CN101269827A - Method for preparing high-dispersion magnesium hydroxide combustion inhibitor with one-step hydrothermal method - Google Patents
Method for preparing high-dispersion magnesium hydroxide combustion inhibitor with one-step hydrothermal method Download PDFInfo
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- CN101269827A CN101269827A CNA2008100609743A CN200810060974A CN101269827A CN 101269827 A CN101269827 A CN 101269827A CN A2008100609743 A CNA2008100609743 A CN A2008100609743A CN 200810060974 A CN200810060974 A CN 200810060974A CN 101269827 A CN101269827 A CN 101269827A
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Abstract
The invention provides a method using one-step hydrothermal method to prepare a magnesium hydroxide flame retardant. Magnesium chloride, ethanol and water are mixed to get mixture, and dispersant polyethyleneglycol is added into the mixture to get magnesium chloride mother liquid. Under the isothermal stirring of 40 to 200 DEG C, the magnesium chloride mother liquid is dropped into aqueous ammonia with 2 to 36 percent of concentration in a closed hydrothermal reaction vessel until the PH of reaction liquid is from 9 to 12, and dropping is stopped. After the isothermal stirring for 0.5 to 5 hours, the reaction liquid passes through purification to get the magnesium hydroxide flame retardant. The invention has the beneficial effects that (1) the synthesis of magnesium hydroxide and hydrothermal modification are finished in one step, which reduced the technological process, improves the production efficiency and reduces the energy consumption; (2) the synthetical magnesium hydroxide has the advantages of perfect crystallinity, low surface polarity and fast filtration, which are difficult to agglomerate; (3) the production process is carried out in the closed hydrothermal reaction vessel, the ammonia is fully utilized, and ammonia gas is not leaked, which reduces cost and does not have environmental pollution.
Description
(1) technical field
The present invention relates to the method that one step hydro thermal method prepares high-dispersion magnesium hydroxide combustion inhibitor.
(2) background technology
Along with macromolecular materials such as plastics, rubber, synthon constantly enter daily life, people require more and more higher to the flame retardant properties of these materials.Especially macromolecular material and electron device (as electric wire, cable) are worked under long-term heating, power generation conditions, easily initiation fire when being used in combination.Need to study effective fire retardant for this reason and solve inflammable, the easy problem such as be fuming of macromolecular material.Compare with other fire retardant (as halogen system, phosphorus system, aluminium hydroxide, ANTIMONY TRIOXIDE SB 203 99.8 PCT), magnesium hydroxide has flame-retardant smoke inhibition, thermostability height (decomposition temperature is at 340～490 ℃), characteristics such as nontoxic.During as weighting agent, can make plastics bear higher temperature, help accelerating extrusion molding speed, shorten molding cycle, especially be fit to be used with thermally stable polymers such as PP, PA, POM.
Though magnesium hydroxide has lot of advantages, the flame retardant of magnesium hydroxide of synthetic high dispersive is a very big difficult problem.Often there are the following problems for common process synthetic magnesium hydroxide: (1) crystal grain crystallization imperfection, and surface polarity is strong, easily gelation, washing and filtering is difficulty very, easy secondary agglomeration in the drying process; (2) size distribution is wide, bad dispersibility; (3) purity is low.Above problem causes magnesium hydroxide and macromolecular material consistency poor, and addition is big, and the mechanical property of material and resistance toheat are reduced.
Angle from microcosmic, the generation of magnesium hydroxide crystal grain comprises crystal nucleation and two steps of growth, common building-up process (precipitator method) crystal nucleation and the speed of growth are generally very fast, and system intermediate ion concentration distribution is inhomogeneous, thereby cause magnesium hydroxide crystal grain imperfection to cause particle inhomogeneous easily, make that the magnesium hydroxide surface energy is higher, easily reunite and filtration difficulty.Use overweight force method (Song Yunhua, old Jiang Ming, Liu Lihua etc. 19～23) and microwave method (Fang Yuxun high-gravity technology prepares the applied research of nano-magnesium hydrate fire retardant, chemical industry mineral and processing, 2004 (5):, He Renbin, Liu Yanhong. bittern-rhombspar microwave catalysis is produced magnesium hydroxide and magnesium oxide. inorganic chemicals industry, 35～37) etc. 2005,37 (2): technology is synthetic, though can improve the homogeneity of ion concentration distribution in the system, thereby improve the distribution of magnesium hydroxide particle diameter.But the method that is adopted be external mechanical energy to magnesium hydroxide generation effect, to grain surface can influence limited, also need follow-up surface modification.
Hydrothermal synthesis method is a kind of method that changes inherent energy field in the magnesium hydroxide building-up process, and it can change the magnesium hydroxide surface polarity, and improves the magnesium hydroxide crystal phase structure.Present bibliographical information (to orchid, Jin Yongcheng, gold gushes. the research of magnesium hydroxide crystal habit. Chinese Journal of Inorganic Chemistry, 2003,19 (8): 837～842; Chinese patent CN1740269) hydro-thermal synthetic technology is a two-step approach, at first by the synthetic magnesium hydroxide crystal grain of normal temperature, with hydrothermal method magnesium hydroxide grain morphology and surface polarity is carried out modification then.But there is following defective in this method: (1) hydrothermal temperature height, long flow path, cost height; (2) easily cause the environmental pollution of ammonia; (3) hydrothermal modification agent (as ammoniacal liquor, sodium hydroxide, urea) is big to equipment corrosion; (4) the hydrothermal modification effect is limited.
(3) summary of the invention
In order to overcome the above-mentioned shortcoming that present magnesium hydroxide hydrothermal modification technology exists, the invention provides the novel process that one step hydro thermal method prepares flame retardant of magnesium hydroxide.Not only technology is simple for this method, cost is low, but and magnesium hydroxide products purity height, scattered, pattern is regular and modulation.
The technical solution used in the present invention is:
One step hydro thermal method prepares the method for flame retardant of magnesium hydroxide, and described method comprises:
(1) magnesium chloride, the mixing of second alcohol and water are obtained mixed solution, in mixed solution, add the dispersion agent polyoxyethylene glycol, obtain the magnesium chloride mother liquor; Described magnesium chloride, ethanol, water and polyoxyethylene glycol amount ratio are: 10～50g: 20～60mL: 40～80mL: 0.05～1.0g;
(2) ammonia soln of getting mass concentration 2～36% is positioned in the airtight hydrothermal reaction kettle, be warming up to 40～200 ℃ under stirring, keep constant temperature in the reactor, then step (1) gained magnesium chloride mother liquor is dropped in the hydrothermal reaction kettle by the high pressure charging pump, until reaction solution pH is 9～12 o'clock, stops to drip, and constant temperature stirred after 0.5～5 hour, reaction solution obtains described flame retardant of magnesium hydroxide through separation and purification.
The present invention preferably carries out under the constant temperature and pressure condition, because reactor is airtight, under the homo(io)thermism condition, its internal pressure also is constant substantially, only needs when operation therefore that controlled temperature is constant to get final product.
It is 500～6000 product that described polyoxyethylene glycol is selected molecular weight usually for use, is preferably PEG6000 among the present invention.
Preferably, the temperature in the reactor is controlled at 100～200 ℃ in the described step (2).
Described separation and purification gets final product according to a conventional method, and purification procedures can be described in the present invention: after reaction finished, leaching filter residue distilled water wash was crossed in the reaction solution cooling, and drying gets described flame retardant of magnesium hydroxide.
Preferably, described method is as follows:
(1) magnesium chloride, the mixing of second alcohol and water are obtained mixed solution, in mixed solution, add dispersion agent PEG6000, obtain the magnesium chloride mother liquor; Described magnesium chloride, ethanol, water and PEG6000 amount ratio are: 15～30.5g: 20～50mL: 50～80mL: 0.1～0.2g;
(2) ammonia soln of preparation mass concentration 2～25%, place in the airtight hydrothermal reaction kettle, under 100～200 ℃ of constant temperature stir, slowly drop to step (1) gained magnesium chloride mother liquor in the reactor, until reaction solution pH is 9～12 o'clock, stop to drip, constant temperature stirred after 2～5 hours, and reaction solution is through naturally cooling, cross leaching filter residue usefulness distilled water wash, 110 ℃ of following dryings, obtain described flame retardant of magnesium hydroxide.
According to the inventive method, preparing the primary particle diameter of high-dispersion magnesium hydroxide particle is 0.1～2.0 μ m, and specific surface area is at 5～20m
2/ g, purity is greater than 99%, and pattern is the hexagonal flake structure.
The beneficial effect of the inventive method is mainly reflected in: (1) magnesium hydroxide is synthetic to be finished with one step of hydrothermal modification, had reduced technical process, had improved production efficiency, had reduced energy consumption; (2) the synthetic magnesium hydroxide has perfect degree of crystallinity, and surface polarity is little, is difficult for reuniting, and filters fast; (3) production process is all carried out in airtight hydrothermal reaction kettle, and ammoniacal liquor makes full use of, and no ammonia leakage had not only reduced cost but also non-environmental-pollution.
(4) description of drawings
Fig. 1 is embodiment 2 (80 a ℃) synthetic magnesium hydroxide particle pattern;
Fig. 2 is embodiment 3 (100 a ℃) synthetic magnesium hydroxide particle pattern;
Fig. 3 is embodiment 4 (120 a ℃) synthetic magnesium hydroxide particle pattern;
Fig. 4 is embodiment 6 (200 a ℃) synthetic magnesium hydroxide particle pattern;
Fig. 5 is embodiment 6 (200 a ℃) synthetic magnesium hydroxide particle X-ray powder diffraction pattern;
(5) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
Embodiment 1:
30.4845g magnesium chloride and 0.2145g PEG 6000 (Shanghai Zhuo Kang bio tech ltd) are dissolved in the 50ml distilled water, add 50ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 6% is positioned in the airtight hydrothermal reaction kettle, be warming up to 40 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 9.5 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 40 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 200～300nm, crystalline thickness mainly is distributed in 20～50nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Embodiment 2:
30.4845g magnesium chloride and 0.2145g PEG 6000 (Shanghai Zhuo Kang bio tech ltd) are dissolved in the 50ml distilled water, add 50ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 6% is positioned in the airtight hydrothermal reaction kettle, be warming up to 80 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 9.5 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 80 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, Figure 1 shows that the magnesium hydroxide of originally executing the example preparation amplifies 50,000 times photo, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 150～200nm, crystalline thickness mainly is distributed in 50～100nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Embodiment 3:
30.4845g magnesium chloride and 0.2145g PEG 6000 (Shanghai Zhuo Kang bio tech ltd) are dissolved in the 50ml distilled water, add 50ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 6% is positioned in the airtight hydrothermal reaction kettle, be warming up to 100 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 10.0 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 100 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, Figure 2 shows that the magnesium hydroxide of originally executing the example preparation amplifies 50,000 times photo, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 200～300nm, crystalline thickness mainly is distributed in 100～150nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Embodiment 4:
30.4845g magnesium chloride and 0.2145g PEG 6000 (Shanghai Zhuo Kang bio tech ltd) are dissolved in the 50ml distilled water, add 50ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 6% is positioned in the airtight hydrothermal reaction kettle, be warming up to 120 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 11.5 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 120 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, Figure 3 shows that the magnesium hydroxide of originally executing the example preparation amplifies 50,000 times photo, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 100～150nm, crystalline thickness mainly is distributed in 50～150nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Embodiment 5:
30.4845g magnesium chloride and 0.2145g PEG 6000 (Shanghai Zhuo Kang bio tech ltd) are dissolved in the 50ml distilled water, add 50ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 20% is positioned in the airtight hydrothermal reaction kettle, be warming up to 140 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 11.0 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 140 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 200～300nm, crystalline thickness mainly is distributed in 20～50nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Embodiment 6:
30.4845g magnesium chloride and 0.2145g PEG 6000 (Shanghai Zhuo Kang bio tech ltd) are dissolved in the 50ml distilled water, add 50ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 10% is positioned in the airtight hydrothermal reaction kettle, be warming up to 200 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 9.0 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 200 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, Figure 4 shows that the magnesium hydroxide of originally executing the example preparation amplifies 50,000 times photo, Fig. 5 is for originally executing the magnesium hydroxide X-ray powder diffraction pattern of example preparation, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 600～700nm, and crystalline thickness mainly is distributed in 100～200nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Embodiment 7:
30.4845g magnesium chloride and 0.2145g PEG 600 (Shanghai Kai Bite chemical industry company limited) are dissolved in the 80ml distilled water, add 20ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 25% is positioned in the airtight hydrothermal reaction kettle, be warming up to 100 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 9.5 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 100 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 150～200nm, crystalline thickness mainly is distributed in 50～100nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Embodiment 8:
15.2425g magnesium chloride and 0.1072g PEG 2000 (Shanghai Kai Bite chemical industry company limited) are dissolved in the 50ml distilled water, add 50ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 3% is positioned in the airtight hydrothermal reaction kettle, be warming up to 100 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 9.5 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 100 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 150～200nm, crystalline thickness mainly is distributed in 20～50nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Embodiment 9:
30.4845g magnesium chloride and 0.2145g PEG 1000 (going up the prompt trade Co., Ltd in ocean) are dissolved in the 50ml distilled water, add 50ml ethanol, get magnesium chloride mother liquor (1).The ammonia soln of getting mass concentration 12% is positioned in the airtight hydrothermal reaction kettle, be warming up to 100 ℃ under stirring, keep constant temperature in the reactor, then magnesium chloride mother liquor (1) being dropped in the hydrothermal reaction kettle by the high pressure charging pump, is 9.5 o'clock until reaction solution pH, stops to drip, constant temperature stirs after 1 hour for 100 ℃ reaction solution is cooled off, filter, use distilled water wash, products therefrom is dry under 110 ℃, obtain white powder.Particle diameter and pattern with transmission electron microscope (SEM) observation sample, powder is a nano level hexagonal flake crystal, purity height (99.5%), scattered, pattern is regular, crystal particle diameter mainly is distributed in 100～200nm, crystalline thickness mainly is distributed in 100～200nm, and specific surface area is at 4～20m
2/ g, surface polarity is little, is difficult for reuniting, and filters fast.
Claims (5)
1. one step hydro thermal method prepares the method for flame retardant of magnesium hydroxide, and described method comprises:
(1) magnesium chloride, the mixing of second alcohol and water are obtained mixed solution, in mixed solution, add the dispersion agent polyoxyethylene glycol, obtain the magnesium chloride mother liquor; Described magnesium chloride, ethanol, water and polyoxyethylene glycol amount ratio are: 10～50g: 20～60mL: 40～80mL: 0.05～1.0g;
(2) ammonia soln of getting mass concentration 2～36% places in the airtight hydrothermal reaction kettle, be warming up to 40～200 ℃ under stirring, keep constant temperature in the reactor, then step (1) gained magnesium chloride mother liquor is dropped in the hydrothermal reaction kettle, until reaction solution pH is 9～12 o'clock, stops to drip, and insulated and stirred is after 0.5～5 hour, reaction solution obtains described flame retardant of magnesium hydroxide through separation and purification.
2. the method for claim 1 is characterized in that described polyoxyethylene glycol is PEG6000.
3. the method for claim 1 is characterized in that the temperature in described step (2) reactor is controlled at 100～200 ℃.
4. the method for claim 1 is characterized in that described purification procedures is: after reaction finished, leaching filter residue distilled water wash was crossed in the reaction solution cooling, and drying gets described flame retardant of magnesium hydroxide.
5. the method for claim 1 is characterized in that described method is as follows:
(1) magnesium chloride, the mixing of second alcohol and water are obtained mixed solution, in mixed solution, add dispersion agent PEG6000, obtain the magnesium chloride mother liquor; Described magnesium chloride, ethanol, water and PEG6000 amount ratio are: 15～30.5g: 20～50mL: 50～80mL: 0.1～0.2g;
(2) ammonia soln of preparation mass concentration 2～25%, place in the airtight hydrothermal reaction kettle, under 100～200 ℃ of constant temperature stir, step (1) gained magnesium chloride mother liquor is dropped in the reactor, until reaction solution pH is 9～12 o'clock, stop to drip, insulated and stirred is after 2～5 hours, and reaction solution is through naturally cooling, cross leaching filter residue usefulness distilled water wash, 110 ℃ of following dryings, obtain described flame retardant of magnesium hydroxide.
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| CN102502728A (en) * | 2011-10-12 | 2012-06-20 | 江苏艾特克阻燃材料有限公司 | Magnesium hydroxide flame retardant and preparation method thereof |
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| CN104724734A (en) * | 2013-12-18 | 2015-06-24 | 中国科学院福建物质结构研究所 | Method for producing flower-like sphere type nanometer magnesium hydroxide with characteristics of light weight and high specific surface area |
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