CN107337187A - 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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- CN107337187A CN107337187A CN201710598598.2A CN201710598598A CN107337187A CN 107337187 A CN107337187 A CN 107337187A CN 201710598598 A CN201710598598 A CN 201710598598A CN 107337187 A CN107337187 A CN 107337187A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/165—Hypophosphorous acid; Salts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses the preparation method of a kind of nanometer of hypo-aluminum orthophosphate, belong to technical field of nanometer material preparation.Comprise the following steps：A) the sodium hypophosphite aqueous solution and cetyl trimethylammonium bromide 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 for the Water-In-Oil that containing water-soluble aluminium salt is made, referred to as B liquid are reacted under the conditions of 50 95 DEG C；C) A liquid and B liquid are mixed, the mol 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) separate, 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, the deficiency for solving existing method and technique.
Description
Technical field
The present invention relates to the preparation method of a kind of nanometer of hypo-aluminum orthophosphate, belong to technical field of nanometer material preparation.
Background technology
Hypo-aluminum orthophosphate is because of the advantages that its phosphorus content is high, heat endurance is good, synthesis technique 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 cooperative effect, improves flame retardant effect.People have carried out many grind to hypo-aluminum orthophosphate
Study carefully, mainly have：
（1）New method and technique prepared by hypo-aluminum orthophosphate.As Publication No. CN104163412A application for a patent for invention file in
Disclose sodium hypophosphite and soluble aluminum reactant salt, separate hypo-aluminum orthophosphate crystal, mother liquor Returning reactor is continuous to prepare time phosphorus
The method of sour aluminium.Disclosed sodium hypophosphite and aluminium salt, hydrogen in Publication No. CN103879979A application for a patent for invention file
Aluminum oxide or aluminum oxide reactive extrursion, curing, washing, filtering and the dry side for preparing hypo-aluminum orthophosphate in double screw extruder
Method.Disclose with sodium hypophosphite and reacting aluminum sulfate and add in Publication No. CN106633187A application for a patent for invention file
The method that hydrogen phosphide absorbent prepares hypo-aluminum orthophosphate.Notification number is to disclose to use hydrogen in CN103496681B patent of invention file
The method that the reaction in water of aluminum oxide and hypophosphorous acid prepares hypo-aluminum orthophosphate.Publication No. CN104860281A application for a patent for invention
The method for preparing hypo-aluminum orthophosphate with the ethanol solution reaction of the sodium hypophosphite aqueous solution and aluminium chloride is disclosed in file.Notification number is
Disclosed in CN103613084B patent of invention file with sodium hypophosphite and reacting aluminum sulfate, before the reaction the phase add melamine
Amine cyanurate is as crystal seed, the method for preparing spherical aluminum hypophosphite.Publication No. CN103145110A application for a patent for invention
The method for preparing hypo-aluminum orthophosphate with sodium hypophosphite and nitric acid reactive aluminum is disclosed in file.
（2）The micro-nano of hypo-aluminum orthophosphate.As Publication No. CN103803516A application for a patent for invention file in disclose
A kind of the addition sodium hypophosphite in the pure water mixture containing surfactant and aluminum soluble salt prepare nanometer hypo-aluminum orthophosphate
Method.
（3）The surface modification of hypo-aluminum orthophosphate and microencapsulation.Such as Publication No. CN105860594A application for a patent for invention
Disclosed in file with sodium hypophosphite and reacting aluminum sulfate, add the organic silicon solution of alcoholysis, prepare organic-silicon-modified secondary phosphorus
The method of sour aluminium.Disclosed in Publication No. CN105457574A application for a patent for invention file with melamino-formaldehyde resin to secondary phosphorus
Sour aluminium is coated, the method for preparing microcapsules hypo-aluminum orthophosphate.Publication No. CN105037808A application for a patent for invention file
In disclose and carry out to hypo-aluminum orthophosphate the in-situ modified microencapsulation hypo-aluminum orthophosphate for preparing with melamino-formaldehyde resin and its derivative
Method.Notification number is to disclose with the sodium hypophosphite solution containing phosphate and contain in CN104448948B patent of invention file
The aluminium reaction for having ethylene glycol prepares modified hypo-aluminum orthophosphate.Notification number is disclosed in CN103992512B patent of invention file
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 serves very big push away in the preparation of hypo-aluminum orthophosphate and process optimization
Enter effect, but for still suffering from some shortcomings when preparing uniform and stable nanometer hypo-aluminum orthophosphate, still need and want its preparation of Improvement
Method.
In the prior art, using micro-emulsion method for preparing nano hypo-aluminum orthophosphate, the grain of microreactor control hypo-aluminum orthophosphate is passed through
Footpath size is nanoscale, and the product can be used as fire retardant or other purposes.
The content of the invention
The present invention exists when being particularly used for for existing disclosed hypo-aluminum orthophosphate preparation method and prepare nanometer hypo-aluminum orthophosphate
The problem of and deficiency, there is provided a kind of method that uniform and stable nanometer hypo-aluminum orthophosphate is prepared using reverse microemulsion process.
For solve the above problems and deficiency, the invention provides the preparation method of a kind of nanometer of hypo-aluminum orthophosphate, and its step is such as
Under：
A) microemulsion containing sodium hypophosphite and cetyl trimethylammonium bromide of Water-In-Oil is prepared, it is molten in organic continuous phases
The sodium hypophosphite aqueous solution is added in agent and cetyl trimethylammonium bromide, the molar concentration of the wherein sodium hypophosphite aqueous solution are
0.3-0.8mol/L, the molar concentration of cetyl trimethylammonium bromide is 0.3-0.5mol/L, is 50-95 DEG C of condition in temperature
Under, prepare the reverse micro emulsion of the Water-In-Oil containing sodium hypophosphite, referred to as A liquid；
B) microemulsion containing aluminium chloride and cetyl trimethylammonium bromide of Water-In-Oil is prepared, in organic continuous phases solvent
Middle addition water-soluble aluminum salt and cetyl trimethylammonium bromide, the molar concentration of wherein cetyl trimethylammonium bromide are
0.3-0.5mol/L, prepare the reverse micro emulsion containing water-soluble aluminum salt of Water-In-Oil, referred to as B liquid；
C) nanometer hypo-aluminum orthophosphate is prepared, by A liquid and B liquid, mixing, sodium hypophosphite and water solubility are adjusted under 80-95 DEG C of normal pressure
The mol ratio of aluminium salt, is heated to reflux, and is reacted in nanometer micro-emulsion reactor and nanometer hypo-aluminum orthophosphate colloid is made；
D) separate, nanometer hypo-aluminum orthophosphate powder is made in purifying and drying nano hypo-aluminum orthophosphate colloid.
Specifically, described organic continuous phases solvent is toluene, benzene or dimethylbenzene.
Specifically, described aqueous aluminum salt solution is liquor alumini chloridi or aluminum sulfate solution.
Specifically, when preparing A liquid, the molar concentration of the described 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 the sodium hypophosphite aqueous solution
Volume ratio be 1：1.
Specifically, when preparing B liquid, if water-soluble aluminum salt selects liquor alumini chloridi, described liquor alumini chloridi
Molar concentration is 0.12-0.25mol/L, and the molar concentration of described 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, described sodium hypophosphite is water-soluble
The mol ratio of liquid and cetyl trimethylammonium bromide is 5：3.6, aluminum chloride aqueous solution and cetyl trimethylammonium bromide
Mol ratio is 1：2.16, the volume ratio of the aluminium chloride microemulsion of water-in-oil type and the sodium hypophosphite microemulsion of water-in-oil type is
1：1.
Specifically, when preparing B liquid, if water-soluble aluminum salt selects aluminum sulfate solution, described aluminum sulfate solution
Molar concentration is 0.06-0.125mol/L, and the molar concentration of described 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 than control:1, aluminium chloride microemulsion is added drop-wise in sodium hypophosphite microemulsion under conditions of being 6 in 85 DEG C, pH value, was added dropwise
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 than control：1, aluminum sulfate microemulsion is added drop-wise in sodium hypophosphite microemulsion under conditions of being 6 in 85 DEG C, pH value, was added dropwise
Stirred in journey, the reaction time is 1 hour.
Beneficial effects of the present invention：Provide and a kind of uniform and stable nanometer hypo-aluminum orthophosphate is prepared using reverse microemulsion process
Method, for preparing uniform and stable nanometer hypo-aluminum orthophosphate, solve the deficiency of existing method and technique, improve the production of product
Rate and dimensional stability.
Embodiment
Technical scheme in order to illustrate the embodiments of the present invention more clearly, the present invention are 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 people in the art
Member understands technical scheme.
Unless otherwise defined, term used herein above（Include scientific and technical terminology）It should be construed to have 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
For with the meaning consistent with their meanings in the content of this specification and correlation technique, and should not be with idealization
Or excessive form is explained, unless expressly so limiting here.
Embodiment 1
The aqueous solution of 100ml sodium hypophosphites containing 10.6g is added in 100ml benzene, adds 13g cetyl trimethylammonium bromides,
Stir and be prepared into water in oil microemulsion, referred to as A liquid；The water-soluble of 100 ml aluminium chloride containing 4.6g is added in 100ml benzene
Liquid, 13g cetyl trimethylammonium bromides are added, stirs and is prepared into water in oil microemulsion, referred to as B liquid；At 90 DEG C
Water-bath in, B liquid is stirred under 30 revolutions per seconds of speed and slowly instilled in A liquid, regulation system pH value obtains time between 5-7
Aluminum phosphate opalescent colloidal, this colloid is evaporated with Rotary Evaporators, uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 2
The aqueous solution of 100ml sodium hypophosphites containing 10.6g is added in 100ml toluene, adds 13g cetyl trimethyl brominations
Ammonium, stir and be prepared into water in oil microemulsion, referred to as A liquid；100ml aluminium chloride containing 4.6g is added in 100ml toluene
The aqueous solution, 13g cetyl trimethylammonium bromides are added, stirs and is prepared into water in oil microemulsion, referred to as B liquid；95
DEG C water-bath in, B liquid is slowly instilled in A liquid under strong agitation effect, regulation system pH value obtains time phosphorus between 5-7
Sour aluminium opalescent colloidal, this colloid is evaporated with Rotary Evaporators, uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 3
Add the aqueous solution of 200ml sodium hypophosphites containing 5.3g in 200ml dimethylbenzene, add 26g cetyl trimethylammonium bromides,
Stir and be prepared into water in oil microemulsion, referred to as A liquid；The water of 200ml aluminium chloride containing 2.3g is added in 200ml dimethylbenzene
Solution, 26g cetyl trimethylammonium bromides are added, stirs and is prepared into water in oil microemulsion, referred to as B liquid；At 85 DEG C
Water-bath in, by B liquid strong agitation effect under slowly instill in A liquid, regulation system pH value obtains hypophosphorous acid between 5-7
Aluminium opalescent colloidal, this colloid is evaporated with Rotary Evaporators, uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 4
The aqueous solution of 500 ml sodium hypophosphites containing 53g is added in 500ml dimethylbenzene, adds 65g cetyl trimethyl brominations
Ammonium, stir and be prepared into water in oil microemulsion, referred to as A liquid；500ml aluminum sulfate containing 29g is added in 500ml dimethylbenzene
The aqueous solution, 65g cetyl trimethylammonium bromides are added, stirs and is 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 agitation effect, regulation system pH value obtains time phosphorus between 5-7
Sour aluminium opalescent colloidal, this colloid is evaporated with Rotary Evaporators, uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 5
The aqueous solution of 500ml sodium hypophosphites containing 53g is added in 500ml benzene, 65g cetyl trimethylammonium bromides is added, stirs
Mix and be uniformly prepared into water in oil microemulsion, referred to as A liquid；The water-soluble of 500ml aluminum sulfate containing 29g is added in 500 ml toluene
Liquid, 65g cetyl trimethylammonium bromides are added, stirs and is prepared into water in oil microemulsion, referred to as B liquid；At 80 DEG C
In water-bath, B liquid is slowly instilled in A liquid under strong agitation effect, regulation system pH value obtains hypo-aluminum orthophosphate between 5-7
Opalescent colloidal, this colloid is evaporated with Rotary Evaporators, uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 6
The aqueous solution of 500ml sodium hypophosphites containing 26g is added in 500ml benzene, 65g cetyl trimethylammonium bromides is added, stirs
Mix and be uniformly prepared into water in oil microemulsion, referred to as A liquid；The water-soluble of 500 ml aluminum sulfate containing 14g is added in 500ml toluene
Liquid, 65g cetyl trimethylammonium bromides are added, stirs and is prepared into water in oil microemulsion, referred to as B liquid；At 90 DEG C
In water-bath, B liquid is slowly instilled in A liquid under strong agitation effect, regulation system pH value obtains hypo-aluminum orthophosphate between 5-7
Opalescent colloidal, this colloid is evaporated with Rotary Evaporators, uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Embodiment 7
The aqueous solution of 500ml sodium hypophosphites containing 26g is added in 500ml dimethylbenzene, adds 65g cetyl trimethyl brominations
Ammonium, stir and be prepared into water in oil microemulsion, referred to as A liquid；The water of 500ml aluminum sulfate containing 14g is added in 500ml toluene
Solution, 65g cetyl trimethylammonium bromides are added, stirs and is prepared into water in oil microemulsion, referred to as B liquid；At 85 DEG C
Water-bath in, by B liquid strong agitation effect under slowly instill in A liquid, regulation system pH value obtains hypophosphorous acid between 5-7
Aluminium opalescent colloidal, this colloid is evaporated with Rotary Evaporators, uniform and stable white nanometer hypo-aluminum orthophosphate powder is made.
Although the present invention has been described with reference to specific aspect, feature and the exemplary embodiment of the present invention herein, should
When understanding, therefore embodiments of the present invention are not restricted, but are extended and covered numerous other technique ginsengs
Number change and alternate embodiment, as will be given those skilled in the art in the invention are implied based on disclosure herein.
Correspondingly, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc., it should be included in this
Within the protection domain of invention.
Claims (10)
1. the preparation method of a kind of nanometer of hypo-aluminum orthophosphate, it is characterised in that comprise the following steps：
A) the sodium hypophosphite aqueous solution and cetyl trimethylammonium bromide are added in organic continuous phases solvent, in 50-95 DEG C of bar
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 bar
The reverse micro emulsion for the Water-In-Oil that containing water-soluble aluminium salt is made, referred to as B liquid are reacted under part；
C) A liquid and B liquid are mixed, the mol ratio of sodium hypophosphite and water-soluble aluminum salt, heating is adjusted under 80-95 DEG C of normal pressure
Backflow, reacted in nanometer micro-emulsion reactor and nanometer hypo-aluminum orthophosphate colloid is made；
D) separate, 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：Described 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：Described 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：Described 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：It is described when preparing A liquid
The molar concentration of the sodium hypophosphite aqueous solution is 0.3-0.8mol/L, and the molar concentration of described cetyl trimethylammonium bromide is
The volume ratio of 0.3-0.5mol/L, organic continuous phases solvent and the 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：It is described when preparing B liquid
The molar concentration of liquor alumini chloridi is 0.12-0.25mol/L, and the molar concentration of described 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：Described sodium hypophosphite is water-soluble
The mol ratio of liquid and cetyl trimethylammonium bromide is 5：3.6, aluminum chloride aqueous solution and cetyl trimethylammonium bromide
Mol ratio is 1：2.16, the volume ratio of the aluminium chloride microemulsion of water-in-oil type and the sodium hypophosphite microemulsion 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：It is described when preparing B liquid
The molar concentration of aluminum sulfate solution is 0.06-0.125mol/L, and the molar concentration of described 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 the nanometer hypo-aluminum orthophosphate according to claim 6 or 7, it is characterised in that：Time phosphorus in A liquid and B liquid
The mol ratio control of sour sodium and aluminium chloride is 3:1, aluminium chloride microemulsion is added drop-wise to time phosphorus under conditions of being 6 in 85 DEG C, pH value
In sour sodium microemulsion, stirred during dropwise addition, 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 mol ratio of sodium and aluminum sulfate is 6：1, aluminum sulfate microemulsion is added drop-wise to hypophosphorous acid under conditions of being 6 in 85 DEG C, pH value
In sodium microemulsion, stirred during dropwise addition, the reaction time is 1 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN111116987A (en) * | 2018-10-31 | 2020-05-08 | 襄阳三沃航天薄膜材料有限公司 | Method for synthesizing fine-grained aluminum hypophosphite composite flame retardant |
| 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 |
| CN114772568A (en) * | 2021-09-30 | 2022-07-22 | 四川金核高分子材料有限公司 | Method for preparing modified aluminum hypophosphite and product thereof |
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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 |
| CN111116987A (en) * | 2018-10-31 | 2020-05-08 | 襄阳三沃航天薄膜材料有限公司 | Method for synthesizing fine-grained aluminum hypophosphite composite flame retardant |
| 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 |
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| 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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| CN107337187B (en) | 2019-05-10 |
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