CN101318673A - Method for preparing magnesium hydroxide with microemulsion in phase opposition - Google Patents
Method for preparing magnesium hydroxide with microemulsion in phase opposition Download PDFInfo
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- CN101318673A CN101318673A CNA2008100553911A CN200810055391A CN101318673A CN 101318673 A CN101318673 A CN 101318673A CN A2008100553911 A CNA2008100553911 A CN A2008100553911A CN 200810055391 A CN200810055391 A CN 200810055391A CN 101318673 A CN101318673 A CN 101318673A
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- microemulsion
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- ammonia
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Abstract
The invention discloses a method for preparing magnesium hydroxide by a reversed phase single micro-emulsion. The method adopts a new preparation process; after selection of the raw chemical substances, a surfactant polyethylene glycol octyl phenyl ether, a cosurfactant n-hexyl alcohol, the oil-phase cyclohexane, and the aqueous-phase magnesium chloride water solution are placed in a flask for stirring and mixing to gain a clear reversed phase single micro-emulsion; the micro-emulsion is added with ammonia gas to adjust the pH value until the micro-emulsion is alkaline, and a white emulsion is gained after reaction and becomes a clear precipitate after heating and emulsion breaking, the clear precipitate is filtered under the vacuum state, washed and filtered by deionized water and absolute ethyl alcohol, dried under minus 55 DEG C frozen state and 15Pa vacuum state, ground, sieved by a 625-mesh sieve, and the white, flakelike, crystalline, and nano-sized magnesium hydroxide powder is obtained. The method has the advantages of less equipment requirement, short technological process and no environmental pollution; the product yield is up to 97%, the product purity is up to 98%, the product has high precision, the powder has the average particle size of 80nm and the average thickness of 20nm, good thermal stability, 353 DEG C initial decomposition temperature, reaches the maximum decomposition rate at the temperature of 387 DEG C, and can match a plurality of organic matters to prepare a plurality of fire retardant materials.
Description
Technical field
The present invention relates to a kind of method, belong to the technical field of inorganics bases compound fire retardant material preparation method with preparing magnesium hydroxide with microemulsion in phase opposition.
Background technology
At modern industrial circle, fire-retardant have a special using value with fire prevention, and the quality of fire retardant material is producing different effects in fire prevention, in fire-retardant.
Magnesium hydroxide is one of fire-retardant interpolation material of inorganic system, compare with similar inorganic series flame retardant material, having and better press down the cigarette effect, mostly is to be suffocated and caused loss of life and personal injury by cigarette in the fire, in flame-retarded technology, press down cigarette and fire-retardant be crucial, the existing flame retardant resistance of magnesium hydroxide has smoke-suppressing again, in use discharge harmful not, can also neutralize aflame acidity and corrosive gases are the environment-friendly fire retardants.
How to prepare magnesium hydroxide, the problem that has become science and technology field research and inquired into, its preparation method also has various ways, but because chemical feedstocks difference, the test conditions difference, preparation synthetic technical process difference, the parameter difference makes the method for producing magnesium hydroxide that multiple pros and cons also arranged, the complex process that has is difficult to be realized, the inferior production yield rate of the starting material that have is low, and the building-up process that has is seriously polluted, easily generates by product, the product precision of producing that has is low, with other chemical substance coupling difficulties, be difficult to use, its preparation method exists not enough.
In the preparation of nano material, a kind of microemulsion preparation method is arranged, be used to prepare nano particles such as metal, muriate, oxide compound, carbide, oxyhydroxide.
Emulsion is divided into microemulsion, miniemulsion and ordinary emulsion, microemulsion is with respect to miniemulsion, ordinary emulsion, with two kinds of immiscible liquid formed isotropic under Action of Surfactant, the dispersion system of appearance transparent is called microemulsion, the microemulsion droplets diameter is at 10～100nm, the miniemulsion droplet dia is at 100～400nm, the ordinary emulsion droplet dia is at 400～1000nm, microemulsion is best suited in the reaction medium of preparation nano material, divide the O/W type again, it is oil-in-water-type, w/o type, it is water-in-oil-type, be also referred to as reverse micro emulsion, also have a kind of osculant transition phase, be called the co-continuous phase structure, form the netted cross structure of oil phase+water, single microemulsion method is a kind of reactive material wherein to be made microemulsion react, and two microemulsion methods are two kinds of reactive material all to be made microemulsion react, and prepare Mg (OH) with single microemulsion method
2Yet there are no report, still a scientific research blank.
Summary of the invention
Goal of the invention
Purpose of the present invention is exactly at disadvantages of background technology, adopt a kind of microemulsion in phase opposition legal system of brand-new water-in-oil-type to be equipped with magnesium hydroxide, by configuration magnesium chloride microemulsion, adjusting potential of hydrogen, constant temperature stirring, breakdown of emulsion, vacuum filtration, washing, vacuum lyophilization, grinding, make the magnesium hydroxide crystal powder, to increase substantially degree of purity of production, precision, production yield rate and flame retardant properties.
Technical scheme
The chemical substance material that the present invention uses is: Magnesium dichloride hexahydrate, and polyoxyethylene glycol octyl phenol ether, n-hexyl alcohol, hexanaphthene, dehydrated alcohol, deionized water, ammonia, its combination matching amount is: with gram, milliliter, centimetre
3Be measure unit
Magnesium dichloride hexahydrate: MgCl
26H
2O 3.0495g ± 0.0005g
Polyoxyethylene glycol octyl phenol ether TX-100:C
34H
62O
1118.6ml ± 0.5ml
N-hexyl alcohol: C
6H
14O 18.6ml ± 0.5ml
Hexanaphthene: C
6H
1240g ± 0.0005g
Dehydrated alcohol: CH
3CH
2OH 200ml ± 5ml
Deionized water: H
2O 1000ml ± 5ml
Ammonia: NH
31000cm
3± 5cm
3
It is as follows to produce synthetic method:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out control of purity:
Magnesium dichloride hexahydrate: solid-state 〉=99.0%
Polyoxyethylene glycol octyl phenol ether TX-100: liquid 〉=99.0%
N-hexyl alcohol: liquid 〉=99.5%
Hexanaphthene: liquid 〉=99.5%
Dehydrated alcohol: liquid 〉=99.7%
Deionized water: liquid 99.999%
Ammonia: gaseous state 〉=99.9%
(2) preparation magnesium chloride brine
Take by weighing magnesium chloride 3.0495g ± 0.0005g, deionized water 22ml ± 1ml, place beaker, under 25 ℃ ± 1 ℃ temperature, on magnetic stirring apparatus, stir 5min ± 1min, become magnesium chloride brine, magnesium chloride brine concentration 0.6mol/L;
(3) preparation microemulsion in phase opposition
1. in four-hole boiling flask, carry out;
2. with surfactant polyethylene octyl phenol ether 18.6ml ± 0.5ml, cosurfactant n-hexyl alcohol 18.6ml ± 0.5ml places four-hole boiling flask, and its volume ratio is 1: 1;
3. oil phase hexanaphthene 40g ± 0.0005g is added in the four-hole boiling flask;
4. magnesium chloride brine 24ml ± 1ml is added in the four-hole boiling flask;
5. inlet pipe, the escape pipe with the ammonia bottle inserts in the four-hole boiling flask respectively;
6. electric mixer is placed four-hole boiling flask;
7. four-hole boiling flask is placed on the well heater;
8. turn on agitator stirs, time 30min ± 2min;
9. open the ammonia bottle, the input ammonia, input speed is 5cm
3/ min;
10. under agitator stirs, under 25 ℃ ± 1 ℃ temperature of room temperature, surfactant polyethylene octyl phenol ether in the four-hole boiling flask, cosurfactant n-hexyl alcohol, oil phase hexanaphthene, magnesium chloride brine form the clear microemulsion through stirring, the ammonia of magnesium chloride and feeding reacts, and reaction equation is as follows:
In the formula:
MgCl
2: magnesium chloride
Mg (OH)
2: magnesium hydroxide
NH
4Cl: ammonium chloride
The hydroxyl on surfactant polyethylene octyl phenol ether TX-100 and magnesium hydroxide surface interacts, and generates hydrogen bond, and reaction formula is as follows:
In the formula:
OH: hydroxyl
In four-hole boiling flask, extract the 1ml mixed solution and place on the precision test paper, carry out the acidity-basicity ph pH-value determination pH, when pH=11, close the ammonia bottle, stop defeated ammonia;
(4) heating demulsification type is collected product
1. four-hole boiling flask is placed on the well heater, heater heats up it, and the mixed solution in the four-hole boiling flask is risen to 60 ℃ ± 1 ℃;
2. continue to stir 10min ± 1min;
3. white emulsion becomes clarification+precipitation state, and this moment, single microemulsion was abolished, became: clarification+precipitation mixed solution, that is: magnesium hydroxide product mixed solution;
(5) vacuum filtration
With clarification+sedimentary magnesium hydroxide product mixed solution that breakdown of emulsion makes, place and carry out suction filtration on the vacuum filtration bottle, with two-layer qualitative filter paper at a slow speed, suction filtration time 10min ± 1min obtains the magnesium hydroxide product filter cake on qualitative filter paper;
(6) deionized water wash, filtration are ten times
The magnesium hydroxide product filter cake is placed beaker, add deionized water 20ml ± 1ml,, become mixed solution with agitator agitator treating 5min;
After the washing mixed solution is placed B, filter, stay the magnesium hydroxide product filter cake on the filter paper with two-layer qualitative filter paper;
Deionized water wash, filtration repeat ten times;
(7) absolute ethanol washing, filtration are three times
Magnesium hydroxide filter cake behind the deionized water wash is placed beaker, add dehydrated alcohol 10ml ± 1ml,, become: the magnesium hydroxide alcohol mixeding liquid with agitator agitator treating 5min;
After the washing mixed solution is placed B, filter, stay the magnesium hydroxide product filter cake on the filter paper with two-layer qualitative filter paper;
Absolute ethanol washing, filtration repeat three times;
(8) vacuum lyophilization
1. deionized water wash, filtration, absolute ethanol washing, filtering magnesium hydroxide product filter cake are placed glassware;
2. glassware is placed vacuum freezing drying oven, and sealing; Open refrigerator, make the freeze drying box temperature reduce to-55 ℃ ± 1 ℃, freezing 180min ± 5min by 20 ℃ ± 3 ℃;
Open vacuum pump, extract the gas in the freeze drying box out, vacuum tightness is 15Pa in the loft drier;
Under vacuum state, under freezing state, magnesium hydroxide filtration cakes torrefaction 1440min ± 20min;
After vacuum, the lyophilize, get product: magnesium hydrate powder;
(9) grind, sieve
Magnesium hydrate powder after vacuum, the lyophilize is placed agate mortar, grind, sieve with 625 eye mesh screens then with agate pestle;
Grind, sieving repeats, finally make: hydrophobicity, nano level, white, sheet, magnesium hydroxide crystal formation powder;
(10) detect, chemically examine, analyze, characterize, contrast
Pattern, color and luster, performance, composition, purity, precision, thermostability to the magnesium hydrate powder of white, the sheet of preparation, loose shape detect, chemically examine, analyze, characterize, contrast;
With X-ray diffractometer assay products crystalline structure;
Carry out morphology analysis with field emission scanning electron microscope, acceleration voltage is 10kV;
With grinding after product crystal formation powder and the Potassium Bromide KBr dry powder blend, be pressed into transparent sheet then, carry out Infrared spectroscopy with infrared spectrometer;
With thermogravimetric analyzer product crystal formation powder is carried out thermogravimetric analysis, be raised to 700 ℃ from 25 ℃ of room temperatures, nitrogen atmosphere keeps the temperature rise rate of 10 ℃/min to analyze down;
(11) store
Magnesium hydroxide white, sheet, crystal formation powder are placed water white Glass Containers, and clean environment is wanted waterproof, protection against the tide, acid-proof, alkali, salt corrosion, 20 ℃ ± 3 ℃ of storing temps, relative humidity≤20%.
The described preparing magnesium hydroxide with microemulsion in phase opposition of using is with Magnesium dichloride hexahydrate MgCl
26H
2O is a raw material, with polyoxyethylene glycol octyl phenol ether C
34H
62O
11Be tensio-active agent, with n-hexyl alcohol C
6H
14O is a cosurfactant, with hexanaphthene C
6H
12Being oil phase, is water with the magnesium chloride brine, is acidity-basicity ph value alkaline conditioner with the ammonia, is product magnesium hydroxide washing composition with deionized water, dehydrated alcohol.
The drying of described magnesium hydroxide product is to be under the 15Pa state, to carry out under-55 ℃ ± 1 ℃ freezing state in vacuum tightness, freezing time 180min ± 5min, and be 1440min ± 20min time of drying.
The quaternary of described microemulsion in phase opposition is mutually: surfactant polyethylene octyl phenol ether, the cosurfactant n-hexyl alcohol, the oil phase hexanaphthene, the water magnesium chloride brine, wherein: polyoxyethylene glycol octyl phenol ether is that tensio-active agent, n-hexyl alcohol are cosurfactant, hexanaphthene is an oil phase, and magnesium chloride brine is a water, is the transparence clear liquor.
The phase region mass ratio of described microemulsion in phase opposition is: hexanaphthene: polyoxyethylene glycol octyl phenol ether+n-hexyl alcohol: magnesium chloride brine=40: 35: 25.
The magnesium hydroxide product of described microemulsion in phase opposition preparation is: hydrophobicity, nano level, white, sheet, crystal formation, powder.
Described preparation microemulsion in phase opposition, breakdown of emulsion, syntheticly in four-hole boiling flask, carry out, four-hole boiling flask 1 is placed on the well heater 2, well heater 2 is provided with temperature regulator 9, four-hole boiling flask 1 top is provided with ammonia pipe 7, addition funnel 4, agitator 3, escape pipe 8 from left to right, ammonia pipe 7 connects ammonia valve 6, ammonia bottle 5, four-hole boiling flask 1 inner bottom part is polyoxyethylene glycol octyl phenol ether+n-hexyl alcohol+hexanaphthene+magnesium chloride+deionized water mixed solution 11, and four-hole boiling flask 1 internal upper part is an ammonia 10.
Beneficial effect
The present invention compares with background technology has tangible advance, adopted brand-new preparation technology's flow process, carry out selected to required chemical substance, and carry out control of purity, prepare magnesium chloride brine earlier, refabrication list microemulsion, with surfactant polyethylene octyl phenol ether, the cosurfactant n-hexyl alcohol, the oil phase hexanaphthene, the water magnesium chloride brine places flask to mix, by the input ammonia, with gaseous ammonia controlled atmosphere joint acidity-basicity ph value is alkalescence, by stirring, carry out chemical reaction, become white emulsion by clarifying microemulsion in phase opposition, be heated to 60 ℃ ± 1 ℃, breakdown of emulsion, white emulsion becomes clarification+precipitation state by cloudy state, again through vacuum filtration, ten washings of deionized water, three washings of dehydrated alcohol, filter repeatedly, under-55 ℃ of freezing states, under the vacuum state of 15Pa, carry out drying, after grind, 625 eye mesh screens sieve, make white, sheet, crystal formation, powder, nano level, the hydrophobicity magnesium hydroxide product, this method uses equipment few, and technical process is short, and is free from environmental pollution, the production yield rate height, can reach 97%, the product purity height can reach 98%, white plates crystal median size is 80nm, thickness is 20nm, its product magnesium hydroxide Heat stability is good, and temperature of initial decomposition is 353 ℃, temperature was 387 ℃ when rate of decomposition was maximum, the end of a period decomposition temperature is 401 ℃, can mate with multiple organism, makes multiple fire retardant material.
Description of drawings
Fig. 1 is preparation technology's schema
Fig. 2 is preparation microemulsion in phase opposition, breakdown of emulsion, synthetic state figure
Fig. 3 is the state graph of breakdown of emulsion solution for vacuum suction filtration
Fig. 4 is the state graph of product vacuum lyophilization
Fig. 5 amplifies 30000 times of shape appearance figures for magnesium hydroxide product
Fig. 6 is a magnesium hydroxide product diffracted intensity collection of illustrative plates
Fig. 7 is the magnesium hydroxide product infrared spectra
Fig. 8 is magnesium hydroxide product thermal weight loss-differential thermal curve figure
Shown in the figure, list of numerals is as follows:
1. four-hole boiling flask, 2. well heater, 3. agitator, 4. addition funnel, 5. ammonia bottle, 6. ammonia valve, 7. ammonia pipe, 8. escape pipe, 9. temperature regulator, 10. ammonia, 11. polyoxyethylene glycol octyl phenol ether+n-hexyl alcohol+hexanaphthene+magnesium chloride+deionized water mixed solutions, 12. filter flasks, 13. the cone seal plug, 14. Bs, 15. vacuum pumps, 16. clarification+precipitation breakdown of emulsion liquid, 17. filter paper, 18. waste liquids, 19. the product filter cake, 20. refrigerators, 21. refrigeration controlers, 22. vacuum chamber, 23. product boats, 24. magnesium hydroxide product, 25. vacuum pump, 26. valve tube, 27. vacuum valves, 28. vacuum freezing drying ovens.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, be preparation technology's schema, carry out in strict accordance with technical process and parameter, according to the order of sequence operation.
The chemical substance material that uses in preparation process is to determine in the numerical range that sets in advance, with gram, milliliter, centimetre
3Be measure unit, when industrialization is produced with kilogram, liter, rice
3Be measure unit.
Prepare required four-hole boiling flask, agitator, dropping funnel, ammonia pipe, vacuum filtration bottle, container, vacuum freezing drying oven, mortar, filter paper etc. and will keep clean, must not have impurity to get involved, in order to avoid generate by product.
The emulsion that this preparation is used is water in oil microemulsion in phase opposition, i.e. w/o type, and W is a water, O is an oil phase, and the magnesium chloride microemulsion is single microemulsion, also has a kind of method that magnesium chloride and alkaline precipitating agent are all made microemulsion and reacts, promptly two microemulsions, two microemulsions are not adopted in this preparation.
The surfactant polyethylene octyl phenol ether that this preparation is used and the volume ratio of cosurfactant n-hexyl alcohol are 1: 1, strict its ratio of control.
Hexanaphthene: polyoxyethylene glycol octyl phenol ether+n-hexyl alcohol: the mass ratio of magnesium chloride brine is 40: 35: 25, strict this ratio of control, otherwise will influence the productive rate of magnesium hydroxide.
Shown in Figure 2, be preparation microemulsion in phase opposition, breakdown of emulsion, synthetic state figure, mixing solutions 11 adds by dropping funnel 4 in the four-hole boiling flask 1, ammonia 10 is by 7 inputs of ammonia pipe, and by ammonia valve 6 its inpuies of control, ammonia 10 enters four-hole boiling flask and executes alkali, adjusts the pH value, unnecessary gas is discharged by escape pipe 8, electric mixer 3 evenly stirs, and wants heater 2 during breakdown of emulsion, and by temperature in the temperature controller control four-hole boiling flask at 60 ℃ ± 1 ℃.
Shown in Figure 3, be the state graph of breakdown of emulsion solution for vacuum suction filtration, cone seal plug 13 is equipped with on filter flask 12 tops, cone seal plug 13 tops are B 14, filter paper 17, the right side is vacuum pump 15, clarification+precipitation breakdown of emulsion mixed solution 16 is housed in the B 14, and vacuum filtration stays filter cake 19 in B 14, and waste liquid 18 is evacuated to filter flask 12 inner bottom parts.
Shown in Figure 4, be the state graph of product vacuum lyophilization, be vacuum freezing drying oven 28 on refrigerator 20 tops, it in vacuum freezing drying oven 28 vacuum chamber 22, vacuum intracavity holding product boat 23 and product magnesium hydroxide 24 are provided with vacuum valve 27, valve tube 26, vacuum pump 25 at vacuum freezing drying oven 28 left parts, and the vacuum tightness in the vacuum chamber 22 is 15Pa, by vacuum valve 27 controls ,-55 ℃ freezing temp in the vacuum chamber 22 is by refrigeration controler 21 controls.
Shown in Figure 5, be that the field emission scan amplifies 30000 times of product shape appearance figures, among the figure as can be known: product is white, sheet, crystal formation, powder, is irregular alignment, and median size is 80nm, and thickness is 20nm, ruler units 100nm.
Shown in Figure 6, be product crystalline diffraction intensity collection of illustrative plates, X-coordinate is diffraction angle 2 θ, ordinate zou is the diffracted intensity index, its diffraction peak is successively corresponding to (001), (100), (101), (102), (110), (111), (103), (201) crystal face of magnesium hydroxide crystal, among the figure as can be known: the pairing diffraction peak intensity maximum of (001) crystal face, the ratio of the diffracted intensity of (001) crystal face and (110) crystal face is 5, shows that product is a flaky powder.
Shown in Figure 7, be the magnesium hydroxide product infrared spectra, X-coordinate is a wave number, ordinate zou is a transmitance, among the figure as can be known: variation has taken place in the infrared spectra before and after the product alcohol washing, a curve for washing before spectrum, b can be found out by a, b curve: 3699cm for washing back spectrum
-1The spike at place is corresponding to the stretching vibration of the O-H key in the magnesium hydroxide crystal structure, 441cm
-1The wide strong peak at place is corresponding to the Mg-O stretching vibration of magnesium hydroxide, and 2926 and 2856cm
-1The small peak at place belongs to methylene radical-CH respectively
2Asymmetric and symmetric vibration peak, by the b curve as can be seen: after washing through alcohol, the characteristic peak of polyoxyethylene glycol octyl phenol ether TX100 still keeps, i.e. 1635cm
-1The phenyl ring skeletal vibration peak υ at place
C=c, 1116cm
-1The place
-O stretching vibration peak and 1055cm
-1The C-O stretching vibration peak at place, 3427cm
-1The peak of the medium tenacity at place belongs to the OH stretching vibration of intermolecular hydrogen bonding between magnesium hydroxide and the tensio-active agent, the increase of magnesium hydroxide characteristic peak relative intensity shows that alcohol is washed and most of organic phase can be washed, remaining a part of tensio-active agent then combines in the hydrogen bond mode with magnesium hydroxide particles, remain in nanoparticle surface, help to improve dispersiveness and the consistency of nanoparticle in macromolecule matrix.
Shown in Figure 8, be magnesium hydroxide product thermostability graphic representation, X-coordinate is a temperature value, and the ordinate zou left part is weight percentage, right part is heat flux, upwards expression heat absorption of arrow, arrow is represented heat radiation downwards, among the figure as can be known: the initial decomposition temperature of product is 353 ℃, and the end of a period decomposition temperature is 401 ℃, and weight loss is decomposed into magnesium oxide corresponding to magnesium hydroxide, the decomposition of magnesium hydroxide is an endothermic process, reaches maximum at 387 ℃ of rate of decomposition.
Claims (8)
1, a kind of method with preparing magnesium hydroxide with microemulsion in phase opposition, it is characterized in that: the chemical substance material of use is: Magnesium dichloride hexahydrate, polyoxyethylene glycol octyl phenol ether, n-hexyl alcohol, hexanaphthene, dehydrated alcohol, deionized water, ammonia, its combination matching amount is: with gram, milliliter, centimetre
3Be measure unit.
Magnesium dichloride hexahydrate: MgCl
26H
2O 3.0495g ± 0.0005g
Polyoxyethylene glycol octyl phenol ether TX-100:C
34H
62O
1118.6ml ± 0.5ml
N-hexyl alcohol: C
6H
14O 18.6ml ± 0.5ml
Hexanaphthene: C
6H
1240g ± 0.0005g
Dehydrated alcohol: CH
3CH
2OH 200ml ± 5ml
Deionized water: H
2O 1000ml ± 5ml
Ammonia: NH
31000cm
3± 5cm
3
It is as follows to produce synthetic method:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out control of purity:
Magnesium dichloride hexahydrate: solid-state 〉=99.0%
Polyoxyethylene glycol octyl phenol ether TX-100: liquid 〉=99.0%
N-hexyl alcohol: liquid 〉=99.5%
Hexanaphthene: liquid 〉=99.5%
Dehydrated alcohol: liquid 〉=99.7%
Deionized water: liquid 99.999%
Ammonia: gaseous state 〉=99.9%
(2) preparation magnesium chloride brine
Take by weighing magnesium chloride 3.0495g ± 0.0005g, deionized water 22ml ± 1ml, place beaker, under 25 ℃ ± 1 ℃ temperature, on magnetic stirring apparatus, stir 5min ± 1min, become magnesium chloride brine, magnesium chloride brine concentration 0.6mol/L;
(3) preparation microemulsion in phase opposition
1. in four-hole boiling flask, carry out;
2. with surfactant polyethylene octyl phenol ether 18.6ml ± 0.5ml, cosurfactant n-hexyl alcohol 18.6ml ± 0.5ml places four-hole boiling flask, and its volume ratio is 1: 1;
3. oil phase hexanaphthene 40g ± 0.0005g is added in the four-hole boiling flask;
4. magnesium chloride brine 24ml ± 1ml is added in the four-hole boiling flask;
5. inlet pipe, the escape pipe with the ammonia bottle inserts in the four-hole boiling flask respectively;
6. electric mixer is placed four-hole boiling flask;
7. four-hole boiling flask is placed on the well heater;
8. turn on agitator stirs, time 30min ± 2min;
9. open the ammonia bottle, the input ammonia, input speed is 5cm
3/ min;
10. under agitator stirs, under 25 ℃ ± 1 ℃ temperature of room temperature, surfactant polyethylene octyl phenol ether in the four-hole boiling flask, cosurfactant n-hexyl alcohol, oil phase hexanaphthene, magnesium chloride brine form the clear microemulsion through stirring, the ammonia of magnesium chloride and feeding reacts, and reaction equation is as follows:
In the formula:
MgCl
2: magnesium chloride
Mg (OH)
2: magnesium hydroxide
NH
4Cl: ammonium chloride
The hydroxyl on surfactant polyethylene octyl phenol ether TX-100 and magnesium hydroxide surface interacts, and generates hydrogen bond, and reaction formula is as follows:
In the formula:
OH: hydroxyl
In four-hole boiling flask, extract the 1ml mixed solution and place on the precision test paper, carry out the acidity-basicity ph pH-value determination pH, when pH=11, close the ammonia bottle, stop defeated ammonia;
(4) heating demulsification type is collected product
1. four-hole boiling flask is placed on the well heater, heater heats up it, and the mixed solution in the four-hole boiling flask is risen to 60 ℃ ± 1 ℃;
2. continue to stir 10min ± 1min
3. white emulsion becomes clarification+precipitation state, and this moment, single microemulsion was abolished, became: clarification+precipitation mixed solution, that is: magnesium hydroxide product mixed solution;
(5) vacuum filtration
With clarification+sedimentary magnesium hydroxide product mixed solution that breakdown of emulsion makes, place and carry out suction filtration on the vacuum filtration bottle, with two-layer qualitative filter paper at a slow speed, suction filtration time 10min ± 1min obtains the magnesium hydroxide product filter cake on qualitative filter paper;
(6) deionized water wash, filtration are ten times
The magnesium hydroxide product filter cake is placed beaker, add deionized water 20ml ± 1ml,, become mixed solution with agitator agitator treating 5min;
After the washing mixed solution is placed B, filter, stay the magnesium hydroxide product filter cake on the filter paper with two-layer qualitative filter paper;
Deionized water wash, filtration repeat ten times;
(7) absolute ethanol washing, filtration are three times
Magnesium hydroxide filter cake behind the deionized water wash is placed beaker, add dehydrated alcohol 10ml ± 1ml,, become: the magnesium hydroxide alcohol mixeding liquid with agitator agitator treating 5min;
After the washing mixed solution is placed B, filter, stay the magnesium hydroxide product filter cake on the filter paper with two-layer qualitative filter paper;
Absolute ethanol washing, filtration repeat three times;
(8) vacuum lyophilization
1. deionized water wash, filtration, absolute ethanol washing, filtering magnesium hydroxide product filter cake are placed glassware;
2. glassware is placed vacuum freezing drying oven, and sealing; Open refrigerator, make the freeze drying box temperature reduce to-55 ℃ ± 1 ℃, freezing 180min ± 5min by 20 ℃ ± 3 ℃;
Open vacuum pump, extract the gas in the freeze drying box out, vacuum tightness is 15Pa in the loft drier;
Under vacuum state, under freezing state, magnesium hydroxide filtration cakes torrefaction 1440min ± 20min;
After vacuum, the lyophilize, get product: magnesium hydrate powder;
(9) grind, sieve
Magnesium hydrate powder after vacuum, the lyophilize is placed agate mortar, grind, sieve with 625 eye mesh screens then with agate pestle;
Grind, sieving repeats, finally make: hydrophobicity, nano level, white, sheet, magnesium hydroxide crystal formation powder;
(10) detect, chemically examine, analyze, characterize, contrast
Pattern, color and luster, performance, composition, purity, precision, thermostability to the magnesium hydrate powder of white, the sheet of preparation, loose shape detect, chemically examine, analyze, characterize, contrast;
With X-ray diffractometer assay products crystalline structure;
Carry out morphology analysis with field emission scanning electron microscope, acceleration voltage is 10kV;
With grinding after product crystal formation powder and the Potassium Bromide KBr dry powder blend, be pressed into transparent sheet then, carry out Infrared spectroscopy with infrared spectrometer;
With thermogravimetric analyzer product crystal formation powder is carried out thermogravimetric analysis, be raised to 700 ℃ from 25 ℃ of room temperatures, nitrogen atmosphere keeps the temperature rise rate of 10 ℃/min to analyze down;
(11) store
Magnesium hydroxide white, sheet, crystal formation powder are placed water white Glass Containers, and clean environment is wanted waterproof, protection against the tide, acid-proof, alkali, salt corrosion, 20 ℃ ± 3 ℃ of storing temps, relative humidity≤20%.
2, a kind of method with preparing magnesium hydroxide with microemulsion in phase opposition according to claim 1, it is characterized in that: the described preparing magnesium hydroxide with microemulsion in phase opposition of using is with Magnesium dichloride hexahydrate MgCl
26H
2O is a raw material, with polyoxyethylene glycol octyl phenol ether C
34H
62O
11Be tensio-active agent, with n-hexyl alcohol C
6H
14O is a cosurfactant, with hexanaphthene C
6H
12Being oil phase, is water with the magnesium chloride brine, is acidity-basicity ph value alkaline conditioner with the ammonia, is product magnesium hydroxide washing composition with deionized water, dehydrated alcohol.
3, a kind of method according to claim 1 with preparing magnesium hydroxide with microemulsion in phase opposition, it is characterized in that: the drying of described magnesium hydroxide product, be to be under the 15Pa state, under-55 ℃ ± 1 ℃ freezing state, to carry out in vacuum tightness, freezing time 180min ± 5min, be 1440min ± 20min time of drying.
4, a kind of method according to claim 1 with preparing magnesium hydroxide with microemulsion in phase opposition, it is characterized in that: the quaternary of described microemulsion in phase opposition is mutually: surfactant polyethylene octyl phenol ether, the cosurfactant n-hexyl alcohol, the oil phase hexanaphthene, the water magnesium chloride brine, wherein: polyoxyethylene glycol octyl phenol ether is that tensio-active agent, n-hexyl alcohol are cosurfactant, and hexanaphthene is an oil phase, magnesium chloride brine is a water, is the transparence clear liquor.
5, a kind of method with preparing magnesium hydroxide with microemulsion in phase opposition according to claim 1, it is characterized in that: the phase region mass ratio of described microemulsion in phase opposition is: hexanaphthene: polyoxyethylene glycol octyl phenol ether+n-hexyl alcohol: magnesium chloride brine=40: 35: 25.
6, a kind of method with preparing magnesium hydroxide with microemulsion in phase opposition according to claim 1, it is characterized in that: the magnesium hydroxide product of described microemulsion in phase opposition preparation is: hydrophobicity, nano level, white, sheet, crystal formation, powder.
7, a kind of method according to claim 1 with preparing magnesium hydroxide with microemulsion in phase opposition, it is characterized in that: described preparation microemulsion in phase opposition, breakdown of emulsion, synthesize and in four-hole boiling flask, carry out, four-hole boiling flask (1) is placed on the well heater (2), well heater (2) is provided with temperature regulator (9), four-hole boiling flask (1) top is provided with ammonia pipe (7) from left to right, addition funnel (4), agitator (3), escape pipe (8), ammonia pipe (7) connects ammonia valve (6), ammonia bottle (5), four-hole boiling flask (1) inner bottom part is polyoxyethylene glycol octyl phenol ether+n-hexyl alcohol+hexanaphthene+magnesium chloride+deionized water mixed solution (11), and four-hole boiling flask (1) internal upper part is ammonia (10).
8, a kind of method according to claim 1 with preparing magnesium hydroxide with microemulsion in phase opposition, it is characterized in that: the initial decomposition temperature of described magnesium hydroxide product is 353 ℃, the end of a period decomposition temperature is 401 ℃, weight loss is decomposed into magnesium oxide corresponding to magnesium hydroxide, the decomposition of magnesium hydroxide is an endothermic process, reaches maximum at 387 ℃ of rate of decomposition.
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| CN110372022A (en) * | 2019-06-26 | 2019-10-25 | 河海大学 | Macroscopical 3D multistage porous nanometer material one-step method for synthesizing |
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