CN1331984C - Prepn of magnesium hydroxide for fire retardant - Google Patents
Prepn of magnesium hydroxide for fire retardant Download PDFInfo
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- CN1331984C CN1331984C CNB2006100424112A CN200610042411A CN1331984C CN 1331984 C CN1331984 C CN 1331984C CN B2006100424112 A CNB2006100424112 A CN B2006100424112A CN 200610042411 A CN200610042411 A CN 200610042411A CN 1331984 C CN1331984 C CN 1331984C
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Abstract
The present invention relates to a process for preparing magnesium hydroxide for fire retardants, and belongs to the field of chemical material technology. The preparation process comprises the following steps: thoroughly mixing light burnt magnesia with water in the weight ratio of (0.5 to 3): (3 to 7); dropping a water solution of sodium hydroxide while stirring, until the final concentration of the sodium hydroxide is from 4 to 6 M; filling 70% to 80% volume of high-pressure reaction vessel with the mixture which is stirred for 10 to 60 minutes; carrying out a hydrothermal reaction at 140 to 180 DEG C for 6 to 10 h; naturally cooling the product to the room temperature, washing the product with water and baking the product to obtain magnesium flakes for fire retardants. The preparation process has the advantages of simple preparation process and low cost, and the prepared products of magnesium hydroxide has good crystallinity, regular shape and uniform particle size and satisfies the requirements of fire-retardant magnesium hydroxide.
Description
(1) technical field
The present invention relates to the method that water-heat process prepares magnesium hydroxide for fire retardant, belong to the chemical material technical field.
(2) background technology
Magnesium hydroxide is a kind of novel inorganic fire retardant of developing in recent years, it have thermostability, non-volatile, do not produce toxic gas, do not corrode advantages such as processing units.Magnesium hydroxide is a kind of industrial chemicals that is rich in crystal water, when decomposes discharges mass crystallization water, stops flame to produce or spreads thereby absorb temperature that a large amount of heat energy reduce heated bodies.And the magnesium oxide of its generation itself is good refractory materials, and Here it is, and it can be as the reason of fire-retardant raw material, and magnesium hydroxide belongs to the addition type inorganic combustion inhibitor, compares with similar inorganic combustion inhibitor, has better smoke suppressing effect.Magnesium hydroxide produce, use and discarded process in all unharmful substance dischargings, and can also in and the acidity and the corrosive gases that produce in the combustion processes, be a kind of environment-friendly fire retardant; Magnesium hydroxide heat decomposition temperature height, exceed 140 ℃ than inorganic combustion inhibitor aluminium hydroxide commonly used at present, can make the synthetic materials that adds magnesium hydroxide can bear higher processing temperature, help accelerating extrusion molding speed, shorten molding cycle, simultaneously also helping to improve flame retarding efficiency, is the most rising, eco-friendly at present inorganic combustion inhibitor, becomes the focus of various countries' research in recent years.
Though magnesium hydroxide has good flame retardancy, but, cause big, the many factors that influence economic benefit such as growth efficiency is low, production cost height of regular flake magnesium hydroxide equipment of industrial product investment of fire-retardant usefulness owing to have morphology control and strainability two large problems in the magnesium hydroxide production process.
The production technique of magnesium hydroxide has multiple, and how the bittern water with magnesium chloride (normally Magnesium dichloride hexahydrate) or salt manufacturing by-product is raw material, adds alkaloids and makes through precipitation.The difference of alkali kind can be divided into calcium hydroxide method, ammonia process, sodium hydroxide method etc. by adding.
There are some problems to some extent in these preparation technologies, product separation difficulty for example, and facility investment is big, production efficiency is low, production cost is high.Simultaneously the ordinary hydrogen magnesium oxide produced of these methods has bigger surface-area, is easy to assemble agglomerating between the particle, and dispersiveness in high molecular synthetic material and consistency are all very poor, can't be directly used in the fire-retardant of material.
(3) summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of novel magnesium hydroxide synthesis technique is provided, promptly utilize light calcined magnesia to prepare the fire-retardant flake magnesium hydroxide of using.
The present invention is raw materials used to be light calcined magnesia, and chemical ingredients is a magnesium oxide, white powder, and particle diameter is about 40-50um, is that magnesite forms through light-burned reflecting kiln, rotary kiln or fluidizing furnace calcining, and production technique is simple, and producer is on sale, and is cheap.
Raw material light calcined magnesia and water are pressed mass ratio and are (0.5-3): (3-7) thorough mixing, in whipping process, dropping is equivalent to the aqueous sodium hydroxide solution of mixture (2-4.5) times volume of light calcined magnesia and water, it is 4-6M that the control concentration sodium hydroxide makes the naoh concentration of final system, change in the autoclave after stirring 10min-1h, compactedness is 70-80%.Hydro-thermal reaction 6-10h in 140 ℃ of-180 ℃ of scopes, products therefrom naturally cools to room temperature, again its washing oven dry is promptly got the regular flake magnesium hydroxide of fire retardant.
Preferably, when final system naoh concentration is 4M, hydrothermal temperature is 160 ℃, and the hydro-thermal time, products therefrom pattern and dispersity were better relatively, and preparation condition is both economical when being 10h.
Compared with prior art, method of the present invention has the advantage that production technique is simple, cost is low, and prepared magnesium hydroxide products crystallinity is good, and the pattern rule mostly is six sides, and size distribution is even, can satisfy the requirement of flame retardant resistance magnesium hydroxide.
(4) description of drawings
Fig. 1 is the transmission electron microscope photo of the magnesium hydroxide for fire retardant of the inventive method preparation.A is embodiment 1 a gained sample, and b is embodiment 2 gained samples, and c is embodiment 3 gained samples.
Fig. 2 is the stereoscan photograph of products obtained therefrom magnesium hydroxide, and wherein a is the low power enlarged view, and b is a high magnification map, and magnification is seen scale among the figure.
Fig. 3 is the electron-diffraction diagram of products obtained therefrom magnesium hydroxide.
Fig. 4 is the XRD spectra of products obtained therefrom magnesium hydroxide.
(5) embodiment
Embodiment 1:
Light-burned type magnesium oxide of raw material and water are pressed 1: 2 thorough mixing of mass ratio, in whipping process, dropping is equivalent to the aqueous sodium hydroxide solution of light calcined magnesia and 2 times of volumes of water mixture, it is 4M that the control concentration sodium hydroxide makes the naoh concentration of final system, change in the autoclave behind the stir about 30min, compactedness is 80%.160 ℃, hydro-thermal reaction 10h, products therefrom naturally cools to room temperature, again its washing oven dry is promptly got the fire retardant flake magnesium hydroxide.The product transmission electron microscope photo is seen Fig. 1 a, stereoscan photograph as shown in Figure 2, electron-diffraction diagram such as Fig. 3, XRD spectra such as Fig. 4.
Embodiment 2:
Raw material light calcined magnesia and water are 1: 1.5 thorough mixing by mass ratio, in whipping process, dropping is equivalent to the aqueous sodium hydroxide solution of light calcined magnesia and 3 times of volumes of water mixture, it is 5M that the control concentration sodium hydroxide makes the naoh concentration of final system, change in the autoclave after stirring 40min, compactedness is 75%.170 ℃ of hydro-thermal reaction 8h, products therefrom naturally cools to room temperature, again its washing oven dry is promptly got the fire retardant flake magnesium hydroxide.The product transmission electron microscope photo is seen Fig. 1 b.
Embodiment 3:
Light-burned type magnesium oxide of raw material and water are pressed 1: 3 thorough mixing of mass ratio, in whipping process, dropping is equivalent to the aqueous sodium hydroxide solution of light calcined magnesia and 1.5 times of volumes of water mixture, it is 6M that the control concentration sodium hydroxide makes the naoh concentration of final system, change in the autoclave behind the stir about 50min, compactedness is 80%.180 ℃, hydro-thermal reaction 6h, products therefrom naturally cools to room temperature, again its washing oven dry is promptly got the fire retardant flake magnesium hydroxide.The product transmission electron microscope photo is seen Fig. 1 c.
Claims (2)
1, preparation process of magnesium hydroxide, light-burned type magnesium oxide and water are 0.5-3 by mass ratio: the 3-7 thorough mixing, in whipping process, dropping is equivalent to the aqueous sodium hydroxide solution of the mixture 2-4.5 times volume of light calcined magnesia and water, it is 4-6M that the control concentration sodium hydroxide makes the naoh concentration of final system, change in the autoclave after stirring 10min-1h, compactedness is 70-80%, hydro-thermal reaction 6-10h in 140 ℃ of-180 ℃ of scopes, products therefrom naturally cools to room temperature, again its washing oven dry is promptly got fire retardant hexagonal flake magnesium hydroxide.
2, preparation process of magnesium hydroxide as claimed in claim 1 is characterized in that final system naoh concentration is 4M, and hydrothermal temperature is 160 ℃, and the hydro-thermal time is 10h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100424112A CN1331984C (en) | 2006-02-23 | 2006-02-23 | Prepn of magnesium hydroxide for fire retardant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100424112A CN1331984C (en) | 2006-02-23 | 2006-02-23 | Prepn of magnesium hydroxide for fire retardant |
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| Publication Number | Publication Date |
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| CN1810927A CN1810927A (en) | 2006-08-02 |
| CN1331984C true CN1331984C (en) | 2007-08-15 |
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| CNB2006100424112A Expired - Fee Related CN1331984C (en) | 2006-02-23 | 2006-02-23 | Prepn of magnesium hydroxide for fire retardant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659146A (en) * | 2012-04-28 | 2012-09-12 | 中国科学院福建物质结构研究所 | Method for preparing flame retardant magnesium hydroxide |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101684B (en) * | 2009-12-16 | 2012-10-24 | 中国科学院过程工程研究所 | Method for preparing submicron lamellar magnesium hydroxide by intensifying alkali |
| CN102030348B (en) * | 2010-10-15 | 2012-07-04 | 北京化工大学 | Device and method for continuously preparing magnesium hydroxide flame retardant |
| CN102408121A (en) * | 2011-03-04 | 2012-04-11 | 山东海龙股份有限公司 | Method for preparing magnesium hydroxide fire retardant with lithium carbonate by-product magnesium oxide slag |
| CN105670296B (en) * | 2015-12-28 | 2020-09-25 | 国家纳米科学中心 | Preparation method of in-situ composite nano cerium dioxide/magnesium hydroxide flame-retardant smoke suppressant for RTV (room temperature vulcanization) |
| SE539377C2 (en) * | 2016-02-24 | 2017-08-29 | Deflamo Ab | A process for manufacturing of fire suppressing crystals |
| CN109761252A (en) * | 2019-03-22 | 2019-05-17 | 中民驰远实业有限公司 | A kind of preparation method of magnesium hydrate powder |
| CN113046098A (en) * | 2019-12-27 | 2021-06-29 | 江苏艾特克阻燃材料有限公司 | Magnesium-boron composite flame retardant and preparation method thereof |
| CN113582209A (en) * | 2021-08-26 | 2021-11-02 | 上海应用技术大学 | Preparation method and application of hexagonal flaky magnesium hydroxide |
| 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 |
| CN113913072B (en) * | 2021-11-02 | 2022-10-14 | 雨中情防水技术集团股份有限公司 | Flame-retardant isolation sand for asphalt-based pre-laid waterproof coiled material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1224041A (en) * | 1997-12-24 | 1999-07-28 | 中国科学院近代物理研究所 | Process for preparing surface-active magnesium hydrooxide flame retardant |
| CN1341694A (en) * | 2001-09-19 | 2002-03-27 | 北京化工大学 | Preparation process of magnesium hydroxide fire-retarding nanomaterial |
| CN1508072A (en) * | 2002-12-13 | 2004-06-30 | 北京化工大学 | Method for preparing nano magnesium oxide |
-
2006
- 2006-02-23 CN CNB2006100424112A patent/CN1331984C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1224041A (en) * | 1997-12-24 | 1999-07-28 | 中国科学院近代物理研究所 | Process for preparing surface-active magnesium hydrooxide flame retardant |
| CN1341694A (en) * | 2001-09-19 | 2002-03-27 | 北京化工大学 | Preparation process of magnesium hydroxide fire-retarding nanomaterial |
| CN1508072A (en) * | 2002-12-13 | 2004-06-30 | 北京化工大学 | Method for preparing nano magnesium oxide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659146A (en) * | 2012-04-28 | 2012-09-12 | 中国科学院福建物质结构研究所 | Method for preparing flame retardant magnesium hydroxide |
| CN102659146B (en) * | 2012-04-28 | 2014-09-17 | 中国科学院福建物质结构研究所 | Method for preparing flame retardant magnesium hydroxide |
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| CN1810927A (en) | 2006-08-02 |
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