CN102500299A - Preparation method for nanoscale modified magnesium hydroxide - Google Patents
Preparation method for nanoscale modified magnesium hydroxide Download PDFInfo
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- CN102500299A CN102500299A CN2011103754859A CN201110375485A CN102500299A CN 102500299 A CN102500299 A CN 102500299A CN 2011103754859 A CN2011103754859 A CN 2011103754859A CN 201110375485 A CN201110375485 A CN 201110375485A CN 102500299 A CN102500299 A CN 102500299A
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- magnesium hydroxide
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical class [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000000227 grinding Methods 0.000 claims abstract description 30
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 28
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 23
- 238000012986 modification Methods 0.000 claims abstract description 17
- 230000004048 modification Effects 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000011324 bead Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000003607 modifier Substances 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000011049 filling Methods 0.000 abstract 2
- 238000004537 pulping Methods 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000003063 flame retardant Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 10
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 235000019504 cigarettes Nutrition 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000009527 percussion Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a preparation method for nanoscale modified magnesium hydroxide and aims to provide a preparation method for superfine magnesium hydroxide. By the preparation method, the yield is high; the technical process is short; no pollution exists in the production process; the grain size is distributed narrowly; and ultrafining and surface modification can be finished at one step. The preparation method is implemented by the following technical scheme: mixing, stirring and pulping 1,000 weight parts of magnesium hydroxide powder with the grain size of 325 to 8,000 meshes, 1 to 80 weight parts of surfactant and 1,000 to 5,000 weight parts of solvent; filling the pulp into a grinding cavity by using spherical medium grinding beads with the diameter of less than or equal to 0.8 mm and grinding the pulp by using the pulp grinding equipment under the conditions that the filling volume is more than 35 percent and the minimum speed of the grinding beams is more than 10 meters per second; and drying the pulp subjected to grinding by using drying equipment under the drying condition of 40 to 320 DEG C to obtain the ultrafine magnesium hydroxide powder with the average grain size of 50 to 500 nanometers and the modified surface.
Description
Technical field
The invention relates to the preparation method of nano level modified magnesium hydroxide, more particularly the invention relates to and to be mainly used in flame retardant area, the preparation method of the nano level modified super fine magnesium hydroxide of surface modification.
Background technology
The magnesium hydrate powder material as inorganic, press down cigarette, nontoxic fire proofing, in the high molecular polymer flame retardant area, be widely used.Magnesium hydroxide has high thermal stability, high caloric receptivity, excellent cigarette ability, the soft of pressing down with it with respect to the aluminium hydroxide flame-retardant material that is widely used; Be considered to the most rising environmentally friendly inorganic combustion inhibitor, become the focus of various countries' research in recent years.
The fast development of nanoscale science and technology, from theory, preparation technology and relevant device aspects such as (comprising analytical and testing instrument), all the ultra-fineization research to flame retardant of magnesium hydroxide has produced great promotion.Utilize ultra fine, the processing method that combines of ultra-fineization and surface treatment especially can be improved the compatibility of flame retardant of magnesium hydroxide and polymer substrate significantly, can obviously improve magnesium hydroxide flame retardant material mechanical performance and processing characteristics.In addition; The fire retardant nanometerization helps to give full play to its fire resistance; As the polymeric material that is added with nano-meter flame retardants is carried out combustion testing, can know that the expanded foam charcoal layer of the polymeric material formation of adding nano-sized magnesium hydroxide (comparing with conventional flame retardant) is fine and closely woven, have high density and high strength.This is because the nano-meter flame retardants size is tiny, specific area is big; Particle evenly disperses in polymer; But nano-sized magnesium hydroxide particle thermally equivalent everywhere in the fire-retardant process, exploded causes polymeric material to become charcoal inhomogeneous with to become charcoal of poor quality when having avoided particle big.
Strengthen the preparation research of nano-sized magnesium hydroxide, promote the production of China's flame retardant of magnesium hydroxide and development to become the inorganic combustion inhibitor hot research fields.In recent years; Units such as Beijing Institute of Technology, Chinese University of Science and Technology, Tsing-Hua University, Beijing University of Chemical Technology are studied the preparation technology and the application of nano-magnesium hydrate fire retardant in succession, and the method for employing mainly contains metal magnesium hydration method, direct precipitation method, sluggish precipitation, deposition-azeotropic distillation method, overweight force method etc.
Metal magnesium hydration legal system magnesium hydroxide has two kinds of technologies, and its requirement to raw material and equipment is high especially, and product purity is high, but cost is also high, and productive rate is low, the difficult suitability for industrialized production that realizes.
The natural brucite that the selection of shepardite pulverizing method is pure relatively etc. is a raw material, and in the presence of grinding aid, warp stirs the mill wet grinding, the level branch, and surface treatment, acquisition reaches the superfine powder of re-set target.But, this preparation method height that consumes energy, the size of particle general 0.7-3 μ m or bigger, yardstick and distribution of shapes are wide, and it is low to reach product quality.
When direct precipitation method uses NaOH as precipitating reagent, severe reaction conditions, wayward; When using NH3-H2O or NH3, be prone to contaminated environment as precipitating reagent; When being deposition with Ca (OH) 2, product purity is low, and the accessory substance calcium salt is hard to manage.
The characteristics of deposition-hydro-thermal method are that product gas purity is high, and particle diameter and form are evenly distributed, but particle diameter is bigger, generally at 0.5～5 μ m, needs high-temperature high-pressure apparatus, intermittent operation.
High shear emulsifying reactor is similar with colloid mill, and the microcosmic of in fact being unrealized evenly mixes, and the product particle diameter distributes wide.
Full back-mixing liquid film reactor comes down to precipitating-the hydro-thermal method operation, the long-time back-mixing of reactant, operate tediously long, the production cost height.
The hypergravity legal system is equipped with nano-sized magnesium hydroxide and has obtained success, has realized industrial-scale production.But, in brin, liquid film, three kinds of different reaction environments of drop, carry out precipitation reaction, it is inhomogeneous to be doomed the particle diameter and the form of products therefrom; Packed bed might be stopped up by magnesium hydrate precipitate.
The percussion flow method adopts injecting type percussion flow reaction crystalizer.Reactor is from the molecular beam reactor in this, and when magnesium salt solution and alkali lye injection stream are big, will reach microcosmic and mix, with the particle diameter that product occurs and form skewness, difficult realization industrial-scale production.
With spin disk reactor synthesis of nano magnesium hydroxide, again through roasting oxygenerating magnesium.Owing on the spin disk, lack, so the uniformity of particle diameter and form distribution is affected with two kinds of uniform mechanisms of reactant liquor rapid mixing.
These methods all exist problems such as technical process is tediously long, cost is high, and productive rate is low, difficulty realizes industrial-scale production, and particle diameter is big and distribution of shapes is wide, product quality is low, and the production process environmental pollution is serious respectively.
Summary of the invention
The objective of the invention is the weak point that exists to prior art, provide a kind of manufacturing productive rate high, technical process is short, and production process is pollution-free, and narrow diameter distribution can be accomplished the preparation method of ultra-fineization and the super fine magnesium hydroxide of surface modification a step.
Above-mentioned purpose of the present invention can reach through following measure: a kind of preparation method of nano level modified magnesium hydroxide is characterized in that comprising the steps:
With magnesium hydrate powder, surface modifier and the solvent of 325～8000 order particle diameters is that 1000: 1～80: 1000～5000 (weight portions) mix, stirring to pulp in proportion, then, above-mentioned slurry is passed through milling apparatus; Spherical medium grinding bead with diameter≤0.8mm; Be filled in and grind in the cavity, than greater than 35%, grind under the environment of minimum movement velocity greater than 10 meter per seconds of grinding bead at packing volume; The slurry that more above-mentioned grinding is obtained; Through drying equipment, under 40 ℃～320 ℃ drying conditions, carry out drying, obtain the ultra-fineization magnesium hydrate powder of average particle size distribution in the process modification of the surface of 50～500 nanometers.
The present invention has following beneficial effect than prior art.
The present invention adopts magnesium hydrate powder and surface modifier and solvent, grinding by a certain percentage; Be different under the process conditions of prior art, with thick magnesium hydrate powder through ultra-fineization, surface modifier, the dry super fine magnesium hydroxide powder that obtains through surface modification under the uniform temperature condition.Accomplish ultra-fineization and the surface modification of magnesium hydrate powder with short technological process, a step; Prior art metal magnesium hydration method, direct precipitation method, sluggish precipitation, deposition-azeotropic distillation method, overweight force method have been solved; Dry method, technical process is tediously long, cost is high, low, the difficult industrial-scale production that realizes of productive rate; Problems such as the particle diameter distribution is wide, product quality is low, and the production process environmental pollution is serious.
The present invention adopts the efficient nano level to grind; Combining nano magnesium hydroxide surface modifying technology; Magnesium hydroxide superfining process and surface modification technology are combined into a step; Both reduced processing step, reduced cost, also improved the quality of products such as degree of modification, particle diameter distribution width simultaneously, the scale volume production of nanoscale surface modification magnesium hydroxide is become a reality.With simple process equipment, the process conditions that realize easily, realized that the technology cost is low, product cut size narrowly distributing, production process be environment friendly and pollution-free, a step is accomplished the surface modification of magnesium hydrate powder and ultra-fineization of magnesium hydrate powder.Be scale cheaply, the high-quality ultra-fineization nano-sized magnesium hydroxide powder of commercial production provides technological shortcut.
The specific embodiment
Be described in detail specific embodiment of the present invention below in conjunction with technical scheme.
In following examples, the technological process of preparation can be as follows:
Step 1: with magnesium hydrate powder by a certain percentage with surface modifier, solvent, stir into slurry; The particle diameter of magnesium hydrate powder usually can be in 325～8000 order scopes; Surface modifier can be a kind of in the pure dilution, long chain organic acid of silane coupler; Solvent is one or more in the alcohol below water, the C1～C4; The ratio of magnesium hydroxide, surface modifier and solvent is 1000: (1～80): (1000～5000); The process conditions of grinding are: abrasive media can adopt spherical ceramic grinding bead, zirconia ball, the spherical metal grinding bead of diameter less than 0.8mm, such as grinding bead such as stainless steel, titanium alloys;
Step 2: the packing volume of slurry that step 1 is obtained grinding bead in having filled the spherical ceramic grinding bead of diameter less than 0.8mm, grinding chamber is than in greater than 35% milling apparatus, and material grinds under 40 ℃～90 ℃, the condition of minimum movement velocity greater than 10 meter per seconds of grinding bead in grinding cavity.
Step 3: with the slurry that step 2 obtains, use drying equipment under 40 ℃～320 ℃ drying conditions, to carry out drying, can obtain the magnesium hydrate powder of average particle size distribution in the process modification of the surface of 50～500 nanometers.Drying equipment can be one or both in spray drying device, flash drying equipment, pneumatic conveying dryer, the trifling drying equipment.
Embodiment 1
According to said method, get 10 kilograms of the commercially available magnesium hydrate powders of 325 orders, mix, stir into slurry with 3-triethoxysilyl-1-propylamine, 20 kilograms of deionized waters of 800 grams, 30% concentration with the ethanol dilution.And the horizontal sand mill that this slurry is flow through repeatedly the 3L cavity capacity of having filled 4.5 kilograms of
alumina balls grinds by 2000 rev/mins rotating speed, and temperature of charge is controlled in 40 ℃～45 ℃ scopes during grinding.Grind after 5 hours, get slurry in 80 ℃ baking oven dry 48 hours, can obtain the magnesium hydroxide of ultra-fineization, modification, its average grain diameter is 421 nanometers.
Embodiment 2
According to said method, get 5 kilograms of the commercially available magnesium hydrate powders of 800 orders, with 200 the gram 50% concentration with ethanol by the dilution 3-triethoxysilyl-1-propylamine, 7 kilograms of deionized waters mix, stir into slurry.And the horizontal sand mill that this slurry is flow through repeatedly the 3L cavity capacity of having filled 5 kilograms of
zirconia balls grinds by 3000 rev/mins rotating speed, and temperature of charge is controlled at 60～65 ℃ during grinding.Grind after 3 hours, get slurry in 110 ℃ baking oven dry 36 hours, can obtain the magnesium hydroxide of ultra-fineization, modification, its average grain diameter is 260 nanometers.
Embodiment 3
According to said method, get commercially available magnesium hydrate powder 500 grams of 2500 orders, mix, stir into slurry with 17.5 gram stearic acid, 1200 gram ethanol.And the test that this slurry flows through the 0.6L cavity capacity of having filled 1.2 kilograms of
zirconium oxide abrasive balls repeatedly ground with the rotating speed of sand mill by 3600 rev/mins, temperature of charge is controlled at 30 ℃～35 ℃ during grinding.Grind after 10 hours, get slurry with vacuum microwave drier 46 ℃ of dryings, can obtain the magnesium hydroxide of ultra-fineization, modification, its average grain diameter is 61 nanometers.
Embodiment 4
According to said method, get 10 kilograms of the commercially available magnesium hydrate powders of 3000 orders, with 800 the gram 30% concentration with ethanol by the dilution γ-methacryloxypropyl trimethoxy silane, 20 kilograms of deionized waters mix, stir into slurry.And the horizontal sand mill that this slurry flows through the 30L cavity capacity of having filled 55 kilograms of
alumina balls repeatedly ground by 2000 rev/mins; Temperature of charge is controlled at 40 ℃～45 ℃ during grinding, grinds after 5 hours.Under 60 ℃～65 ℃ temperature of charge condition, grind after 2 hours afterwards, get slurry in 80 ℃ baking oven dry 48 hours, can obtain the magnesium hydroxide of ultra-fineization, modification, its average grain diameter is 421 nanometers.
Embodiment 5
According to said method, get 1000 kilograms of the commercially available magnesium hydrate powders of 1500 orders, mix, stir into slurry with N-(β one aminoethyl)-γ-aminopropyl front three (second) TMOS, 2000 kilograms of deionized waters of 10 kilogram of 20% concentration with the ethanol dilution.And the horizontal sand mill that this slurry flows through the 30L cavity capacity of having filled 50 kilograms of
zirconia balls repeatedly ground by 2500 rev/mins, temperature of charge is controlled at 80 ℃～85 ℃ during grinding.Grind after 18 hours, it is dry with spray drying device to get slurry, can obtain the magnesium hydroxide of ultra-fineization, modification, and its average grain diameter is 73 nanometers.
Claims (5)
1. the preparation method of a nano level modified magnesium hydroxide is characterized in that comprising the steps:
With magnesium hydrate powder, surface modifier and the solvent of 325～8000 order particle diameters is that 1000: 1～80: 1000～5000 (weight portions) mix, stirring to pulp in proportion, then, above-mentioned slurry is passed through milling apparatus; Spherical medium grinding bead with diameter≤0.8mm; Be filled in and grind in the cavity, than greater than 35%, grind under the environment of minimum movement velocity greater than 10 meter per seconds of grinding bead at packing volume; The slurry that more above-mentioned grinding is obtained; Through drying equipment, under 40 ℃～320 ℃ drying conditions, carry out drying, obtain the ultra-fineization magnesium hydrate powder of average particle size distribution in the process modification of the surface of 50～500 nanometers.
2. the preparation method of nano level modified magnesium hydroxide as claimed in claim 1 is characterized in that, described surface modifier is a kind of in the pure dilution, long chain organic acid of silane coupler.
3. the preparation method of nano level modified magnesium hydroxide as claimed in claim 1 is characterized in that, described solvent is one or more in the alcohol of deionized water, C1～C4.
4. the preparation method of nano level modified magnesium hydroxide as claimed in claim 1 is characterized in that, described abrasive media is a kind of in the spherical ceramic grinding bead.
5. the preparation method of nano level modified magnesium hydroxide as claimed in claim 1 is characterized in that, the magnesium hydroxide temperature of charge is controlled in 40 ℃～90 ℃ scopes during grinding.
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| CN201110375485.9A CN102500299B (en) | 2011-11-23 | 2011-11-23 | Preparation method for nanoscale modified magnesium hydroxide |
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Cited By (6)
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| CN107056151A (en) * | 2017-03-03 | 2017-08-18 | 筑成联合资产管理有限公司 | A kind of fire-proof plate |
| CN108285552A (en) * | 2017-12-27 | 2018-07-17 | 江苏艾特克阻燃材料有限公司 | A kind of modified magnesium hydroxide, method of modifying and application |
| CN110229516A (en) * | 2019-07-10 | 2019-09-13 | 西北师范大学 | A kind of preparation method of the intrinsic fire-retardant Nylon 66 composite material of low smoke, zero halogen |
| CN110342552A (en) * | 2019-08-16 | 2019-10-18 | 大连环球矿产股份有限公司 | A kind of method that chemical method prepares active micron/nanometer flame retardant of magnesium hydroxide |
| CN114538485A (en) * | 2022-02-25 | 2022-05-27 | 安徽大学绿色产业创新研究院 | Method for preparing flame retardant magnesium hydroxide by taking industrial-grade magnesium hydroxide as raw material |
| CN115780035A (en) * | 2022-11-25 | 2023-03-14 | 大连亚泰科技新材料股份有限公司 | Horizontal wet ball mill with heating system and pressure control system and method for producing hexagonal flaky magnesium hydroxide by using same |
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| CN101368009A (en) * | 2007-12-12 | 2009-02-18 | 清华大学深圳研究生院 | Modification method of nano-magnesium hydroxide |
| CN101544388A (en) * | 2008-03-26 | 2009-09-30 | 南京理工大学 | Method for preparing modified sheeted nanometer magnesium hydroxide |
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| CN101058429A (en) * | 2006-04-22 | 2007-10-24 | 朱晓林 | Method of preparing magnesium hydroxide superfine powder |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107056151A (en) * | 2017-03-03 | 2017-08-18 | 筑成联合资产管理有限公司 | A kind of fire-proof plate |
| CN108285552A (en) * | 2017-12-27 | 2018-07-17 | 江苏艾特克阻燃材料有限公司 | A kind of modified magnesium hydroxide, method of modifying and application |
| CN110229516A (en) * | 2019-07-10 | 2019-09-13 | 西北师范大学 | A kind of preparation method of the intrinsic fire-retardant Nylon 66 composite material of low smoke, zero halogen |
| CN110342552A (en) * | 2019-08-16 | 2019-10-18 | 大连环球矿产股份有限公司 | A kind of method that chemical method prepares active micron/nanometer flame retardant of magnesium hydroxide |
| CN110342552B (en) * | 2019-08-16 | 2021-12-10 | 大连环球矿产股份有限公司 | Method for preparing active micro-nano magnesium hydroxide flame retardant by chemical method |
| CN114538485A (en) * | 2022-02-25 | 2022-05-27 | 安徽大学绿色产业创新研究院 | Method for preparing flame retardant magnesium hydroxide by taking industrial-grade magnesium hydroxide as raw material |
| CN114538485B (en) * | 2022-02-25 | 2023-09-15 | 安徽大学绿色产业创新研究院 | Method for preparing flame retardant magnesium hydroxide by taking industrial magnesium hydroxide as raw material |
| CN115780035A (en) * | 2022-11-25 | 2023-03-14 | 大连亚泰科技新材料股份有限公司 | Horizontal wet ball mill with heating system and pressure control system and method for producing hexagonal flaky magnesium hydroxide by using same |
| CN115780035B (en) * | 2022-11-25 | 2023-09-29 | 大连亚泰科技新材料股份有限公司 | Horizontal wet ball mill with heating system and pressure control system and method for producing hexagonal flaky magnesium hydroxide by using horizontal wet ball mill |
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