CN107337187B - A kind of preparation method of nanometer of hypo-aluminum orthophosphate - Google Patents
A kind of preparation method of nanometer of hypo-aluminum orthophosphate Download PDFInfo
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- CN107337187B CN107337187B CN201710598598.2A CN201710598598A CN107337187B CN 107337187 B CN107337187 B CN 107337187B CN 201710598598 A CN201710598598 A CN 201710598598A CN 107337187 B CN107337187 B CN 107337187B
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/165—Hypophosphorous acid; Salts thereof
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Abstract
The invention discloses the preparation methods of a kind of nanometer of hypo-aluminum orthophosphate, the following steps are included: sodium hypophosphite aqueous solution and cetyl trimethylammonium bromide a) are added in organic continuous phases solvent, the reverse micro emulsion that the Water-In-Oil containing sodium hypophosphite is made, referred to as A liquid are reacted under the conditions of 50-95 DEG C；B) aqueous aluminum salt solution and cetyl trimethylammonium bromide are added in organic continuous phases solvent, the reverse micro emulsion that the Water-In-Oil of containing water-soluble aluminium salt is made, referred to as B liquid are reacted under the conditions of 50-95 DEG C；C) B liquid is slowly instilled in A liquid under strong stirring action, the molar ratio of sodium hypophosphite and water-soluble aluminum salt is adjusted under 80-95 DEG C of normal pressure, is heated to reflux, reacted in nanometer micro-emulsion reactor and nanometer hypo-aluminum orthophosphate colloid is made；D) it separates, nanometer hypo-aluminum orthophosphate powder is made in purifying and drying nano hypo-aluminum orthophosphate colloid.This method prepares uniform and stable nanometer hypo-aluminum orthophosphate using reverse microemulsion process, solves the deficiency of existing method and technique.
Description
Technical field
The present invention relates to the preparation methods of a kind of nanometer of hypo-aluminum orthophosphate, belong to technical field of nanometer material preparation.
Background technique
Hypo-aluminum orthophosphate is because of the advantages that its phosphorus content is high, thermal stability is good, synthesis technology is relatively easy and price is relatively cheap
It is widely used in flame retardant area.It can promote the charing of polymer in combustion process, realize that condensed phase is fire-retardant, can also be with it
He compounds fire retardant, plays the effect of synergistic effect, improves flame retardant effect.People have carried out various grind to hypo-aluminum orthophosphate
Study carefully, mainly have:
(1) new method and technique of hypo-aluminum orthophosphate preparation.Such as the application for a patent for invention text of Publication No. CN104163412A
It is disclosed in part by sodium hypophosphite and soluble aluminum reactant salt, separates hypo-aluminum orthophosphate crystal, mother liquor Returning reactor is continuous to prepare
The method of hypo-aluminum orthophosphate.It discloses in the application for a patent for invention file of Publication No. CN103879979A by sodium hypophosphite and aluminium
Salt, aluminium hydroxide or aluminium oxide reactive extrursion, curing, washing, filtering and drying in double screw extruder prepare hypo-aluminum orthophosphate
Method.It is disclosed in the application for a patent for invention file of Publication No. CN106633187A with sodium hypophosphite and reacting aluminum sulfate simultaneously
The method that hydrogen phosphide absorbent prepares hypo-aluminum orthophosphate is added.It is disclosed in the patent of invention file that notification number is CN103496681B
With aluminium hydroxide and the hypophosphorous acid method that reaction prepares hypo-aluminum orthophosphate in water.The patent of invention of Publication No. CN104860281A
The method for preparing hypo-aluminum orthophosphate with the ethanol solution reaction of sodium hypophosphite aqueous solution and aluminium chloride is disclosed in application documents.Bulletin
Number to disclose in the patent of invention file of CN103613084B with sodium hypophosphite and reacting aluminum sulfate, the phase is added three before the reaction
Poly cyanamid cyanurate is as crystal seed, the method for preparing spherical aluminum hypophosphite.The patent of invention of Publication No. CN103145110A
The method for preparing hypo-aluminum orthophosphate with sodium hypophosphite and nitric acid reactive aluminum is disclosed in application documents.
(2) micro-nano of hypo-aluminum orthophosphate.As Publication No. CN103803516A application for a patent for invention file in disclose
It is a kind of that sodium hypophosphite and aluminum soluble salt preparation nanometer hypo-aluminum orthophosphate being added in the pure water mixture containing surfactant
Method.
(3) the surface modification of hypo-aluminum orthophosphate and microencapsulation.Such as the application for a patent for invention of Publication No. CN105860594A
It is disclosed in file with sodium hypophosphite and reacting aluminum sulfate, the organic silicon solution of alcoholysis is added, prepares organic-silicon-modified secondary phosphorus
The method of sour aluminium.It is disclosed in the application for a patent for invention file of Publication No. CN105457574A with melamino-formaldehyde resin to secondary phosphorus
Sour aluminium is coated, the method for preparing microcapsules hypo-aluminum orthophosphate.The application for a patent for invention file of Publication No. CN105037808A
In disclose the in-situ modified microencapsulation hypo-aluminum orthophosphate for preparing carried out to hypo-aluminum orthophosphate with melamino-formaldehyde resin and its derivative
Method.It discloses with the sodium hypophosphite solution containing phosphate and contains in the patent of invention file that notification number is CN104448948B
There is the aluminium reaction of ethylene glycol to prepare modified hypo-aluminum orthophosphate.It is disclosed in the patent of invention file that notification number is CN103992512B
With cross-linked polymer containing triazine ring coating modification is carried out to hypo-aluminum orthophosphate, the method for preparing microcapsules hypo-aluminum orthophosphate.
Process disclosed in these patent documents plays very big push away in the preparation of hypo-aluminum orthophosphate and process optimization
Into effect, but when being used to prepare uniform and stable nanometer hypo-aluminum orthophosphate, there are still some shortcomings, and it is still necessary to want its preparation of Improvement
Method.
In the prior art, using micro-emulsion method for preparing nano hypo-aluminum orthophosphate, the grain of hypo-aluminum orthophosphate is controlled by microreactor
Diameter size is nanoscale, which can be used as fire retardant or other purposes.
Summary of the invention
The present invention exists when being especially used to prepare nanometer hypo-aluminum orthophosphate for existing disclosed hypo-aluminum orthophosphate preparation method
The problem of and deficiency, a kind of method being prepared uniform and stable nanometer hypo-aluminum orthophosphate using reverse microemulsion process is provided.
In order to solve the above problem and insufficient, the present invention provides the preparation methods of a kind of nanometer of hypo-aluminum orthophosphate, and step is such as
Under:
A) microemulsion containing sodium hypophosphite and cetyl trimethylammonium bromide for preparing Water-In-Oil, organic continuous
Sodium hypophosphite aqueous solution and cetyl trimethylammonium bromide are added in phase solvent, wherein the molar concentration of sodium hypophosphite aqueous solution
For 0.3-0.8mol/L, the molar concentration of cetyl trimethylammonium bromide is 0.3-0.5mol/L, is 50-95 DEG C of item in temperature
Under part, the reverse micro emulsion of the Water-In-Oil containing sodium hypophosphite, referred to as A liquid are prepared；
B) microemulsion containing aluminium chloride and cetyl trimethylammonium bromide for preparing Water-In-Oil, in organic continuous phases
Water-soluble aluminum salt and cetyl trimethylammonium bromide are added in solvent, wherein the molar concentration of cetyl trimethylammonium bromide
For 0.3-0.5mol/L, the reverse micro emulsion containing water-soluble aluminum salt of Water-In-Oil, referred to as B liquid are prepared；
C) nanometer hypo-aluminum orthophosphate is prepared, B liquid is slowly instilled in A liquid under strong stirring action, it is normal at 80-95 DEG C
Pressure adjusts the molar ratio of sodium hypophosphite and water-soluble aluminum salt, is heated to reflux, and reacts to be made in nanometer micro-emulsion reactor and receive
Rice hypo-aluminum orthophosphate colloid；
D) it separates, nanometer hypo-aluminum orthophosphate powder is made in purifying and drying nano hypo-aluminum orthophosphate colloid.
Specifically, the organic continuous phases solvent is toluene, benzene or dimethylbenzene.
Specifically, the aqueous aluminum salt solution is liquor alumini chloridi or aluminum sulfate solution.
Specifically, when preparing A liquid, the molar concentration of the sodium hypophosphite aqueous solution is 0.3-0.8mol/L, described
The molar concentration of cetyl trimethylammonium bromide be 0.3-0.5mol/L, organic continuous phases solvent and sodium hypophosphite aqueous solution
Volume ratio be 1:1.
Specifically, when preparing B liquid, if water-soluble aluminum salt selects liquor alumini chloridi, the liquor alumini chloridi
Molar concentration is 0.12-0.25mol/L, and the molar concentration of the cetyl trimethylammonium bromide is 0.3-0.5mol/L,
The volume ratio of organic continuous phases solvent and liquor alumini chloridi is 1:1.
Specifically, when preparing B liquid, if water-soluble aluminum salt selects liquor alumini chloridi, the sodium hypophosphite is water-soluble
The molar ratio of liquid and cetyl trimethylammonium bromide is 5:3.6, aluminum chloride aqueous solution and cetyl trimethylammonium bromide
Molar ratio is 1:2.16, and the volume ratio of the sodium hypophosphite microemulsion of the aluminium chloride microemulsion and water-in-oil type of water-in-oil type is
1:1.
Specifically, when preparing B liquid, if water-soluble aluminum salt selects aluminum sulfate solution, the aluminum sulfate solution
Molar concentration is 0.06-0.125mol/L, and the molar concentration of the cetyl trimethylammonium bromide is 0.3-0.5mol/
The volume ratio of L, organic continuous phases solvent and aluminum sulfate solution is 1:1.
More specifically, when water-soluble aluminum salt selects liquor alumini chloridi, mole of sodium hypophosphite and aluminium chloride in A liquid and B liquid
It is 3:1 than control, aluminium chloride microemulsion is added drop-wise in sodium hypophosphite microemulsion under conditions of 85 DEG C, pH value are 6, was added dropwise
It is stirred in journey, the reaction time is 1 hour.
More specifically, when water-soluble aluminum salt selects aluminum sulfate solution, mole of sodium hypophosphite and aluminum sulfate in A liquid and B liquid
It is 6:1 than control, aluminum sulfate microemulsion is added drop-wise in sodium hypophosphite microemulsion under conditions of 85 DEG C, pH value are 6, was added dropwise
It is stirred in journey, the reaction time is 1 hour.
Beneficial effects of the present invention: it provides and a kind of prepares uniform and stable nanometer hypo-aluminum orthophosphate using reverse microemulsion process
Method, be used to prepare uniform and stable nanometer hypo-aluminum orthophosphate, solve the deficiency of existing method and technique, improve the production of product
Rate and dimensional stability.
Specific embodiment
To describe the technical solutions in the embodiments of the present invention more clearly, the present invention is of the invention real now with reference to showing
The preparation method for applying example is described more fully hereinafter.However, the present invention can be embodied simultaneously with many different parameter settings
And it should not be construed as being limited to specific embodiment set forth herein.On the contrary, these embodiments are supplied to those skilled in the art
Member understands technical solution of the present invention.
Unless otherwise defined, term (including scientific and technical terminology) used herein above should be construed as having as belonging to the present invention
The identical meaning that those skilled in the art are commonly understood by.It will also be understood that term used herein above should be explained
To have the meaning consistent with their meanings in the content of this specification and the relevant technologies, and should not be with idealization
Or excessive form is explained, unless expressly so limiting here.
Embodiment 1
The aqueous solution of 100ml sodium hypophosphite containing 10.6g is added in 100ml benzene, 13g cetyl trimethyl bromination is added
Ammonium stirs evenly and is prepared into water in oil microemulsion, referred to as A liquid；The water of 100 ml aluminium chloride containing 4.6g is added in 100ml benzene
Solution is added 13g cetyl trimethylammonium bromide, stirs evenly and be prepared into water in oil microemulsion, referred to as B liquid；90
DEG C water-bath in, B liquid is stirred under 30 revolutions per seconds of speed slowly instill A liquid in, regulation system pH value obtains between 5-7
This colloid is evaporated by hypo-aluminum orthophosphate opalescent colloidal with Rotary Evaporators, and uniform and stable white nanometer hypophosphorous acid aluminium powder is made
End.
Embodiment 2
The aqueous solution of 100ml sodium hypophosphite containing 10.6g is added in 100ml toluene, 13g cetyl trimethyl bromine is added
Change ammonium, stirs evenly and be prepared into water in oil microemulsion, referred to as A liquid；100ml aluminium chloride containing 4.6g is added in 100ml toluene
Aqueous solution, be added 13g cetyl trimethylammonium bromide, stir evenly and be prepared into water in oil microemulsion, referred to as B liquid；?
In 95 DEG C of water-bath, B liquid is slowly instilled in A liquid under strong stirring action, regulation system pH value obtains secondary between 5-7
This colloid is evaporated by aluminum phosphate opalescent colloidal with Rotary Evaporators, and uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 3
The aqueous solution for adding 200ml sodium hypophosphite containing 5.3g in 200ml dimethylbenzene, is added 26g cetyl trimethyl bromine
Change ammonium, stirs evenly and be prepared into water in oil microemulsion, referred to as A liquid；200ml chlorination containing 2.3g is added in 200ml dimethylbenzene
The aqueous solution of aluminium is added 26g cetyl trimethylammonium bromide, stirs evenly and be prepared into water in oil microemulsion, referred to as B liquid；
In 85 DEG C of water-bath, B liquid is slowly instilled in A liquid under strong stirring action, regulation system pH value obtains between 5-7
This colloid is evaporated by hypo-aluminum orthophosphate opalescent colloidal with Rotary Evaporators, and uniform and stable white nanometer hypophosphorous acid aluminium powder is made
End.
Embodiment 4
The aqueous solution of 500 ml sodium hypophosphites containing 53g is added in 500ml dimethylbenzene, 65g cetyl trimethyl is added
Ammonium bromide stirs evenly and is prepared into water in oil microemulsion, referred to as A liquid；500ml sulfuric acid containing 29g is added in 500ml dimethylbenzene
The aqueous solution of aluminium is added 65g cetyl trimethylammonium bromide, stirs evenly and be prepared into water in oil microemulsion, referred to as B liquid；
In 85 DEG C of water-bath, B liquid is slowly instilled in A liquid under strong stirring action, regulation system pH value obtains between 5-7
This colloid is evaporated by hypo-aluminum orthophosphate opalescent colloidal with Rotary Evaporators, and uniform and stable white nanometer hypophosphorous acid aluminium powder is made
End.
Embodiment 5
The aqueous solution of 500ml sodium hypophosphite containing 53g is added in 500ml benzene, 65g cetyl trimethyl bromination is added
Ammonium stirs evenly and is prepared into water in oil microemulsion, referred to as A liquid；500ml aluminum sulfate containing 29g is added in 500 ml toluene
Aqueous solution is added 65g cetyl trimethylammonium bromide, stirs evenly and be prepared into water in oil microemulsion, referred to as B liquid；80
DEG C water-bath in, B liquid is slowly instilled in A liquid under strong stirring action, regulation system pH value obtains time phosphorus between 5-7
This colloid is evaporated by sour aluminium opalescent colloidal with Rotary Evaporators, and uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 6
The aqueous solution of 500ml sodium hypophosphite containing 26g is added in 500ml benzene, 65g cetyl trimethyl bromination is added
Ammonium stirs evenly and is prepared into water in oil microemulsion, referred to as A liquid；500 ml aluminum sulfate containing 14g are added in 500ml toluene
Aqueous solution is added 65g cetyl trimethylammonium bromide, stirs evenly and be prepared into water in oil microemulsion, referred to as B liquid；90
DEG C water-bath in, B liquid is slowly instilled in A liquid under strong stirring action, regulation system pH value obtains time phosphorus between 5-7
This colloid is evaporated by sour aluminium opalescent colloidal with Rotary Evaporators, and uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 7
The aqueous solution of 500ml sodium hypophosphite containing 26g is added in 500ml dimethylbenzene, 65g cetyl trimethyl bromine is added
Change ammonium, stirs evenly and be prepared into water in oil microemulsion, referred to as A liquid；500ml aluminum sulfate containing 14g is added in 500ml toluene
Aqueous solution is added 65g cetyl trimethylammonium bromide, stirs evenly and be prepared into water in oil microemulsion, referred to as B liquid；85
DEG C water-bath in, B liquid is slowly instilled in A liquid under strong stirring action, regulation system pH value obtains time phosphorus between 5-7
This colloid is evaporated by sour aluminium opalescent colloidal with Rotary Evaporators, and uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Although the present invention has been described referring to specific aspect of the invention, feature and exemplary embodiment herein, answer
When understanding, therefore embodiments of the present invention are not restricted, but are extended and covered numerous other technique ginsengs
Number variation and alternate embodiment, as will be given those skilled in the art in the invention are implied based on disclosure herein.
Correspondingly, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this
Within the protection scope of invention.
Claims (10)
1. the preparation method of a kind of nanometer of hypo-aluminum orthophosphate, it is characterised in that the following steps are included:
A) sodium hypophosphite aqueous solution and cetyl trimethylammonium bromide are added in organic continuous phases solvent, in 50-95 DEG C of item
The reverse micro emulsion that the Water-In-Oil containing sodium hypophosphite is made, referred to as A liquid are reacted under part；
B) aqueous aluminum salt solution and cetyl trimethylammonium bromide are added in organic continuous phases solvent, in 50-95 DEG C of item
The reverse micro emulsion that the Water-In-Oil of containing water-soluble aluminium salt is made, referred to as B liquid are reacted under part；
C) B liquid is slowly instilled in A liquid under strong stirring action, under 80-95 DEG C of normal pressure adjust sodium hypophosphite with it is water-soluble
Property aluminium salt molar ratio, be heated to reflux, in nanometer micro-emulsion reactor react be made nanometer hypo-aluminum orthophosphate colloid；
D) it separates, nanometer hypo-aluminum orthophosphate powder is made in purifying and drying nano hypo-aluminum orthophosphate colloid.
2. the preparation method of according to claim 1 nanometer of hypo-aluminum orthophosphate, it is characterised in that: the organic continuous phases are molten
Agent is toluene, benzene or dimethylbenzene.
3. the preparation method of according to claim 1 nanometer of hypo-aluminum orthophosphate, it is characterised in that: the water-soluble aluminum salt is molten
Liquid is liquor alumini chloridi.
4. the preparation method of according to claim 1 nanometer of hypo-aluminum orthophosphate, it is characterised in that: the water-soluble aluminum salt is molten
Liquid is aluminum sulfate solution.
5. the preparation method of according to claim 1 nanometer of hypo-aluminum orthophosphate, it is characterised in that: described when preparing A liquid
The molar concentration of sodium hypophosphite aqueous solution is 0.3-0.8mol/L, and the molar concentration of the cetyl trimethylammonium bromide is
The volume ratio of 0.3-0.5mol/L, organic continuous phases solvent and sodium hypophosphite aqueous solution is 1:1.
6. the preparation method of according to claim 3 nanometer of hypo-aluminum orthophosphate, it is characterised in that: described when preparing B liquid
The molar concentration of liquor alumini chloridi is 0.12-0.25mol/L, and the molar concentration of the cetyl trimethylammonium bromide is
The volume ratio of 0.3-0.5mol/L, organic continuous phases solvent and liquor alumini chloridi is 1:1.
7. the preparation method of according to claim 3 nanometer of hypo-aluminum orthophosphate, it is characterised in that: the sodium hypophosphite is water-soluble
The molar ratio of liquid and cetyl trimethylammonium bromide is 5:3.6, aluminum chloride aqueous solution and cetyl trimethylammonium bromide
Molar ratio is 1:2.16, and the volume ratio of the sodium hypophosphite microemulsion of the aluminium chloride microemulsion and water-in-oil type of water-in-oil type is
1:1.
8. the preparation method of according to claim 4 nanometer of hypo-aluminum orthophosphate, it is characterised in that: described when preparing B liquid
The molar concentration of aluminum sulfate solution is 0.06-0.125mol/L, and the molar concentration of the cetyl trimethylammonium bromide is
The volume ratio of 0.3-0.5mol/L, organic continuous phases solvent and aluminum sulfate solution is 1:1.
9. the preparation method of according to claim 6 or 7 nanometer of hypo-aluminum orthophosphate, it is characterised in that: time phosphorus in A liquid and B liquid
The control of the molar ratio of sour sodium and aluminium chloride is 3:1, and aluminium chloride microemulsion is added drop-wise to time phosphorus under conditions of 85 DEG C, pH value are 6
It in sour sodium microemulsion, is stirred during being added dropwise, the reaction time is 1 hour.
10. the preparation method of according to claim 8 nanometer of hypo-aluminum orthophosphate, it is characterised in that: hypophosphorous acid in A liquid and B liquid
The control of the molar ratio of sodium and aluminum sulfate is 6:1, and aluminum sulfate microemulsion is added drop-wise to hypophosphorous acid under conditions of 85 DEG C, pH value are 6
It in sodium microemulsion, is stirred during being added dropwise, the reaction time is 1 hour.
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| CN109368611A (en) * | 2018-10-30 | 2019-02-22 | 浙江加州国际纳米技术研究院台州分院 | A method of nano phosphate is prepared by reverse micro emulsion |
| CN111116987B (en) * | 2018-10-31 | 2022-05-17 | 襄阳三沃航天薄膜材料有限公司 | Method for synthesizing fine-grained aluminum hypophosphite composite flame retardant |
| CN114772568B (en) * | 2021-09-30 | 2023-08-11 | 四川金核高分子材料有限公司 | Method for preparing modified aluminum hypophosphite and product thereof |
| CN114314538A (en) * | 2021-12-16 | 2022-04-12 | 湖北省兴发磷化工研究院有限公司 | Synthesis method of superfine aluminum hypophosphite |
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| CN101654233A (en) * | 2009-06-19 | 2010-02-24 | 昆明理工大学 | Method for preparing sodium hypophosphite by integrally using sludge phosphorus |
| US9976010B2 (en) * | 2012-04-06 | 2018-05-22 | Rhodia Operations | Process for the production of hypophosphite salts |
| CN104163412A (en) * | 2014-08-08 | 2014-11-26 | 武汉科技大学 | Method for preparing aluminum hypophosphite via continuous reaction crystallization process |
| CN104860281A (en) * | 2015-06-01 | 2015-08-26 | 武汉理工大学 | Preparation method of aluminum hypophosphite |
| CN106006589A (en) * | 2015-08-24 | 2016-10-12 | 湖北航天化学技术研究所 | Method for joint production of hypophosphite of calcium, magnesium and aluminum |
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