CN110980780A - Preparation method of flaky magnesium hydroxide flame retardant - Google Patents
Preparation method of flaky magnesium hydroxide flame retardant Download PDFInfo
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- CN110980780A CN110980780A CN201911331567.6A CN201911331567A CN110980780A CN 110980780 A CN110980780 A CN 110980780A CN 201911331567 A CN201911331567 A CN 201911331567A CN 110980780 A CN110980780 A CN 110980780A
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 49
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 49
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 49
- 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 35
- 239000003063 flame retardant Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 63
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 24
- 229920000428 triblock copolymer Polymers 0.000 claims abstract description 19
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 230000032683 aging Effects 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 12
- 239000012267 brine Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 238000011085 pressure filtration Methods 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 3
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- -1 hydroxide ions Chemical class 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- 159000000003 magnesium salts Chemical class 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000012066 reaction slurry Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
Images
Classifications
-
- 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
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a preparation method of a flaky magnesium hydroxide flame retardant, which comprises the following steps: putting a magnesium chloride solution into a reaction kettle, adding an amphoteric triblock copolymer crystal form directing agent, uniformly stirring, heating to 30-70 ℃ for the first time, dropwise adding sodium hydroxide into the reaction kettle at a constant speed under a stirring state, and keeping the temperature of 50-65 ℃ after dropwise adding is finished, stirring and reacting for 1 h; stopping stirring, heating to 70-90 ℃, carrying out normal-pressure hydrothermal aging reaction for 12-36h, and carrying out filter pressing, washing, drying and crushing to obtain the flaky magnesium hydroxide flame retardant; the crystal form directing agent is an amphiphilic triblock copolymer of polyethylene oxide and polypropylene oxide. In the invention, the sheet magnesium hydroxide flame retardant is prepared by one-step reaction at normal pressure and medium temperature by using the amphiphilic triblock copolymer of polyethylene oxide and polypropylene oxide as a crystallization guiding agent without replacing a reaction container.
Description
Technical Field
The invention relates to the technical field of chemical materials, and particularly belongs to a preparation method of a flaky magnesium hydroxide flame retardant.
Background
Magnesium hydroxide is a novel filling type flame retardant, releases combined water in the process of thermal decomposition, absorbs a large amount of latent heat, reduces the surface temperature of the filled material in flame, has the effects of inhibiting the decomposition of polymers and cooling the generated combustible gas, optimizes the fire resistance of the synthetic material, and has the effect of inhibiting smoke by the water vapor released by decomposition. Therefore, the magnesium hydroxide is a high-quality flame retardant with triple functions of smoke suppression, filling and flame retardance. In conclusion, the magnesium hydroxide has the characteristics of no toxicity, no harm, acid resistance and thermodynamic stability, has the advantages of heat absorption and smoke suppression functions when a polymer is combusted, and belongs to an environment-friendly flame retardant. The characteristics and advantages are derived from the crystal morphology, size and dispersity of the magnesium hydroxide crystal, and are the physical and chemical properties of the magnesium hydroxide crystal; the magnesium hydroxide crystal with the sheet structure has the filling, halogen-free and flame-retardant functions in thermoplastic polymers and fiber materials due to the special structure, mechanical property and dispersity, and can improve the combustion initial temperature of the polymer materials and enhance the thermal stability of the polymer materials. Therefore, the flaky magnesium hydroxide crystal flame retardant material becomes one of the hot spots of research in the field of flame retardants.
Chinese patent document CN102205980B discloses a preparation method of a monodisperse flaky magnesium hydroxide flame retardant, which comprises the following steps:
(1) preparing a soluble magnesium salt solution, wherein the concentration of magnesium ions is between 4mol/L and 0.5 mol/L;
(2) preparing an alkali solution, wherein the concentration of hydroxide ions is between 8 and 0.5 mol/L;
(3) under the conditions of normal pressure, reaction temperature of 25-60 ℃, stirring speed of 1500-;
(4) transferring the slurry into a high-pressure reaction kettle for hydrothermal reaction, wherein the water temperature is 100-;
(5) filtering, washing, and drying the washed product at the temperature of 100-160 ℃ for 4-6h to obtain the magnesium hydroxide flame retardant with the shape of hexagonal sheet or disk and the particle size of 200-500 nm.
The preparation process is divided into two steps of operation, wherein one step is carried out at normal pressure and the reaction temperature is 25-60 ℃; then the slurry is transferred to a high-pressure reaction kettle for hydrothermal reaction, and the water temperature is 100-200 ℃.
Chinese patent document CN106673027A discloses a preparation and synthesis method of hexagonal flaky magnesium hydroxide flame retardant, which comprises the following steps:
adding a magnesium salt solution and a crystallization guiding agent into a reaction container, uniformly stirring at 30-50 ℃, dropwise adding an inorganic alkali solution into the reaction container at a constant speed under the temperature condition, after the reaction is completed, carrying out ultrasonic oscillation on reaction slurry for 20-30min, transferring the reaction slurry into a high-pressure reaction kettle, adding anhydrous ethanol, carrying out hydrothermal reaction at the temperature of 150 ℃ and 220 ℃ for 12-72h, and finally carrying out filter pressing, washing and drying to obtain a magnesium hydroxide product.
The preparation process is divided into two steps of operation, and the reaction temperature of one step is 30-50 ℃; after ultrasonic oscillation, the mixture is transferred into a high-pressure reaction kettle for carrying out hydrothermal reaction at the temperature of 150-220 ℃.
The processes for preparing the magnesium hydroxide flame retardant are all carried out in a high-pressure reaction kettle, and the requirements on reaction conditions are high.
Disclosure of Invention
The preparation method of the flaky magnesium hydroxide flame retardant provided by the invention is used for achieving the purposes of reducing the process reaction conditions and adjusting the morphology of magnesium hydroxide in the preparation process.
A preparation method of a flaky magnesium hydroxide flame retardant is characterized by comprising the following steps:
putting the weighed magnesium chloride solution into a reaction kettle, adding the amphoteric triblock copolymer crystal form directing agent, uniformly stirring, heating to 30-70 ℃ for the first time, and stirring sodium hydroxideDropwise adding into the reaction kettle at a constant speed, and keeping the temperature of 50-65 ℃ after the dropwise adding is finished, stirring and reacting for 1 h; stopping stirring, heating to 70-90 ℃, carrying out normal-pressure hydrothermal aging reaction for 12-36h, and carrying out filter pressing, washing, drying and crushing to obtain the flaky magnesium hydroxide flame retardant; wherein the molar ratio of the magnesium chloride to the sodium hydroxide is nMagnesium chloride：nSodium hydroxide1: 2-4; the crystal form directing agent is an amphoteric triblock copolymer (EO) of polyethylene oxide and polypropylene oxidenPOmEOn)。
Preferably, the molar ratio of the magnesium chloride to the sodium hydroxide is nMagnesium chloride：nSodium hydroxide＝1:2.5。
Preferably, the magnesium chloride solution is obtained by refining underground brine after solar salt drying, or is obtained by dissolving solid magnesium chloride, and the concentration of the magnesium chloride in a reaction system is 0.5-3 mol/L; the concentration of the sodium hydroxide is 1-5 mol/L.
Preferably, the stirring speed of the sodium hydroxide during adding is 150-500 r/min.
Preferably, the concentration of magnesium chloride in the reaction system is 0.75 mol/L; the concentration of sodium hydroxide was 2.35 mol/L.
Preferably, the amphiphilic triblock copolymer is a triblock copolymer of polyethylene oxide and polypropylene oxide (EO)nPOmEOn) Wherein m isPolypropylene oxide70, the ratio of polyethylene oxide units to polypropylene oxide units nPolyethylene oxide：mPolypropylene oxide0.1-2.0; the concentration in the reaction system is 0.5-5.0 g/L.
Preferably, the amphiphilic triblock copolymer of polyethylene oxide and polypropylene oxide is EO106PO70EO106The concentration in the reaction system was 2.0 g/L.
Preferably, the first temperature rise temperature is 35 ℃; the hydrothermal aging reaction temperature is 80 ℃, and the time is 24 h.
The invention has the beneficial effects that:
in the invention, the amphoteric triblock copolymer (EO) of polyethylene oxide and polypropylene oxide is adoptednPOmEOn) The flaky magnesium hydroxide flame retardant is prepared by one-step reaction of a crystallization guiding agent at normal pressure and medium temperature, and a reaction container does not need to be replaced. By utilizing the oxygen affinity of magnesium ions, in the process of generating magnesium hydroxide, the amphoteric triblock copolymer is added as a crystal form directing agent to regulate the nucleation of magnesium hydroxide, control the growth of crystal forms and modify the surface of magnesium hydroxide crystals so as to prepare the magnesium hydroxide crystals with sheet structures.
The method has the advantages of convenient raw material source, low price, simple operation steps, short process flow, low energy consumption, less input equipment, avoidance of the use of a high-pressure reaction kettle, stable flaky shape of the prepared magnesium hydroxide, uniform particle size distribution and the like, and has good market application prospect.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of the magnesium hydroxide prepared in example 5 of the present invention as dispersed flaky crystals.
FIG. 2 is an X-ray diffraction (XRD) pattern of magnesium hydroxide prepared in example 2 of the present invention, which is substantially identical to the standard pattern JCPDS44-1482 of magnesium hydroxide.
FIG. 3 is a graph showing the distribution of the particle size distribution (abscissa unit is μm) of magnesium hydroxide prepared in example 5 of the present invention, the particle size distribution being uniform, and D50 being 1.88. mu.m.
FIG. 4 is a Scanning Electron Microscope (SEM) image of magnesium hydroxide in the prior art, which is irregular in shape and has agglomeration.
Detailed Description
The present invention will be further described with reference to specific examples, wherein the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A25L reactor was charged with 7.5L of a 1.5mol/L aqueous magnesium chloride solution, 22 g of an amphiphilic triblock copolymer of polyethylene oxide and polypropylene oxide (EO)20PO70EO20) Heating to 60 deg.c; the stirring speed is adjusted to 400 r/m, then 8 liters of sodium hydroxide solution with the concentration of 4mol/L is added by a constant flow pump, and the flow rate is controlled to be aboutThe temperature is 0.2 liter/minute, and the reaction is continued to be carried out for 1 hour at the temperature of 60 ℃ after the addition; heating to 90 ℃, stopping stirring and ageing for 12h, cooling to room temperature, then filtering, discharging, filtering by using a positive pressure filter, washing a filter cake for 3-5 times by using distilled water, taking the detection of no chloride ion in the filtrate as an end point, and placing the precipitate in a 105 ℃ oven for drying and crushing to obtain a magnesium hydroxide flame retardant product (marked as MH-1).
Example 2
A25 liter reaction vessel was charged with 10 liters of a 1.5mol/L magnesium chloride aqueous solution, and 9 g of an amphiphilic triblock copolymer of polyethylene oxide and polypropylene oxide (EO)45PO70EO45) Heating to 30 ℃; adjusting the stirring speed to 350 r/m, adding 8 liters of sodium hydroxide solution with the concentration of 4mol/L by a constant flow pump, controlling the flow rate to be about 0.2L/m, and continuing to perform heat preservation reaction at 50 ℃ for 1h after the addition is finished; heating to 70 ℃, stopping stirring and ageing for 30h, cooling to room temperature, then filtering, discharging, filtering by using a positive pressure filter, washing a filter cake for 3-5 times by using distilled water, taking the detection of no chloride ion in the filtrate as an end point, and placing the precipitate in a 105 ℃ oven for drying and crushing to obtain a magnesium hydroxide flame retardant product (marked as MH-2).
Example 3
A25 liter reaction vessel was charged with 7 liters of a 4mol/L magnesium chloride aqueous solution, and 50 g of an amphiphilic triblock copolymer of polyethylene oxide and polypropylene oxide (EO)60PO70EO60) Heating to 50 deg.c; adjusting the stirring speed to 150 r/m, adding 5 liters of sodium hydroxide solution with the concentration of 12mol/L by a constant flow pump, controlling the flow rate to be about 0.2 liter/m, and continuing to perform heat preservation reaction at 55 ℃ for 1h after the addition is finished; heating to 80 ℃, stopping stirring and ageing for 18h, cooling to room temperature, then filtering, discharging, filtering by using a positive pressure filter, washing a filter cake for 3-5 times by using distilled water, taking the detection of no chloride ion in the filtrate as an end point, and placing the precipitate in a 105 ℃ oven for drying and crushing to obtain a magnesium hydroxide flame retardant product (marked as MH-3).
Example 4
4 liters of a 3mol/L magnesium chloride aqueous solution was added to a 25 liter reaction vessel, and 35 g of polyethylene oxide and polyethylene oxide were addedAmphiphilic triblock copolymers of propane (EO)80PO70EO80) Heating to 70 deg.c; adjusting the stirring speed to 450 r/m, adding 6 liters of 6mol/L sodium hydroxide solution by a constant flow pump, controlling the flow rate to be about 0.2 liter/m, and continuing to perform heat preservation reaction at 60 ℃ for 1h after the addition is finished; heating to 75 ℃, stopping stirring and ageing for 36h, cooling to room temperature, then filtering, discharging, filtering by using a positive pressure filter, washing a filter cake for 3-5 times by using distilled water, taking the detection of no chloride ion in the filtrate as an end point, and placing the precipitate in a drying oven at 105 ℃ for drying and crushing to obtain a magnesium hydroxide flame retardant product (marked as MH-4).
Example 5
A25 liter reaction vessel was charged with 10 liters of a 1.5mol/L magnesium chloride aqueous solution, 2.5 liters of distilled water, 40 g of an amphoteric triblock copolymer of polyethylene oxide and polypropylene oxide (EO)106PO70EO106) Heating to 35 ℃; adjusting the stirring speed to 500r/m, adding 7.5 liters of sodium hydroxide solution with the concentration of 4mol/L by a constant flow pump, controlling the flow rate to be about 0.2 liter/m, and continuing to perform heat preservation reaction at 60 ℃ for 1 hour after the addition is finished; heating to 80 ℃, stopping stirring and ageing for 24 hours, cooling to room temperature, then filtering, discharging, filtering by using a positive pressure filter, washing a filter cake for 3-5 times by using distilled water, taking the detection of no chloride ion in the filtrate as an end point, and placing the precipitate in a 105 ℃ oven for drying and crushing to obtain a magnesium hydroxide flame retardant product (marked as MH-5).
The products obtained in examples 1 to 5 were subjected to the performance test, and the results of the test items are shown in Table 1 below
TABLE 1 magnesium hydroxide flame retardant product Properties
The performance tests in Table 1 show that the magnesium hydroxide flame retardant product prepared by the invention meets the MC-2-15 index requirements in the chemical industry standard HG/T4531-2013.
Claims (8)
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| CN108975360A (en) * | 2018-07-20 | 2018-12-11 | 大连理工大学 | A kind of preparation method, device and the application of spherical shape magnesia |
| CN109133126A (en) * | 2018-08-23 | 2019-01-04 | 中国科学院青海盐湖研究所 | A kind of magnesium hydroxide products and preparation method thereof |
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- 2019-12-21 CN CN201911331567.6A patent/CN110980780B/en active Active
Patent Citations (7)
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|---|---|---|---|---|
| CN1359853A (en) * | 2000-12-19 | 2002-07-24 | 中国科学技术大学 | Acidular or flaky nano magnesium hydroxide and its preparing process |
| CN101700899A (en) * | 2009-10-28 | 2010-05-05 | 钟辉 | Technology for producing and preparing high-purity lamellar magnesium hydroxide |
| CN104495883A (en) * | 2014-12-02 | 2015-04-08 | 中国科学院青海盐湖研究所 | Preparation method of magnesium hydrate with high-concentration slurry |
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