CN114956135A - Method for preparing nano magnesium hydroxide flame retardant through high shear force - Google Patents
Method for preparing nano magnesium hydroxide flame retardant through high shear force Download PDFInfo
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- CN114956135A CN114956135A CN202210530412.0A CN202210530412A CN114956135A CN 114956135 A CN114956135 A CN 114956135A CN 202210530412 A CN202210530412 A CN 202210530412A CN 114956135 A CN114956135 A CN 114956135A
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- magnesium
- high shear
- flame retardant
- magnesium hydroxide
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 35
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 35
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000003063 flame retardant Substances 0.000 title claims abstract description 27
- 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 title claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 63
- 239000011777 magnesium Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000012716 precipitator Substances 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 9
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 abstract description 7
- 238000010008 shearing Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 22
- 159000000003 magnesium salts Chemical class 0.000 description 7
- 229940091250 magnesium supplement Drugs 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000012267 brine Substances 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229960002337 magnesium chloride Drugs 0.000 description 3
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 description 3
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241001131796 Botaurus stellaris Species 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 1
- 239000003830 anthracite Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229960003390 magnesium sulfate Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
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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
-
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/028—Compounds containing only magnesium as metal
-
- 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
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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
- C01P2004/01—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
- C01P2004/30—Particle morphology extending in three dimensions
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a method for preparing a nano magnesium hydroxide flame retardant by high shearing force, which comprises the following steps: step 1, adopting a magnesium-containing solution as a raw material and adopting a sodium hydroxide solution as a precipitator; step 2, adding a magnesium-containing solution into the high-shear reactor, adding a sodium hydroxide solution into the high-shear reactor, and performing precipitation reaction to obtain slurry; step 3, carrying out hydrothermal reaction on the slurry obtained in the step 2; and 4, filtering the product obtained after the hydrothermal reaction in the step 3 to obtain the nano-scale magnesium hydroxide flame retardant. The method has the advantages of simple process, easy operation, no need of additives, cheap and easily-obtained raw materials, low production cost and easy industrial production.
Description
Technical Field
The invention relates to the field of preparation methods of magnesium hydroxide flame retardants, in particular to a method for preparing a nano magnesium hydroxide flame retardant through high shear force.
Background
Magnesium hydroxide, as an inorganic material, has the characteristics of no toxicity, no odor, no corrosiveness, high decomposition temperature and the like, and has very important application in the fields of flame retardance, environmental protection, medical use, food, ceramics, cosmetics and the like. The advantages of magnesium hydroxide as an inorganic flame retardant are particularly prominent with the increasing demand for halogen-free flame retardants in recent years. The preparation method of the magnesium hydroxide mainly comprises the following steps: 1. brine lime method: is prepared by reacting bittern with slaked lime. 2. Brine ammonia water method: taking brine which is subjected to purification treatment to remove impurities such as sulfate, carbon dioxide, a small amount of boron and the like as a raw material, and taking ammonia water as a precipitator to perform precipitation reaction in a reaction kettle to obtain a finished product of magnesium hydroxide; 3. magnesia ammonia hydrochloride method: the magnesite and anthracite or coke are calcined to generate magnesium oxide and carbon dioxide, the magnesium oxide and the carbon dioxide are reacted with hydrochloric acid with specified concentration after calcination to prepare magnesium chloride solution, and the magnesium chloride solution and ammonia water with certain concentration are reacted in a reactor to obtain a magnesium hydroxide product.
The high shearing force is that under the action of centrifugal force generated by the rotor rotating at high speed, materials are sucked into the working cavity from the upper feeding area and the lower feeding area of the working head and from the axial direction. Powerful centrifugal force throws the material from radially getting into between the stator, the narrow accurate clearance of rotor, receives comprehensive effort such as centrifugal extrusion, liquid layer friction, hydraulic impact simultaneously, and the material is by preliminary dispersion.
The high-concentration magnesium salt reacts with sodium hydroxide to prepare magnesium hydroxide, and because colloid is easy to generate and the viscosity is high, agglomeration can be caused, and the particle size is large. When the conventional stirring equipment is in a low rotating speed, the prepared magnesium hydroxide has too large particle diameter due to large viscosity and insufficient stirring, and cannot be used as a flame retardant, and when the rotating speed is too large, reactants splash and cannot react. Therefore, the preparation of magnesium hydroxide from magnesium salt and sodium hydroxide requires a device with high stirring speed and less splashing. The high shear reactor can satisfy the above requirements because it contains a stator and a rotor.
Disclosure of Invention
The invention aims to provide a method for preparing a nano magnesium hydroxide flame retardant by high shear force, which aims to solve the problem that magnesium hydroxide prepared by magnesium salt and sodium hydroxide in the prior art cannot be used as a flame retardant.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a nano magnesium hydroxide flame retardant by high shear force comprises the following steps:
step 1, adopting a magnesium-containing solution as a raw material and adopting a sodium hydroxide solution as a precipitator;
step 3, carrying out hydrothermal reaction on the slurry obtained in the step 2;
and 4, filtering the product obtained after the hydrothermal reaction in the step 3 to obtain a filter cake, and drying the filter cake to obtain the nano-scale magnesium hydroxide flame retardant.
In a further step 1, the ratio of the amount of the substance of the sodium hydroxide solution to the amount of the substance of the magnesium-containing solution is n (Mg) 2+ )：n(OH - )=1:2-1:2.4。
In the further step 1, the concentration of magnesium in the magnesium-containing solution is 3-4 mol/L.
Further, in the step 1, the magnesium-containing solution is any one or more of magnesium chloride, magnesium sulfate and magnesium nitrate.
In the further step 1, the concentration of the sodium hydroxide solution is 2-8 mol/L.
In the further step 3, the temperature of the hydrothermal reaction is 140-180 ℃ and the time is 4-8 h.
Further, the drying temperature in the step 4 is 80-110 ℃, and the drying time is 5-10 h.
The preparation method of the nanoscale magnesium hydroxide flame retardant comprises the following reaction equation through a precipitation reaction between a magnesium-containing solution and sodium hydroxide:
the nanometer magnesium hydroxide fire retardant prepared by the invention is hexagonal, and the grain diameter D50 is 0.3-1 μm.
The invention provides a method for preparing magnesium hydroxide by high shearing force, which effectively solves the problem that the traditional stirring device cannot meet the problem that the viscosity generated by the reaction of magnesium salt and sodium hydroxide is high due to high concentration.
The method has the advantages that the magnesium hydroxide is prepared by using high-concentration strong base and magnesium salt, the nucleation is rapidly carried out by using high shearing force, and the crystal growth is carried out by hydrothermal reaction, so that the problem of slow filtration is solved, and the problem of secondary agglomeration of the magnesium hydroxide prepared by using sodium hydroxide and magnesium salt is also solved, wherein the secondary particle size D50 of the magnesium hydroxide prepared by the method is 0.3-1 mu m, and the particle size distribution range is narrow.
Compared with the prior art, the invention has the advantages that: the precipitation reaction of the magnesium salt and the sodium hydroxide is carried out at room temperature, so the energy consumption is low.
The method has the advantages of simple process, easy operation, no need of additives, cheap and easily-obtained raw materials, low production cost and easy industrial production.
Drawings
FIG. 1 is an X-ray diffraction pattern of the product of example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of a product of example 1 of the present invention.
FIG. 3 is an X-ray diffraction pattern of the product of example 2 of the present invention.
FIG. 4 is a scanning electron micrograph of a product of example 2 of the present invention.
FIG. 5 is an X-ray diffraction pattern of the product of example 3 of the present invention.
FIG. 6 is a scanning electron micrograph of a product according to example 3 of the present invention.
FIG. 7 is a graph showing the particle size distribution in examples 1, 2 and 3 of the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Example 1
The process of this embodiment is as follows:
1. 375ml of magnesium chloride hexahydrate is measured at 4mol/L and added into the high shear reactor as a base solution, the rotating speed of the high shear reactor is adjusted to 2000r/min, and 1100ml of 3mol/L sodium hydroxide solution is gradually added into the high shear reactor through a pump.
2. After the sodium hydroxide solution is added, the rotating speed of the high-shear reactor is adjusted to 3000r/min, and precipitation reaction is carried out for 30min at room temperature, so as to obtain slurry.
3. And transferring the slurry obtained in the step 2 into a high-pressure reaction kettle for hydrothermal reaction at 140 ℃ for 6 hours.
4. Naturally cooling the reaction kettle with the same pressure, filtering and washing the reaction product, drying the filter cake at 105 ℃ for 5h to obtain Mg (OH) with the purity of over 99.6 percent, the D50 of 0.4-1 mu m and the shape of regular hexagonal sheets 2 And (3) a flame retardant.
Example 2
The process of this embodiment is as follows:
1. 510ml of 4mol/L magnesium chloride hexahydrate is measured and added into a high shear reactor as a base solution, the rotating speed of the high shear reactor is adjusted to 2000r/min, and 900ml of 5mol/L sodium hydroxide solution is gradually added into the high shear reactor through a pump.
2. After the sodium hydroxide solution is added, the high shearing force rotating speed is adjusted to 4000r/min, and precipitation reaction is carried out for 30min at room temperature, so as to obtain slurry.
3. And transferring the slurry obtained in the step 2 into a high-pressure reaction kettle for hydrothermal reaction for 4 hours at 160 ℃.
4. Naturally cooling the reaction kettle, filtering and washing the reaction product, drying the filter cake at 105 deg.C for 5h to obtain the product with purity of over 99.4%, D50 of 0.3-0.8 μm and regular shape of sixAngular sheet-like Mg (OH) 2 And (3) a flame retardant.
Example 3
The process of this embodiment is as follows:
1. 375ml of magnesium chloride hexahydrate is measured at 4mol/L and added into the high shear reactor as a base solution, the rotating speed of the high shear reactor is adjusted to 2000r/min, and 1100ml of 3mol/L sodium hydroxide solution is gradually added into the high shear reactor through a pump.
2. After the sodium hydroxide solution is added, the high shearing force rotating speed is adjusted to 3000r/min, and precipitation reaction is carried out for 30min at room temperature, so as to obtain slurry.
3. And transferring the slurry obtained in the step 2 into a high-pressure reaction kettle to perform hydrothermal reaction for 6 hours at 160 ℃.
4. Naturally cooling the reaction kettle with the same pressure, filtering and washing the reaction product, drying the filter cake at 105 ℃ for 5h to obtain Mg (OH) with the purity of over 99.5 percent, the D50 of 0.4-1 mu m and the shape of regular hexagonal sheets 2 And (3) a flame retardant.
The X-ray diffraction pattern analysis in fig. 1, 3, 5 shows that the prepared sample is consistent with the standard card of magnesium hydroxide, indicating that the product obtained by the above method is consistent with the product of the present application.
As can be seen from the scanning electron micrographs at 8 ten thousand times magnification in fig. 2, 4 and 6, the morphology of the product is a regular hexagonal sheet shape, and the size is in the nanometer level, which indicates that the product obtained by the above method is consistent with the product of the present application.
The particle size distribution diagram in fig. 7 shows that the main distribution area of the particle size is below 1 μm, which indicates that the particle size of the product obtained by the above method is consistent with that of the product of the present invention, and is in nanometer level.
The embodiments of the present invention are described only for the preferred embodiments of the present invention, and not for the limitation of the concept and scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the design concept of the present invention shall fall into the protection scope of the present invention, and the technical content of the present invention which is claimed is fully set forth in the claims.
Claims (8)
1. A method for preparing a nano magnesium hydroxide flame retardant by high shear force is characterized by comprising the following steps:
step 1, adopting a magnesium-containing solution as a raw material and adopting a sodium hydroxide solution as a precipitator;
step 2, adding a magnesium-containing solution into the high shear reactor as a reaction bottom solution, adjusting the rotating speed of the high shear reactor to 1800-;
step 3, carrying out hydrothermal reaction on the slurry obtained in the step 2;
and 4, filtering the product obtained after the hydrothermal reaction in the step 3 to obtain a filter cake, and drying the filter cake to obtain the nano-scale magnesium hydroxide flame retardant.
2. The method for preparing nano magnesium hydroxide flame retardant with high shear force according to claim 1, wherein in the step 1, the ratio of the amount of the substance of the sodium hydroxide solution to the amount of the substance of the magnesium-containing solution is n (Mg) 2+ )：n(OH - )=1:2-1:2.4。
3. The method for preparing nano magnesium hydroxide flame retardant with high shear force according to claim 1, wherein the concentration of magnesium in the magnesium-containing solution in step 1 is 3-4 mol/L.
4. The method for preparing nano magnesium hydroxide flame retardant with high shear force according to claim 1 or 3, wherein the solution containing magnesium in step 1 is any one or more of magnesium chloride, magnesium sulfate and magnesium nitrate.
5. The method for preparing nano magnesium hydroxide fire retardant with high shear force according to claim 1, wherein the concentration of the sodium hydroxide solution in step 1 is 2-8 mol/L.
6. The method for preparing nano magnesium hydroxide fire retardant with high shear force as claimed in claim 1, wherein the hydrothermal reaction temperature in step 3 is 140-180 ℃ and the time is 4-8 h.
7. The method for preparing nano magnesium hydroxide flame retardant with high shear force according to claim 1, wherein the drying temperature in the step 4 is 80-110 ℃ and the drying time is 5-10 h.
8. The method for preparing nano magnesium hydroxide flame retardant with high shear force according to claim 1, wherein: the nano magnesium hydroxide flame retardant obtained in the step 4 is in a hexagonal sheet shape, and the particle size D50 is 0.3-1 μm.
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| CN202210530412.0A CN114956135A (en) | 2022-05-16 | 2022-05-16 | Method for preparing nano magnesium hydroxide flame retardant through high shear force |
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| CN202210530412.0A Pending CN114956135A (en) | 2022-05-16 | 2022-05-16 | Method for preparing nano magnesium hydroxide flame retardant through high shear force |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1542036A (en) * | 2003-11-04 | 2004-11-03 | 上海大学 | Method for manufacturing nanometer magnesium hydroxide fire retardant |
| CN102205980A (en) * | 2011-04-07 | 2011-10-05 | 中国科学院青海盐湖研究所 | Method for preparing monodisperse flaky magnesium hydroxide flame retardant |
| US20160264868A1 (en) * | 2013-10-29 | 2016-09-15 | Otkrytoe Aktsionernoe Obshchestvo "Kaustik" | Nanoparticles of flame retardant magnesium hydroxide and method of production the same |
| CN109926055A (en) * | 2017-12-16 | 2019-06-25 | 万华化学集团股份有限公司 | The method for preparing catalyst of hydrogenation of acetophenone alpha-phenyl ethyl alcohol and application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1542036A (en) * | 2003-11-04 | 2004-11-03 | 上海大学 | Method for manufacturing nanometer magnesium hydroxide fire retardant |
| CN102205980A (en) * | 2011-04-07 | 2011-10-05 | 中国科学院青海盐湖研究所 | Method for preparing monodisperse flaky magnesium hydroxide flame retardant |
| US20160264868A1 (en) * | 2013-10-29 | 2016-09-15 | Otkrytoe Aktsionernoe Obshchestvo "Kaustik" | Nanoparticles of flame retardant magnesium hydroxide and method of production the same |
| CN109926055A (en) * | 2017-12-16 | 2019-06-25 | 万华化学集团股份有限公司 | The method for preparing catalyst of hydrogenation of acetophenone alpha-phenyl ethyl alcohol and application |
Non-Patent Citations (1)
| Title |
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| 刘志启 等: "用水氯镁石制备单分散六角片状氢氧化镁", 材料科学与工艺, vol. 19, no. 4, pages 138 - 144 * |
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