CN105256405B - The method that magnesia aquation method prepares fibrous magnesium hydroxide - Google Patents
The method that magnesia aquation method prepares fibrous magnesium hydroxide Download PDFInfo
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- CN105256405B CN105256405B CN201510595799.8A CN201510595799A CN105256405B CN 105256405 B CN105256405 B CN 105256405B CN 201510595799 A CN201510595799 A CN 201510595799A CN 105256405 B CN105256405 B CN 105256405B
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- magnesium hydroxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/40—Production or processing of lime, e.g. limestone regeneration of lime in pulp and sugar mills
Abstract
The present invention relates to a kind of method that magnesia aquation method prepares fibrous magnesium hydroxide, comprise the following steps that：Magnisite calcining prepares light calcined magnesia；Modifying agent is added into ultrasonic disperse in ethanol and is made into modifier solution；Then it is 1 in mass ratio by light calcined magnesia, magnesium salts, water, dispersant：(0.02~4.5)：(10~100)：(0.03~0.5), is well mixed with modifier solution, obtains suspension, in after 2~6h of stirring reaction under 50 DEG C~100 DEG C of water bath with thermostatic control, then adds crystal seed and activating agent.Fibrous magnesium hydroxide is obtained after aged post processing.Present invention process is simple and easy to apply, and production cost is low, and product purity is high, easily-controlled reaction conditions；It is adapted to industrialized production；Low temperature hydrated reaction, saves energy consumption.
Description
Technical field
The invention belongs to inorganic particle technical field, and in particular to a kind of magnesia aquation method prepares fibrous magnesium hydroxide
Method.
Background technology
Current halogen organic fire-retardant is commercially applied than wide, and it has flame retarding efficiency high, and unit macromolecule is closed
The advantages of lacking into the addition consumption in material, but halogen organic fire-retardant can discharge poisonous or mordant gas in burning
Body, these toxic and harmful gas will make the life and health of people be made great efforts finding a kind of by grave danger, thus researcher
Low toxicity, low cigarette, the fire retardant with bright market prospects.Flame retardant of magnesium hydroxide is that current application amount is maximum, with fastest developing speed
One of inorganic no-halogen fire retardant, because good flame retardation effect, smokeless, nonhazardous, filling capacity is good in the material the advantages of extensive use
In Polymer Industry.
There is good anti-flammability in high polymer material, the loading of magnesium hydroxide need to be more than 50%, and high fills out
Charge makes the mechanical strength of material be decreased obviously therewith.Research finds sample its mechanical performance after the fibrous magnesium hydroxide of addition
Significantly better than the sample of the magnesium hydroxide of addition other shapes, therefore to ensure that magnesium hydroxide produces high resistant in high polymer material
Ensure that the mechanical property of material is not reduced while combustion performance, it should using a kind of threadiness, with good dispersion and compatible
The magnesium hydroxide products of property.
Preparing the method for fibrous magnesium hydroxide at present mainly has：First, direct precipitation method (CN101177289,
CN103803596A, Cao Ying, fibrous magnesium hydroxide [journal article], Ren Qingli are prepared using mother liquid of boric acid, prepared by hydro-thermal method
Fibrous Mg (OH)2[journal article])；2nd, presoma conversion method (CN1458066A, Zhang Shuyong, the system of fibrous magnesium hydroxide
Standby [journal article], CN1884633), such as CN1884633, using magnesite as raw material, produces extra light calcined magnesia, using its as
Waste alkali magnesium sulfate crystal whisker, then it is brilliant by hydrothermal synthesis method preparing magnesium hydroxide by raw material of alkali magnesium sulfate crystal whisker
Palpus.Technological process is complicated and is difficult to control reaction condition.
At present, this seminar prepares the research of magnesium hydroxide to magnesia aquation method and has done many relevant reports,
Such as：A kind of hexagonal sheet magnesium hydroxide of the inventions such as money petrel preparation method patent (China, CN201110336270.6 [P],
2012-6-20)；Preparation method patent (China, CN201510342011.2 of a kind of acicular magnesium hydroxide of the inventions such as money petrel
[P], 2015-6-18), but above-mentioned work is the preparation method for studying hexagonal flake and acicular magnesium hydroxide respectively, is also not directed to
Low-temperature oxidation magnesium aquation directly prepares fibrous magnesium hydroxide.
The content of the invention
A kind of oxygen high by simple and environmentally-friendly, yield is provided the invention aims to improve the deficiencies in the prior art
Change the method that magnesium aquation method prepares fibrous magnesium hydroxide.
The technical scheme is that：The method that magnesia aquation method prepares fibrous magnesium hydroxide, is comprised the following steps that：
A) magnisite is calcined, and prepares light calcined magnesia；
B) modifying agent is added into ultrasonic disperse in ethanol and is made into modifier solution；
C) it is 1 in mass ratio by light calcined magnesia, magnesium salts, water, dispersant：(0.02~4.5)：(10~100)：(0.03
~0.5), and it is well mixed with the step b) modifier solutions being made into, obtains suspension, suspension ultrasonic disperse is uniform, stirring
Under the conditions of mixing, in after 50 DEG C~100 DEG C of water bath with thermostatic control, 2~6h of reaction, crystal seed and activating agent are added；
D) step c) reaction solutions are aged；
E) in step d) reaction product through filtering, washing, be dried to obtain fibrous magnesium hydroxide.
The calcining heat of magnisite is 600 DEG C~1250 DEG C in preferred steps a)；Calcination time is 2~6h.
The ratio of the quality of modifying agent and ethanol volume is 1 in preferred steps b)：(10~100) g/ml.
The addition of modifier solution is that to control the addition quality of modifying agent be light calcined magnesia quality in preferred steps c)
1%~10%.
It is preferred that above-mentioned modifying agent be stearic acid, aluminate coupling agent H-3, stearic acid sodium or one kind in zinc stearate or
It is several.
It is preferred that described dispersant is polyvinylpyrrolidone, cetyl trimethylammonium bromide or PEG-400
One or more；Magnesium salts is magnesium sulfate.
It is preferred that described crystal seed is basic magnesium chloride whisker, alkali magnesium sulfate crystal whisker or magnesium hydroxide crystal whisker；Crystal seed is added
Quality is the 0.8%~50% of light calcined magnesia quality.
It is preferred that described activating agent is one kind or several of ethylenediamine, propane diamine, butanediamine, triethylamine or hexa
Kind.It is preferred that the volume of activating agent addition and the ratio of magnesia quality are 0.007~0.15ml/g.
Aging Temperature in preferred steps d) is 5 DEG C~50 DEG C, and digestion time is 2~10 days.Filtering in step e), wash
Wash, drying is handled according to a conventional method.
Beneficial effect：
Present invention process is simple and easy to apply, and production cost is low, and product purity is high, easily-controlled reaction conditions；It is adapted to industry metaplasia
Production；Low temperature hydrated reaction, saves energy consumption.The present invention can be prepared by changing dispersant, the addition of activating agent, species
The fibrous magnesium hydroxide of different draw ratios；Fibrous magnesium hydroxide prepared by the present invention can be recycled as crystal seed, be saved
Cost.
By raw material of magnesite, calcining obtains light calcined magnesia, can in preparing magnesium hydroxide with water reaction under lower temperature
To take full advantage of the magnesite resource of China's abundant, the fibrous magnesium hydroxide of one-step synthesis at low temperature, simple production process,
It is energy-saving, it is a kind of method of the fibrous magnesium hydroxide of preferable production with considerable economic value.
Brief description of the drawings
Fig. 1 prepares the XRD spectrum of fibrous magnesium hydroxide for the present invention；
Fig. 2 is the microscope figure of the products therefrom of embodiment 1；
Fig. 3 is the microscope figure of the products therefrom of embodiment 2；
Fig. 4 is the microscope figure of the products therefrom of embodiment 3；
Fig. 5 is the microscope figure of the products therefrom of embodiment 4；
Fig. 6 is the microscope figure of the products therefrom of embodiment 5.
Embodiment
Embodiment 1
0.03g stearic acid ultrasonic disperse in 2ml ethanol is weighed, magnesite is weighed in 650 DEG C of magnesia calcined after 6h
2.32g, adds 1.07g PEG-20000,0.65g magnesium sulfate and 25ml water is made into the aqueous solution, adds above-mentioned ethanol solution and continues
Ultrasonic disperse is uniform, after 50 DEG C of stirred in water bath reaction 6h, adds 0.28g basic magnesium chloride whiskers and 0.02ml propane diamine,
React and stop stirring after 8min, be aged 9 days at 6 DEG C, through filtering, washing, be dried to obtain fibrous magnesium hydroxide.The Mg of generation
(OH)2The XRD of crystal is as shown in figure 1, as seen from Figure 1, diffraction maximum and the magnesium hydroxide JCPDS86-2164 standard cards of generation
Match, free from admixture.Fig. 2 is the microscope photograph of this example products therefrom, and the magnesium hydroxide generated as can be seen from Figure 2 is fiber
, there is few irregular particle in shape, length is about 300 μm~1400 μm.
Embodiment 2
0.06g aluminate coupling agents H-3 ultrasonic disperses in 6ml ethanol are weighed, magnesite is weighed and is calcined in 900 DEG C after 4h
Magnesia 4.06g, add 0.56g polyvinylpyrrolidones, 0.56g cetyl trimethylammonium bromides, 18.07g magnesium sulfate
The aqueous solution is made into 400ml water, above-mentioned ethanol solution is added and continues ultrasonic disperse, after 80 DEG C of stirring in water bath reaction 4h, addition
1.92g alkali magnesium sulfate crystal whiskers react 10min as crystal seed and 0.20ml ethylenediamines, stop stirring, are aged 7 days at 12 DEG C,
Fibrous magnesium hydroxide can be obtained through filtering, washing, drying.Fig. 3 is the microscope photograph of this example products therefrom, as can be seen from Figure 3
The magnesium hydroxide of generation is threadiness, and more regular, length is about 400 μm~1900 μm.
Embodiment 3
Weigh that 0.13g stearic acids sodium is ultra-dispersed in 6ml ethanol, weigh magnesite in 1050 DEG C of magnesia calcined after 3h
4.13g, adds 0.13gPEG-20000,8.76g magnesium sulfate and 200ml water is made into the aqueous solution, adds above-mentioned ethanol solution and continues
Ultrasonic disperse, after 95 DEG C of stirring in water bath reaction 2h, addition 0.93g basic magnesium chloride whiskers crystal seed and 0.40ml butanediamine, instead
Answer after 6min, be placed at 20 DEG C and be aged 5 days, fibrous magnesium hydroxide (Fig. 4) can be obtained through filtering, washing, drying, its length is about
240 μm~1500 μm.
Embodiment 4
Weigh that 0.31g zinc stearates are ultra-dispersed in 15ml ethanol, weigh magnesite in 1050 DEG C of oxidations calcined after 3h
Magnesium 6.08g, adds 0.49g polyvinylpyrrolidones, 0.49g cetyl trimethylammonium bromides, 11.80g magnesium sulfate and 200ml
Water is made into the aqueous solution, adds above-mentioned ethanol solution and continues ultrasonic disperse, after 85 DEG C of stirring in water bath reaction 4h, adds 1.39g alkali
Formula magnesium sulfate crystal whisker crystal seed and 0.60ml triethylamines, reaction 6min, stop stirring, are aged 4 days at 22 DEG C, through filtering, washing,
Drying can obtain fibrous magnesium hydroxide.The microscope photograph of this example product is as shown in figure 5, the product draw ratio as can be seen from Figure 5
It is larger, Chang Du≤2200 μm.
Embodiment 5
0.81g stearic acid ultrasonic disperse in 12ml ethanol is weighed, magnesia obtained by 1250 DEG C of calcining 2h magnesite is weighed
8.15g, adds 0.21g polyvinylpyrrolidones, 0.21g cetyl trimethylammonium bromides, 0.18g magnesium sulfate and 560ml water
The aqueous solution is made into, above-mentioned ethanol solution is added and continues ultrasonic disperse uniformly, after 90 DEG C of stirring in water bath reaction 3h, 0.08g is added
Magnesium hydroxide crystal whisker reacts 6min as crystal seed and 1.20ml hexas, stops stirring, is aged 2 days at 45 DEG C, warp
Filtering, washing, drying can obtain fibrous magnesium hydroxide.Fig. 6 is the microscope photograph of this example products therefrom, and product exists a small number of
Needle-like, major diameter is about 200 μm~2200 μm.
Claims (9)
1. the method that magnesia aquation method prepares fibrous magnesium hydroxide, is comprised the following steps that：
A) magnisite is calcined, and prepares light calcined magnesia；
B) modifying agent is added into ultrasonic disperse in ethanol and is made into modifier solution；Wherein described modifying agent is stearic acid, aluminic acid
One or more in ester coupling agent H-3, stearic acid sodium or zinc stearate；
C) it is 1 in mass ratio by light calcined magnesia, magnesium salts, water, dispersant：(0.02~4.5)：(10~100)：(0.03~
0.5), it is well mixed with the step b) modifier solutions being made into, obtains suspension, suspension ultrasonic disperse is uniform, in stirring
Under the conditions of, in after 50 DEG C~100 DEG C of water bath with thermostatic control, 2~6h of reaction, add crystal seed and activating agent；
D) step c) reaction solutions are aged；
E) in step d) reaction product through filtering, washing, be dried to obtain fibrous magnesium hydroxide.
2. in accordance with the method for claim 1, it is characterised in that in step a) calcining heat of magnisite be 600 DEG C~
1250℃；Calcination time is 2~6h.
3. in accordance with the method for claim 1, it is characterised in that the ratio of the quality of modifying agent and ethanol volume in step b)
For 1：(10~100) g/ml.
4. in accordance with the method for claim 1, it is characterised in that the addition of modifier solution is modified for control in step c)
The addition quality of agent is the 1%~10% of light calcined magnesia quality.
5. in accordance with the method for claim 1, it is characterised in that described dispersant is polyvinylpyrrolidone, cetyl
The one or more of trimethylammonium bromide or PEG-400；Magnesium salts is magnesium sulfate.
6. the method as described in claim 1, it is characterised in that described crystal seed is basic magnesium chloride whisker, alkali magnesium sulfate crystalline substance
Palpus or magnesium hydroxide crystal whisker；Crystal seed adds 0.8%~50% that quality is light calcined magnesia quality.
7. in accordance with the method for claim 1, it is characterised in that described activating agent is ethylenediamine, propane diamine, butanediamine, three
The one or more of ethamine or hexa.
8. the method as described in claim 1, it is characterised in that the volume of activating agent addition and the ratio of magnesia quality are
0.007~0.15ml/g.
9. in accordance with the method for claim 1, it is characterised in that the Aging Temperature in step d) is 5 DEG C~50 DEG C, during ageing
Between be 2~10 days.
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| CN108752980A (en) * | 2018-05-16 | 2018-11-06 | 唐山师范学院 | The preparation method of modified magnesium hydroxide flame retardant agent and modified magnesium hydroxide flame retardant agent |
| CN113213511A (en) * | 2021-06-21 | 2021-08-06 | 马鞍山市安工大工业技术研究院有限公司 | Method for recovering high-purity magnesium oxide by taking ethyl maltol waste residue as raw material |
| CN113979455A (en) * | 2021-11-10 | 2022-01-28 | 大连交通大学 | Preparation method and application of flaky superfine magnesium hydroxide |
| CN114318367B (en) * | 2022-01-10 | 2023-10-27 | 东莞理工学院 | High-dispersion modified nano magnesium hydroxide and preparation method thereof |
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| JP2007016153A (en) * | 2005-07-08 | 2007-01-25 | Konoshima Chemical Co Ltd | Magnesium hydroxide-based flame retardant with high heat resistance, flame retardant resin composition and molded product |
| JP2009517328A (en) * | 2005-11-28 | 2009-04-30 | マーティン マリエッタ マテリアルズ，インコーポレイテッド | Flame retardant magnesium hydroxide composition and related methods of manufacture and use |
| CN102502726B (en) * | 2011-10-28 | 2013-12-25 | 南京工业大学 | Preparation method for hexagonal sheet magnesium hydroxide |
| WO2013121412A1 (en) * | 2012-02-15 | 2013-08-22 | Bromine Compounds Ltd. | Flame-retarded compositions of polyamides |
| CN103849924B (en) * | 2014-02-12 | 2016-06-29 | 沈阳理工大学 | A kind of method utilizing alkali magnesium sulfate crystal whisker to prepare nano-sized magnesium hydroxide whisker |
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