CN1982410A - Production of high-dispersion flake nano-magnesium hydrate fire retardant - Google Patents
Production of high-dispersion flake nano-magnesium hydrate fire retardant Download PDFInfo
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- CN1982410A CN1982410A CN 200510130957 CN200510130957A CN1982410A CN 1982410 A CN1982410 A CN 1982410A CN 200510130957 CN200510130957 CN 200510130957 CN 200510130957 A CN200510130957 A CN 200510130957A CN 1982410 A CN1982410 A CN 1982410A
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Abstract
Process of high-dispersing magnesium hydrate is carried out by mixing alkaline solution with water solution containing magnesium ion, fast depositing, synthesizing>100degree and hydrothermal treating>100degree. The magnesium hydrate crystal grain is hexagonal laminated sheet, the size is between 300-1000 nanometer and thickness is between 50-100 nanometer. It's efficient, has long hydrothermal treatment time, better dispersion and compatibility, and less rheological property and mechanical performance. It can be used for halogen-free smokeless fire-retardant polymer additive.
Description
The present invention relates generally to preparation method's technical field of high-dispersion flake nano-magnesium hydrate fire retardant.
Magnesium hydroxide since have fire-retardant, press down cigarette, environmental protection and heat decomposition temperature advantages of higher, be one of polymer flame retardant that has huge market potential.Because magnesium hydroxide is the very strong mineral compound of a kind of polarity, its crystal has the microcosmic internal stress in (101) direction, the plane of crystal possess hydrophilic property, adopting traditional technology synthetic magnesium hydroxide under normal temperature condition is nanocrystal, surface polarity is stronger, being easy to reunite, to form particle diameter be 10～100 microns secondary example, has very big surface-area, dispersiveness and consistency in synthetic materials are very poor, the processing characteristics of havoc polymer materials and mechanical property, thereby can't be directly used in the fire-retardant of polymer materials.Magnesium hydroxide as fire retardant requires to have low specific surface area and low microcosmic internal stress.
Through literature survey, we find that the preparation technology of present flame retardant of magnesium hydroxide is: at first make magnesium salts and alkaline solution generation precipitin reaction under low temperature or room temperature, carry out 4～20 hours hydrothermal treatment consists then under high temperature (100～250 ℃) and make.The flame retardant of magnesium hydroxide specific surface area of this method preparation is little, has dispersing property preferably in polymer materials.But since its at high temperature time of hydrothermal treatment consists longer, production efficiency is lower, cost is higher.
In order to improve the production efficiency of magnesium hydroxide crystal, the present invention proposes a kind of new preparation process of high-dispersion flake nano level flame retardant of magnesium hydroxide.
The preparation method of this high-dispersion flake nano level magnesium hydroxide crystal, be characterised in that: with the at high temperature direct short mix of the alkaline solution and the aqueous solution that contains magnesium ion, precipitin reaction takes place, [, be mixed into the shallow lake temperature of reaction and be controlled at 80-250 ℃ (temperature is more economical in 80～160 ℃ of scopes) for the alkaline solution system of ammoniacal liquor; Alkaline solution system for sodium hydroxide or potassium hydroxide, being mixed into the shallow lake temperature of reaction is controlled at 110-300 ℃ and carries out (temperature is more economical in 160～220 ℃ of scopes)], insulation 0-5 hour in 110-300 ℃ of scope then (holding temperature is more economical in 0～2 hour scope in 160～220 ℃ of scopes, soaking time); Suction filtration afterwards, washing, dry white powder product.
The described aqueous solution that contains magnesium ion comprises the aqueous solution of magnesium chloride, magnesium nitrate or sal epsom, and its amount of substance concentration is 0.5-2mol/l;
Described alkaline solution can adopt the 0.5-2mol/l sodium hydroxide that amount of substance concentration is or the aqueous solution or the ammoniacal liquor or the ammonia of potassium hydroxide.
Can add a small amount of magnesium hydroxide crystal seed in described magnesium ion solution or the alkaline solution, Zhi Bei magnesium hydroxide crystal particle size is bigger like this, and crystallization is more complete.
The magnesium hydroxide of this processing method preparation is characterized by laminar hexagon crystal grain, and particle size is in 300～1000 nanometers, and thickness is 50～100 nanometers; The crystal grain specific surface area is little, and good dispersity is not easy to reunite, and is better with the consistency of polymer materials, and is less to influences such as the processing rheological property of synthetic materials, mechanical properties, can be used as the additive of low cigarette, the nontoxic flame-retardant polymer of Halogen.
The magnesium hydroxide of this processing method preparation, its crystal grain size and crystalline integrated degree improve with the increase of soaking time and holding temperature, thereby its polarity decreases, and its consistency in polymeric matrix increases thereupon.
Preparation method of the present invention compares with the preparation method who has traditional flame retardant of magnesium hydroxide now, owing to adopted high temperature precipitin reaction method, can directly be settled out and have crystalline size magnesium hydroxide crystal particle bigger, that crystallization is more complete, the high-temperature water thermal treatment of a need short period afterwards can obtain the magnesium hydroxide crystal particle of high comprehensive performance, thereby shortened the reaction times greatly, and the product of gained is easy to filter, so improved its production efficiency greatly, reduced the production cost of flame retardant of magnesium hydroxide.
Below be embodiments of the invention:
Embodiment 1
The 81.2g Magnesium dichloride hexahydrate is dissolved in the 250ml distilled water, be dissolved in 32g sodium hydroxide in the 60ml distilled water and the ready made polypropylene film bag of packing into, together put into autoclave with magnesium chloride solution after heat-sealing is good, being warming up to 160 ℃ begins to stir, continue to be warming up to 180 ℃ of constant temperature, stir cooling fast afterwards in 60 minutes, with distilled water wash, suction filtration back (strainability is better) repeatedly, with the gained paste 105 ± 5 ℃ down oven dry obtain white powder product.Direct viewing particle diameter and pattern under scanning electronic microscope (SEM), and take a picture (seeing accompanying drawing 1), the result shows that this product is a thin slice hexagon crystal, and thickness is 70～80 nanometers, and particle diameter is in 300～1000 nanometers, wherein based on the particle diameter about 800 nanometers.Measure with XSS-300 type torque rheometer, the result shows that the melt rheological property of the EVA mixture that not surface treated this product of content 50% is filled can be better, and balancing moment is 21Nm.Mechanical property detects and shows that the tensile strength of this mixture reaches 14.4MPa, and elongation at break is 180%.
(accompanying drawing 1 is the electromicroscopic photograph that the magnesium hydroxide products that obtains in the present embodiment amplifies 10,000 times and 30,000 times.)
Embodiment 2
The 81.2g Magnesium dichloride hexahydrate is dissolved in the 250ml distilled water, be dissolved in 32g sodium hydroxide in the 60ml distilled water and the ready made polypropylene film bag of packing into, together put into autoclave with magnesium chloride solution after heat-sealing is good, being warming up to 160 ℃ begins to stir, continue to be warming up to 180 ℃ of constant temperature, stir cooling fast afterwards in 3 hours, with distilled water wash, suction filtration back (strainability is fine) repeatedly, with the gained paste 105 ± 5 ℃ down oven dry obtain white powder product.Direct viewing particle diameter and pattern under SEM, and take a picture (seeing accompanying drawing 2), the result shows that this product is close with example 1, but the product crystal crystallization is more complete.Measure with XSS-300 type torque rheometer, the result shows that the melt rheological property of the EVA mixture that not surface treated this product of content 50% is filled can be better, and balancing moment is 16Nm.Mechanical property detects and shows that the tensile strength of this mixture is 11.0MPa, and elongation at break reaches 430%.
(accompanying drawing 2 is electromicroscopic photographs that the magnesium hydroxide products that obtains in the present embodiment amplifies 10,000 times and 30,000 times.)
Embodiment 3
The 81.2g Magnesium dichloride hexahydrate is dissolved in the 250ml distilled water, be dissolved in 32g sodium hydroxide in the 60ml distilled water and the ready made polypropylene film bag of packing into, together put into autoclave with magnesium chloride solution after heat-sealing is good, being warming up to 160 ℃ begins to stir, continue to be warming up to 180 ℃ of constant temperature, stir cooling fast afterwards in 5 hours, with distilled water wash, suction filtration back (strainability is fine) repeatedly, with the gained paste 105 ± 5 ℃ down oven dry obtain white powder product.Direct viewing particle diameter and pattern under SEM, and take a picture (seeing accompanying drawing 3), the result shows that this product is close with example 2 with example 1, but the product crystal crystallization is more complete.
(accompanying drawing 3 is electromicroscopic photographs that the magnesium hydroxide products that obtains in the present embodiment amplifies 10,000 times and 30,000 times.)
Embodiment 4
The 81.2g Magnesium dichloride hexahydrate is dissolved in the 130ml distilled water, with 121ml concentration is 25% ammoniacal liquor and a small amount of nano-sized magnesium hydroxide crystal seed ready made polypropylene film bag of together packing into, together put into autoclave with magnesium chloride solution after heat-sealing is good, being warming up to 160 ℃ begins to stir, continue to be warming up to 180 ℃ of constant temperature, stir cooling fast afterwards in 10 minutes, with distilled water wash, suction filtration back (strainability is good) repeatedly, with the gained paste 105 ± 5 ℃ down oven dry obtain white powder product.Direct viewing particle diameter and pattern under SEM, and take a picture (seeing accompanying drawing 4), the result shows that this product is a thin slice hexagon crystal, and thickness is 50～60 nanometers, and particle diameter is in 300～1000 nanometers, wherein based on the particle diameter about 600 nanometers.Measure with XSS-300 type torque rheometer, the result shows that the melt rheological property of the EVA mixture that not surface treated this product of content 50% is filled can be better, and balancing moment is 18.5Nm.Mechanical property detects and shows that the tensile strength of this mixture is 10.5MPa, and elongation at break is 280%.
(accompanying drawing 4 is electromicroscopic photographs that the magnesium hydroxide products that obtains in the present embodiment amplifies 10,000 times and 30,000 times.)
Embodiment 5
The 81.2g Magnesium dichloride hexahydrate is dissolved in the 130ml distilled water, with 121ml concentration is 25% ammoniacal liquor and a small amount of nano-sized magnesium hydroxide crystal seed ready made polypropylene film bag of together packing into, together put into autoclave with magnesium chloride solution after heat-sealing is good, being warming up to 160 ℃ begins to stir, continue to be warming up to 180 ℃ of constant temperature, stir cooling fast afterwards in 1 hour, with distilled water wash, suction filtration back (strainability is good) repeatedly, with the gained paste 105 ± 5 ℃ down oven dry obtain white powder product.Measure with XSS-300 type torque rheometer, the result shows that the melt rheological property of the EVA mixture that not surface treated this product of content 50% is filled can be better, and balancing moment is 17Nm.Mechanical property detects and shows, the EVA mixture that not surface treated this product is filled has mechanical property preferably, tensile strength 10.9MPa, elongation at break 470%.
Embodiment 6
The 81.2g Magnesium dichloride hexahydrate is dissolved in the 130ml distilled water, with 121ml concentration is 25% ammoniacal liquor and a small amount of nano-sized magnesium hydroxide crystal seed ready made polypropylene film bag of together packing into, together put into autoclave with magnesium chloride solution after heat-sealing is good, being warming up to 160 ℃ begins to stir, continue to be warming up to 180 ℃ of constant temperature, stir cooling fast afterwards in 3 hours, with distilled water wash, suction filtration back (strainability is good) repeatedly, with the gained paste 105 ± 5 ℃ down oven dry obtain white powder product.Direct viewing particle diameter and pattern under SEM, and take a picture (seeing accompanying drawing 5), the result shows that this product is close with example 4, but the product crystal particle diameter is bigger, and crystallization is more complete.
(accompanying drawing 5 is electromicroscopic photographs that the magnesium hydroxide products that obtains in the present embodiment amplifies 10,000 times and 30,000 times.)
Claims (1)
- The present invention proposes a kind of new preparation process of high-dispersion flake nano level flame retardant of magnesium hydroxide.The preparation method of this high-dispersion flake nano level magnesium hydroxide crystal, be characterised in that: with the at high temperature direct short mix of the alkaline solution and the aqueous solution that contains magnesium ion, precipitin reaction takes place, [, be mixed into the shallow lake temperature of reaction and be controlled at 80-250 ℃ (temperature is more economical in 80～160 ℃ of scopes) for the alkaline solution system of ammoniacal liquor; Alkaline solution system for sodium hydroxide or potassium hydroxide, being mixed into the shallow lake temperature of reaction is controlled at 110-300 ℃ and carries out (temperature is more economical in 160～220 ℃ of scopes)], insulation 0-5 hour in 110-300 ℃ of scope then (holding temperature is more economical in 0～2 hour scope in 160～220 ℃ of scopes, soaking time); Suction filtration afterwards, washing, dry white powder product.The described aqueous solution that contains magnesium ion comprises the aqueous solution of magnesium chloride, magnesium nitrate or sal epsom, and its amount of substance concentration is 0.5-2mol/l;Described alkaline solution can adopt the 0.5-2mol/l sodium hydroxide that amount of substance concentration is or the aqueous solution or the ammoniacal liquor or the ammonia of potassium hydroxide.Can add a small amount of magnesium hydroxide crystal seed in described magnesium ion solution or the alkaline solution, Zhi Bei magnesium hydroxide crystal particle size is bigger like this, and crystallization is more complete.
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| CN 200510130957 CN1982410A (en) | 2005-12-13 | 2005-12-13 | Production of high-dispersion flake nano-magnesium hydrate fire retardant |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495882A (en) * | 2014-12-09 | 2015-04-08 | 中国日用化学工业研究院 | Preparation method of highly-dispersed nano-magnesium hydroxide |
| CN106673027A (en) * | 2016-12-30 | 2017-05-17 | 安徽壹石通材料科技股份有限公司 | Preparation and synthesis method of hexagonal flaky magnesium hydroxide fire retardant |
| CN108587239A (en) * | 2018-04-10 | 2018-09-28 | 青海民族大学 | A kind of preparation method of modified magnesium hydroxide |
| CN110437379A (en) * | 2019-08-10 | 2019-11-12 | 南京青龙线缆材料有限公司 | A kind of low temperature resistant halogen-free flame retardant insulation material of ultraviolet light cross-linking scratch-resistant and preparation method thereof |
| CN113881445A (en) * | 2021-09-29 | 2022-01-04 | 白银康宝新型节能建材有限责任公司 | Preparation method of magnesium-based flame-retardant material |
| CN114436301A (en) * | 2022-02-18 | 2022-05-06 | 洛阳中超新材料股份有限公司 | Preparation method of magnesium hydroxide large single crystal |
| CN115417436A (en) * | 2022-09-20 | 2022-12-02 | 西部金属材料股份有限公司 | Preparation method of two-dimensional magnesium hydroxide nanosheet |
-
2005
- 2005-12-13 CN CN 200510130957 patent/CN1982410A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495882A (en) * | 2014-12-09 | 2015-04-08 | 中国日用化学工业研究院 | Preparation method of highly-dispersed nano-magnesium hydroxide |
| CN104495882B (en) * | 2014-12-09 | 2016-08-24 | 中国日用化学工业研究院 | A kind of preparation method of high-dispersion nano magnesium hydroxide |
| CN106673027A (en) * | 2016-12-30 | 2017-05-17 | 安徽壹石通材料科技股份有限公司 | Preparation and synthesis method of hexagonal flaky magnesium hydroxide fire retardant |
| CN108587239A (en) * | 2018-04-10 | 2018-09-28 | 青海民族大学 | A kind of preparation method of modified magnesium hydroxide |
| CN110437379A (en) * | 2019-08-10 | 2019-11-12 | 南京青龙线缆材料有限公司 | A kind of low temperature resistant halogen-free flame retardant insulation material of ultraviolet light cross-linking scratch-resistant and preparation method thereof |
| CN113881445A (en) * | 2021-09-29 | 2022-01-04 | 白银康宝新型节能建材有限责任公司 | Preparation method of magnesium-based flame-retardant material |
| CN114436301A (en) * | 2022-02-18 | 2022-05-06 | 洛阳中超新材料股份有限公司 | Preparation method of magnesium hydroxide large single crystal |
| CN114436301B (en) * | 2022-02-18 | 2024-04-05 | 洛阳中超新材料股份有限公司 | Preparation method of magnesium hydroxide large monocrystal |
| CN115417436A (en) * | 2022-09-20 | 2022-12-02 | 西部金属材料股份有限公司 | Preparation method of two-dimensional magnesium hydroxide nanosheet |
| CN115417436B (en) * | 2022-09-20 | 2023-08-11 | 西部金属材料股份有限公司 | Preparation method of two-dimensional magnesium hydroxide nano-sheet |
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