids component after, stir, dissolve.In this aqueous solution of sodium stearate, add magnesium hydroxide powder 100g, stirred 1 hour when keeping 70 ℃ temperature, in aqueous solution of sodium stearate, disperse magnesium hydroxide powder, the surface of magnesium hydroxide powder is handled with stearic acid by embodiment 2 preparations.
With magnesium hydroxide dispersion liquid Nutsche suction strainer, with the hydrogeneous magnesian solids component that obtains, using with respect to solids component is 20 times water washing.Then to the solids component after the washing with the box-shaped drying machine after carrying out 12 hours dryings under 120 ℃ the temperature, use the sample mill fragmentation.The magnesium hydroxide powder that obtains, with respect to magnesium hydroxide 100 mass parts, attaching surface treatment agent 2.3 mass parts.
The moisture-absorption characteristics of surface-treated magnesium hydroxide powder as shown in Figure 2.Rate of moisture absorption after 360 minutes is 0.5 quality %, is about 40% of the magnesium hydroxide powder before the surface treatment (embodiment 2).
[embodiment 4]
Surface-treated magnesium hydroxide 100 mass parts that the foregoing description 3 is obtained and ethylene-ethyl acrylate copolymer (EEA) 100 mass parts are with being heated to 170 ℃ the brabender plasticorder of temperature under the condition of revolution 60rpm mixing 15 minutes, then with being heated to 150 ℃ the roller of temperature after mixing 5 minutes, further under 160 ℃ temperature with the mixing resin combination that obtains of mixing roll.With the resin combination extrusion forming under 160 ℃ temperature that obtains, obtain the resin combination sheet of thickness 1mm and 3mm.
For the resin combination sheet that as above obtains, carry out the mensuration of melt flow index (MFI), tensile stress at break, elongation and oxygen index.MFI is 0.25g/10 minute (measuring temperature is 190 ℃, mensuration is loaded is 2.16kg) as a result, and tensile stress at break is 9.0MPa, and elongation is 850%, and oxygen index is 26.0.
And, the resin combination sheet of the mensuration used thickness 1mm of MFI, tensile stress at break and elongation, the resin combination sheet of the mensuration used thickness 3mm of oxygen index.Tensile stress at break and elongation are used based on the method for JIS-K-7113 and are measured (No. 1 dumbbell of use-testing sheet).Oxygen index is used based on the method for JIS-K-7201 and is measured.
Description of drawings
[Fig. 1] is the scanning electron microscope photo of the magnesium hydroxide powder of embodiment 1 preparation.
[Fig. 2] is the figure of the measurement result of the moisture-absorption characteristics of the magnesium hydroxide powder of expression embodiment 1～3 and comparative example 1 preparation.
Claims (12)
1. magnesium hydroxide powder, its spherical offspring, BET specific surface area that contains that the median size that is formed by lepidiod primary particle is 1.0～4.8 μ m is 1～10m
2/ g.
2. magnesium hydroxide powder as claimed in claim 1, wherein, the length of longest diameter is 1 o'clock in the diameter of three directions that spherical offspring is mutually orthogonal, the length of other two diameters is respectively 0.6～1.
3. magnesium hydroxide powder as claimed in claim 1, wherein, the aperture is that the maximum value of logarithmic differentiation pore volume in the hole of 3～5nm is 0.001～0.14cm
3/ g.
4. as any described magnesium hydroxide powder in the claim 1～3, wherein, handle with lipid acid, fatty acid soaps or silane coupling agent on the surface.
5. magnesium hydroxide powder as claimed in claim 4 wherein, with respect to magnesium hydroxide 100 mass parts, contains lipid acid, fatty acid soaps or silane coupling agent 0.1～10 mass parts.
6. as any described magnesium hydroxide powder in the claim 1～5, it is as resin fire retardant.
7. resin combination, it is mixed with any described magnesium hydroxide powder in the claim 1～5.
8. the preparation method of the described magnesium hydroxide powder of claim 1, it comprises: will react the magnesium hydroxide slurries that is dispersed with the spherical offspring that is formed by lepidiod primary particle that obtains by magnesium ion in the seawater and alkali source, or this magnesium hydroxide slurries is carried out the water ratio that processed obtains is the moisture magnesium hydroxide solids of 10～50 quality %, dry under the drying conditions that until water ratio is the time of 5 quality % needs more than 2 hours, obtaining water ratio is the moisture magnesium hydroxide powder of 1～5 quality %, and then should moisture magnesium hydroxide powder being dried to water ratio is below the 0.5 quality %.
9. the preparation method of magnesium hydroxide powder as claimed in claim 8, wherein, the drying conditions of magnesium hydroxide slurries or moisture magnesium hydroxide solids is that temperature is that 50～100 ℃, relative humidity are the condition of 50～85%RH.
10. the preparation method of the described magnesium hydroxide powder of claim 1, it comprises: make by the magnesium hydroxide slurries preparation to contain spherical offspring, the BET specific surface area that the median size that is formed by lepidiod primary particle is 1.0～4.8 μ m be 11～50m
2/ g, water ratio are the following magnesium hydroxide powder of 0.5 quality %, under the moisture absorption condition that until water ratio is the time of 1 quality % needs more than 30 minutes, contact with water vapour, obtaining water ratio is the above moisture magnesium hydroxide powder of 1 quality %, then should moisture magnesium hydroxide powder being dried to water ratio is below the 0.5 quality %
Wherein said magnesium hydroxide slurries is the magnesium hydroxide slurries that is dispersed with the spherical offspring that is formed by lepidiod primary particle that obtains by magnesium ion in the seawater and alkali source reaction.
11. the preparation method of magnesium hydroxide powder as claimed in claim 10, wherein, the water ratio of moisture magnesium hydroxide powder is below the 5 quality %.
12. the preparation method of magnesium hydroxide powder as claimed in claim 10, wherein, the moisture absorption condition of magnesium hydroxide powder is that temperature is that 10～100 ℃, relative humidity are the condition of 50～98%RH.
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| JP2007092113 | 2007-03-30 | ||
| JP092113/2007 | 2007-03-30 | ||
| PCT/JP2008/056178 WO2008120746A1 (en) | 2007-03-30 | 2008-03-28 | Magnesium hydroxide powder and method for producing the same |
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| CN101679058B CN101679058B (en) | 2012-11-14 |
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|---|---|
| JP (1) | JP5172824B2 (en) |
| KR (1) | KR101369121B1 (en) |
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| WO (1) | WO2008120746A1 (en) |
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| JP2731854B2 (en) * | 1989-02-10 | 1998-03-25 | 協和化学工業株式会社 | Method for producing high hydration resistant and high fluidity magnesium oxide |
| JP2736545B2 (en) * | 1989-04-27 | 1998-04-02 | 宇部マテリアルズ株式会社 | Magnesium hydroxide particles |
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-
2008
- 2008-03-28 KR KR1020097022533A patent/KR101369121B1/en active IP Right Grant
- 2008-03-28 WO PCT/JP2008/056178 patent/WO2008120746A1/en active Application Filing
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Also Published As
| Publication number | Publication date |
|---|---|
| CN101679058B (en) | 2012-11-14 |
| KR101369121B1 (en) | 2014-03-04 |
| JPWO2008120746A1 (en) | 2010-07-15 |
| KR20090125212A (en) | 2009-12-03 |
| WO2008120746A1 (en) | 2008-10-09 |
| JP5172824B2 (en) | 2013-03-27 |
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