CN115259185A - Method for preparing magnesium hydroxide flame retardant with regular structure by hydrothermal method - Google Patents
Method for preparing magnesium hydroxide flame retardant with regular structure by hydrothermal method Download PDFInfo
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- CN115259185A CN115259185A CN202210046690.9A CN202210046690A CN115259185A CN 115259185 A CN115259185 A CN 115259185A CN 202210046690 A CN202210046690 A CN 202210046690A CN 115259185 A CN115259185 A CN 115259185A
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 84
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 79
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 79
- 238000000034 method Methods 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 19
- 239000003063 flame retardant Substances 0.000 title claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000000725 suspension Substances 0.000 claims abstract description 15
- 230000001788 irregular Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract 2
- 239000000843 powder Substances 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical group [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 8
- 238000012986 modification Methods 0.000 abstract description 7
- 230000004048 modification Effects 0.000 abstract description 7
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000011268 mixed slurry Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 29
- 239000013078 crystal Substances 0.000 description 23
- 239000000047 product Substances 0.000 description 11
- 238000001816 cooling Methods 0.000 description 9
- 238000000227 grinding Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 238000001132 ultrasonic dispersion Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000002861 polymer material Substances 0.000 description 4
- -1 chemical engineering Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000004800 polyvinyl chloride Substances 0.000 description 3
- 229920000915 polyvinyl chloride Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010327 methods by industry Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000009333 tian-xian Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
- C01P2006/12—Surface area
-
- 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
-
- 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
The invention provides a method for preparing a magnesium hydroxide flame retardant with a regular structure by a hydrothermal method, which comprises the steps of mixing irregular magnesium hydroxide dispersion suspension and a sodium hydroxide aqueous solution with a certain concentration, adding the mixed slurry into a closed hydrothermal reaction kettle, stirring at a constant temperature of 120-200 ℃ for 2-4 hours to obtain a recrystallized magnesium hydroxide solution, standing for 1 hour, filtering, washing, drying and crushing a precipitate to obtain the magnesium hydroxide flame retardant with the regular structure. The method of the invention has the following beneficial effects: (1) The irregular magnesium hydroxide is hydrothermally modified into the magnesium hydroxide with a regular structure, so that the form of the magnesium hydroxide is improved, the technological process of modification is reduced, the production efficiency is improved, and the cost is reduced; (2) The hydrothermally modified magnesium hydroxide has a regular structure, good dispersibility and a small surface area; (3) The separation liquid is magnesium hydroxide, no impurities can be recycled, the production cost is reduced, no sewage is discharged, and the method is safe and environment-friendly.
Description
(I) technical field
The invention relates to a method for preparing a magnesium hydroxide flame retardant with a regular structure by a hydrothermal method
(II) background of the invention
With the wide application of high molecular polymer materials in the fields of construction, traffic, electricity and the like, in which a fire easily occurs under the conditions of high pressure, heat generation, electricity generation and the like, and a large amount of toxic gas and smoke are released during combustion, a large amount of casualties and huge property loss are caused, and these problems directly promote the development of the flame retardant market and the development of the research and development of magnesium hydroxide.
Magnesium hydroxide is widely used in various resins, such as PE, PP and the like, and is used as an excellent flame retardant and filler for high polymer materials such as plastics, rubber and the like in the industrial fields of chemical engineering, environmental protection and the like. The magnesium hydroxide is widely applied to high polymer materials such as rubber, chemical engineering, building materials, plastics (polypropylene, polyethylene, polyvinyl chloride and ethylene propylene diene monomer rubber), electronics, unsaturated polyester, paint, coating and the like, and is particularly applied to coating cloth for mining air ducts, PVC integral core conveyor belts, flame-retardant rubber plates, tarpaulins, PVC wire and cable materials and mining cable sheaths. The flame-retardant aluminum hydroxide is characterized by environmental protection, can replace aluminum hydroxide and has excellent flame-retardant effect.
Magnesium hydroxide has many advantages, but dispersion and compatibility problems during synthetic production are also important factors affecting product performance. The normally synthesized magnesium hydroxide suffers from the following problems: (1) The crystal structure is incomplete in growth, the surface polarity is poor, and the agglomeration is easy to happen; (2) The filtering is slow, the drying energy consumption is large, and secondary agglomeration is easy to occur in the drying process; (3) The particle size distribution is wide, the dispersion is poor, and the application performance is unstable; the above problems seriously affect the performance of magnesium hydroxide in the application of high polymer materials, and the problems of dispersion, particle size and the like seriously affect the application performance and the addition proportion under the condition of meeting the requirements of flame retardant grade and performance, thereby hindering the development of magnesium hydroxide.
The crystal grain formation of the magnesium hydroxide is divided into two aspects of crystal nucleation and production, the growth and nucleation speed of the commonly synthesized magnesium hydroxide crystal are inconsistent, and the appearance is irregular, so that the surface energy of the magnesium hydroxide is higher, the dispersion is not good, and the agglomeration is easy. The dispersibility and particle size distribution of the magnesium hydroxide are improved by external mechanical action such as supergravity, ultrasonic method/microwave method and the like, but the improvement of the surface energy of the particle size is limited, and the magnesium hydroxide flame retardant with excellent performance parameters needs to be obtained by further surface modification.
The hydrothermal modification is a process for reducing the surface energy of magnesium hydroxide, and can reduce the polarity of the surface of the magnesium hydroxide, ensure the uniform growth of a crystal structure and improve the structure and the powder dispersibility of the magnesium hydroxide. There are many relevant documents, such as:
(1) (1) hydrothermal modification of magnesium hydroxide in blue, gold-permanent, gold-surge, magnesium hydroxide solution [ J ] Process engineering Package, 2003 (02): 116-120.
(2) Zhao valia, magnesium hydroxide particle morphology control research [ D ] Hebei science university, 2011
(3) Dynasty emperor Mao Men, hei Tian Xian, gangtian Zhangin, etc. basic magnesium chloride or basic magnesium nitrate [ P ] Japanese patent No. Hei 2.204321,1990 08.
(4) Dynasty emperor Mao Men, hei Tianxian, gangtian Zhangong, etc. Synthesis of magnesium hydroxide having a novel structure [ P ] Japanese patent No. Hei 2.199019,1990 08.
(5) Dynasty emper county men, point blow ren, guang Rex-Shao-jin high-activity high-dispersion magnesium hydroxide and preparation method thereof [ P ] Japanese patent No. Hei 2.111625,1990 04.
(6) (method for producing magnesium hydroxide for Western Shang and Man [ P ] Japanese patent No. Sho 57.100918,1982 06 23.
(7) A method for producing magnesium hydroxide having a low specific surface area [ P ] according to the characterization, japanese patent No. Hei 2.164713, 1990 05.
(8) Influence of JinyongCheng, van, jinyong, solution composition on hydrothermal modification of magnesium hydroxide [ J ] lake salt and chemical, 2002,31 (1): 1.)
The problems of this method are: (1) high hydrothermal temperature, long time and high energy consumption; (2) the process is easy to cause environmental pollution; (3) The modifier is alkaline environment, has great corrosion to equipment and influences the safety problem; and (4) the process is long, the flow is complex, and the production efficiency is low.
Disclosure of the invention
The invention aims to provide a preparation method for producing a high-purity regular magnesium hydroxide flame retardant, which has the advantages of simplicity, low cost, simple process, high product purity and regular appearance.
The technical scheme of the invention is as follows: a process for the hydrothermal preparation of a regular magnesium hydroxide flame retardant, the process comprising:
(1) Mixing the irregular magnesium hydroxide dispersion suspension, sodium hydroxide solid and water, adding the mixture into a closed hydrothermal reaction kettle, and stirring at the constant temperature of 120-200 ℃ for 2-6 hours to obtain recrystallized magnesium hydroxide suspension, wherein the dosage ratio of the irregular magnesium hydroxide raw powder, the sodium hydroxide solid and the water is as follows: 150g-250g:240-960g:3L, 0.5 to 1 percent of dispersant by mass of magnesium hydroxide;
(2) And (2) standing the suspension obtained in the step (1) for 1 hour, and filtering and washing precipitates to obtain the regular magnesium hydroxide flame retardant.
The method is carried out under the conditions of constant temperature and constant pressure, the used equipment is a closed reaction kettle, and the temperature is controlled during operation.
The magnesium hydroxide is high-purity chemical method magnesium synthesized conventionally, the mesh number is larger than 5000 meshes, and the content is larger than 99%.
The sodium hydroxide and the sodium oxide are flaky solids with the content of more than 99 percent,
the dispersant is sodium oleate with the content of more than 99 percent.
The temperature of the reaction kettle in the step (2) is 120-200 ℃.
The filtration washing is a conventional method, and the filtration washing steps of the invention are as follows: after the hydrothermal modification, cooling, filtering to obtain filter pressing, washing to obtain distilled water, drying at 105 ℃, preferably selecting flash evaporation equipment, and crushing to obtain a millstone type crusher to obtain the magnesium hydroxide flame retardant
According to the invention, the high-purity and high-dispersion magnesium hydroxide is prepared, the crystal structure of the product is 1.5-2.5um, and the specific surface area is 8-14m2The purity is more than 99.2 percent, and the crystal is in a hexagonal plate structure.
The invention is best embodied in that: (1) The hydrothermal modification of magnesium hydroxide is completed in one step, so that the process flow is reduced, the cost is reduced, the filtering is quick, the time is short, and the energy consumption is reduced; (2) The recrystallized magnesium hydroxide has high crystallinity, regular appearance, uniform particle size, small specific surface area and good dispersion; (3) The production process is carried out in a closed reaction kettle, and after the production process is finished, the filtered and washed water can be continuously used without leakage, so that no environmental pollution is ensured, no sewage is discharged, and the cost and the environmental pollution are reduced.
Description of the drawings
FIG. 1 example one (120 ℃ C.) hydrothermally modifying the appearance of magnesium hydroxide particles;
FIG. 2 example two (150 ℃ C.) the appearance of the hydrothermally modified magnesium hydroxide particles;
FIG. 3 example III (180 ℃) hydrothermally modifies the appearance of magnesium hydroxide particles;
FIG. 4 example four (200 ℃ C.) hydrothermally modifying the appearance of magnesium hydroxide particles;
FIG. 5 example five (2 mol/L NaOH solution) hydrothermally modifying the appearance of magnesium hydroxide particles;
FIG. 6 example six (6 mol/L NaOH solution) hydrothermally modifying the appearance of magnesium hydroxide particles;
FIG. 7 example eight (2 h) appearance of hydrothermally modified magnesium hydroxide particles;
FIG. 8 example nine (6 h) appearance of hydrothermally modified magnesium hydroxide particles;
FIG. 9 XRD pattern of hydrothermally modified magnesium hydroxide of example four (200 ℃);
(V) detailed description of the preferred embodiments
The following further description of the present technology is provided in connection with specific embodiments, and the scope of the present invention is not limited to the following.
Example one
200g of magnesium hydroxide powder (5000 mesh) was wetted with 2L of water, and 2g of sodium oleate was added. Adding the components into an ultrasonic dispersion device together, preheating and dispersing for 1h at 80 ℃, adding the prepared dispersion suspension into a hydrothermal reaction kettle, adding 1L of water and 480g of sodium hydroxide, stirring and dissolving, stirring and heating to 120 ℃, keeping the temperature constant for 4 h, standing for 1h after constant-temperature stirring, cooling, separating, filtering, washing (distilled water), drying the obtained product at 105 ℃, and crushing and grinding to obtain white powder. The particle size and morphology of the sample are observed by a transmission electron microscope (SEM), and FIG. 1 shows that the magnesium hydroxide (with the magnification of 40 ten thousand times) prepared by the embodiment has a regular sheet structure, the purity is higher than 99%, the dispersibility is improved, the crystal particle size is mainly distributed between 300 and 1000nm, the thickness of the crystal is mainly distributed between 50 and 80nm, and the specific surface area is between 5 and 12m2And/g, the powder agglomeration phenomenon is low, and the bulk density is reduced.
Example two
200g of magnesium hydroxide powder (5000 mesh) was wetted with 2L of water, and 2g of sodium oleate was added. Adding into ultrasonic dispersion equipment, preheating at 80 deg.C for dispersing for 1 hr, adding the prepared dispersion suspension into hydrothermal reaction kettle, adding 1L water and 480g sodium hydroxide, stirring for dissolving, heating to 150 deg.C, keeping constant temperature for 4 hr, stirring at constant temperature, standingAfter standing for 1 hour, cooling, separating, filtering, washing (distilled water), drying the obtained product at 105 ℃, crushing and grinding to obtain white powder. The particle size and morphology of the sample are observed by a transmission electron microscope (SEM), and FIG. 2 shows that the magnesium hydroxide (with the magnification of 40 ten thousand times) prepared by the embodiment has a regular lamellar structure, is similar to a hexagonal plate structure, has the purity higher than 99 percent, improves the dispersibility, has the crystal particle size mainly distributed between 200 and 800nm, the thickness mainly distributed between 40 and 80nm and the specific surface area between 5 and 13m2And/g, the powder is not easy to agglomerate, and the bulk density is reduced.
EXAMPLE III
200g of magnesium hydroxide powder (5000 mesh) was wetted with 2L of water, and 2g of sodium oleate was added. Adding the components into an ultrasonic dispersion device together, preheating and dispersing for 1h at 80 ℃, adding the prepared dispersion suspension into a hydrothermal reaction kettle, adding 1L of water and 480g of sodium hydroxide, stirring and dissolving, stirring and heating to 180 ℃, keeping the temperature constant for 4 h, standing for 1h after constant-temperature stirring, cooling, separating, filtering, washing (distilled water), drying the obtained product at 105 ℃, and crushing and grinding to obtain white powder. The particle size and morphology of the sample are observed by a transmission electron microscope (SEM), and FIG. 3 shows that the magnesium hydroxide (with the magnification of 40 ten thousand times) prepared by the embodiment has a powder structure similar to a hexagonal plate structure, the purity of the magnesium hydroxide is higher than 99%, the dispersibility of the magnesium hydroxide is improved, the particle size of the crystal is mainly distributed between 200 nm and 600nm, the thickness of the crystal is mainly distributed between 40 nm and 80nm, and the specific surface area of the crystal is between 5 m and 12m2(g), powder is not easy to agglomerate, and the bulk density is reduced
Example four
200g of magnesium hydroxide powder (5000 mesh) was wetted with 2L of water, and 2g of sodium oleate was added. Adding the components into an ultrasonic dispersion device together, preheating and dispersing for 1h at 80 ℃, adding the prepared dispersion suspension into a hydrothermal reaction kettle, adding 1L of water and 480g of sodium hydroxide, stirring and dissolving, stirring and heating to 200 ℃, keeping the temperature constant for 4 h, standing for 1h after constant-temperature stirring, cooling, separating, filtering, washing (distilled water), drying the obtained product at 105 ℃, and crushing and grinding to obtain white powder. The particle size and morphology of the sample were observed by transmission electron microscopy (SEM), and FIG. 4 shows the magnesium hydroxide (magnified at a magnification of one embodiment) prepared in this example40 ten thousand times), and fig. 9 is a diffraction diagram of the X-ray powder of magnesium hydroxide prepared by the embodiment, the powder structure is similar to a hexagonal plate, the purity is higher than 99 percent, the appearance is regular, the dispersibility is good, the grain diameter of the crystal is mainly distributed between 200 nm and 600nm, the thickness of the crystal is mainly distributed between 40 nm and 60nm, and the specific surface area is between 6m and 12m2And/g, the powder is not easy to agglomerate and is easy to filter.
EXAMPLE five
200g of magnesium hydroxide powder (5000 mesh) was wetted with 2L of water, and 2g of sodium oleate was added. Adding the components into an ultrasonic dispersion device together, preheating and dispersing for 1h at 80 ℃, adding the prepared dispersion suspension into a hydrothermal reaction kettle, adding 1L of water and 240g of sodium hydroxide, stirring and dissolving, stirring and heating to 200 ℃, keeping the temperature constant for 4 h, standing for 1h after constant-temperature stirring is finished, cooling, separating, filtering, washing (distilled water), drying the obtained product at 105 ℃, and crushing and grinding to obtain white powder. The particle size and morphology of the sample are observed by a transmission electron microscope (SEM), and FIG. 5 shows that the magnesium hydroxide (with the magnification of 40 ten thousand times) prepared by the embodiment has a powder structure similar to a hexagonal plate, the purity is higher than 99%, the appearance is regular, the dispersibility is good, the crystal particle size is mainly distributed between 200 nm and 600nm, the thickness of the crystal is mainly distributed between 30 nm and 60nm, and the specific surface area is 5-12m2And/g, the powder is not easy to agglomerate and is easy to filter.
Example six
200g of magnesium hydroxide powder (5000 mesh) was wetted with 2L of water, and 2g of sodium oleate was added. Adding the components into an ultrasonic dispersion device together, preheating and dispersing for 1h at 80 ℃, adding the prepared dispersion suspension into a hydrothermal reaction kettle, adding 1L of water and 720g of sodium hydroxide, stirring and dissolving, stirring and heating to 200 ℃, keeping the temperature and stirring for 4 h, standing for 1h after the constant-temperature stirring is finished, cooling, separating, filtering, washing (distilled water), drying the obtained product at 105 ℃, and crushing and grinding to obtain white powder. The particle size and morphology of the sample are observed by a transmission electron microscope (SEM), and FIG. 6 shows that the magnesium hydroxide (with the magnification of 40 ten thousand times) prepared by the embodiment has a powder structure similar to a hexagonal plate, the purity is higher than 99%, the appearance is regular, the dispersibility is good, the crystal particle size is mainly distributed between 200 nm and 600nm, the thickness of the crystal is mainly distributed between 30 nm and 60nm, and the specific surface area is 5 m to 14m2And/g, the powder is not easy to agglomerate and is easy to filter.
EXAMPLE seven
200g of magnesium hydroxide powder (5000 mesh) was wetted with 2L of water, and 2g of sodium oleate was added. Adding the components into an ultrasonic dispersion device together, preheating and dispersing for 1h at 80 ℃, adding the prepared dispersion suspension into a hydrothermal reaction kettle, adding 1L of water and 480g of sodium hydroxide, stirring and dissolving, stirring and heating to 200 ℃, keeping the constant temperature and stirring for 2h, standing for 1h after the constant temperature stirring is finished, cooling, separating, filtering, washing (distilled water), drying the obtained product at 105 ℃, crushing and grinding to obtain white powder. The particle size and morphology of the sample are observed by a transmission electron microscope (SEM), and FIG. 7 shows that the magnesium hydroxide (with the magnification of 40 ten thousand times) prepared by the embodiment has a powder structure similar to a hexagonal plate, the purity is higher than 99%, the appearance is regular, the dispersibility is good, the crystal particle size is mainly distributed between 400 and 800nm, the thickness of the crystal is mainly distributed between 20 and 60nm, and the specific surface area is 6 to 12m2And/g, the powder is not easy to agglomerate and is easy to filter.
Example eight
200g of magnesium hydroxide powder (5000 mesh) was wetted with 2L of water, and 2g of sodium oleate was added. Adding the components into an ultrasonic dispersion device together, preheating and dispersing for 1h at 80 ℃, adding the prepared dispersion suspension into a hydrothermal reaction kettle, adding 1L of water and 480g of sodium hydroxide, stirring and dissolving, stirring and heating to 200 ℃, keeping the temperature constant for 6h, standing for 1h after constant-temperature stirring, cooling, separating, filtering, washing (distilled water), drying the obtained product at 105 ℃, and crushing and grinding to obtain white powder. The particle size and morphology of the sample are observed by a transmission electron microscope (SEM), and FIG. 8 shows that the magnesium hydroxide (with the magnification of 40 ten thousand times) prepared by the embodiment has a powder structure similar to a hexagonal plate, the purity is higher than 99%, the appearance is regular, the dispersibility is good, the crystal particle size is mainly distributed between 400 and 900nm, the thickness of the crystal is mainly distributed between 30 and 60nm, and the specific surface area is 5 to 12m2And/g, the powder is not easy to agglomerate and is easy to filter.
Claims (6)
1. A method of hydrothermally preparing a structurally regular magnesium hydroxide flame retardant, the method comprising:
(1) Mixing the irregular magnesium hydroxide dispersion suspension, sodium hydroxide solid and water, adding the mixture into a closed hydrothermal reaction kettle, and stirring at the constant temperature of 120-200 ℃ for 2-6 hours to obtain recrystallized magnesium hydroxide suspension, wherein the dosage ratio of the irregular magnesium hydroxide raw powder, the sodium hydroxide solid and the water is as follows: 150g-250g:240-960g:3L, wherein the dispersant accounts for 0.5-1% of the mass of the magnesium hydroxide;
(2) And (2) standing the suspension obtained in the step (1) for 1 hour, filtering, washing, drying and crushing the precipitate to obtain the regular magnesium hydroxide flame retardant.
2. The method of claim 1, wherein the irregular magnesium hydroxide is 5000 mesh prismatic magnesium hydroxide.
3. The method of claim 1 wherein the dispersant is sodium oleate, the purity being greater than 99%.
4. The method of claim 1, wherein the dispersing is ultrasonic dispersing during which a dispersing agent is added.
5. The method according to claim 1, wherein the filtration washing process comprises a step of filtering the mixture by a filter pressing device after separation by a hydrogen-oxygen standing method and a step of washing the mixture by distilled water.
6. The method of claim 1, wherein said drying, crushing to 105 ℃ drying, crushing equipment breaking up to obtain said magnesium hydroxide flame retardant with regular structure.
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| CN116835616A (en) * | 2023-08-30 | 2023-10-03 | 山东艾科高分子材料有限公司 | Method for preparing high-dispersion hexagonal flaky magnesium hydroxide by high-activity light-burned magnesium oxide through one-step hydrothermal method |
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| Title |
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| 李秋菊等: "水热介质对氢氧化镁晶体生长的影响", 《浙江工业大学学报》 * |
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| CN116835616A (en) * | 2023-08-30 | 2023-10-03 | 山东艾科高分子材料有限公司 | Method for preparing high-dispersion hexagonal flaky magnesium hydroxide by high-activity light-burned magnesium oxide through one-step hydrothermal method |
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