CN105504879A - Method for preparing core-shell type silicon dioxide coated ammonium phosphate based on reversed-phase micro-emulsion method - Google Patents
Method for preparing core-shell type silicon dioxide coated ammonium phosphate based on reversed-phase micro-emulsion method Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention discloses a method for preparing core-shell type silicon dioxide coated ammonium phosphate based on a reversed-phase micro-emulsion method. The method comprises the following steps: (1) preparing reversed-phase micro-emulsion A of non-ionic surfactant/n-hexane/phosphoric acid; (2) preparing reversed-phase micro-emulsion B of non-ionic surfactant/n-hexane/ammonia water; (3) mixing the reversed-phase micro-emulsion A and the reversed-phase micro-emulsion B to obtain dispersion liquid of nano-particles; (4) dropwise adding a n-hexane solution of tetraethyl orthosilicate into the dispersion liquid of the nano-particles to obtain dispersion liquid of core-shell type silicon dioxide coated ammonium phosphate; and (4) dropwise adding a n-hexane solution of a silane coupling agent into the dispersion liquid of the core-shell type silicon dioxide coated ammonium phosphate, and then carrying out emulsion breaking, separation and drying treatments to obtain surface modified core-shell type silicon dioxide coated ammonium phosphate. The particle size of the core-shell type silicon dioxide coated ammonium phosphate prepared by the method disclosed by the invention can be controlled to be 100-800nm, and the core-shell type silicon dioxide coated ammonium phosphate is relatively small in particle size, narrow in distribution and good in dispersity.
Description
Technical field
The present invention relates to a kind of preparation method of ammonium phosphate salt, be specifically related to a kind of method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion process.
Background technology
The preparation method of ultra-fine ammonium phosphate salt is mainly divided into two large classes: physical method and chemical process.Conventional physical method has comminuting method, machine-alloying and evaporative condenser to send out, and first two method is simple to operate, and cost is low, but quality of item is low, and particle size uniformity is poor.Evaporative condenser sends out the nanoparticle that can obtain high-quality, and granularity is controlled, but technical requirements is high.Chemical preparation process can be divided into homogeneous system reaction method and heterogeneous system reaction method two class, and the former comprises the precipitator method and solvent evaporated method; The latter has sol-gel method, aerosol processing and microemulsion method etc.Homogeneous precipitation method accurately can control the chemical constitution of particle, easily add trace ingredients and obtain the homogeneous high-purity complex chemical compound of Multiple components, but in preparation process, controlling factor is many, is easily mixed into impurity, and size of particles is also difficult to control.Sol-gel method also can obtain the nanoparticle of high-quality, but also has certain range of application, is namely applicable to prepare the nano material that some is easy to phase inversion.Microemulsion method experimental installation is simple, processing ease, and by controlling solvent load, reactant concn, surfactant concentration and appropriate reaction condition, being easy to the nanoparticle obtaining uniform particle sizes, even can controlling the size of particle diameter within the specific limits.In addition, the nanoparticle of preparation directly can realize the coated of nanoparticle and surface modification in substance system.
ZL200910253739.2 discloses a kind of preparation method of core-shell silica coated ammonium polyphosphate, first ammonium polyphosphate joins in aqueous ethanolic solution by the method, vigorous stirring is to completely dispersed, with the alkali lye such as ammoniacal liquor or ammonium phosphate, pH value is transferred to 9 ~ 12, then adds silicon ester, produce silicon sol and carry out coated ammonium polyphosphate, finally adding the coupling agents such as titanic acid ester again carries out surface treatment, again after filtration, washing with alcohol, obtained a kind of core-shell silica coated ammonium polyphosphate after drying.This method solve APP infiltration migration, affect the problems such as product strength and thermotolerance are not enough, the flame retardant synergistic effect of same nitrogen phosphorus silicon effectively can improve flame retardant effect.But the product cut size that the method obtains is 5 ~ 50 microns, particle diameter is comparatively large, and size distribution is relatively wide.
Summary of the invention
The object of this invention is to provide a kind of method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method, diameter of particle can control in less and more concentrated scope by microemulsion method.The size tunable of the ammonium phosphate salt that core-shell silica prepared by the present invention is coated built in 100 ~ 800nm, the less and narrowly distributing of particle diameter, good dispersity, and directly can realize the surface modification to nanoparticle in substance system.
The object of the invention is to be achieved through the following technical solutions:
Prepare a method for the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method, comprise the steps:
(1) the reverse micro emulsion A of nonionogenic tenside/normal hexane/phosphoric acid is prepared: under normal temperature condition, get 3 ~ 5g normal hexane and 2.5 ~ 3.5g nonionogenic tenside, 10 ~ 20min is stirred after mixing, add 1 ~ 2g phosphoric acid again, 0.8 ~ 1g Pentyl alcohol is added after stirring 10 ~ 20min, after continuing stirring 0.5 ~ 1h, obtain transparent reverse micro emulsion A;
(2) the reverse micro emulsion B of nonionogenic tenside/normal hexane/ammoniacal liquor is prepared: under normal temperature condition, get 2 ~ 5g normal hexane and 2.0 ~ 3.5g nonionogenic tenside, 10 ~ 20min is stirred after mixing, add 1.0 ~ 2.8g weak ammonia again, after continuing stirring 0.5 ~ 1h, obtain transparent reverse micro emulsion B;
(3) temperature controls is 0 ~ 20 DEG C, reverse micro emulsion A is poured in the four-hole bottle with agitator, stirring velocity is set as 300 ~ 400r/min, after keeping 5 ~ 15min, again reverse micro emulsion B is added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, after stirring 2 ~ 3h, obtains the dispersion liquid of nanoparticle;
(4) temperature controls is 0 ~ 20 DEG C, be added drop-wise in four-hole bottle by the hexane solution of 0.5 ~ 4.0g tetraethoxy, rate of addition is 3 ~ 4mL/min, and stirring velocity is 300 ~ 400r/min, after keeping 2 ~ 6h, obtain the dispersion liquid of the coated ammonium phosphate salt of core-shell silica;
(5) temperature controls is 0 ~ 20 DEG C, the hexane solution of 0.1 ~ 1.5g silane coupling agent is added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, stirring velocity is 300 ~ 400r/min, after keeping 12 ~ 24h, again after the process such as breakdown of emulsion, separation and drying, finally obtain the ammonium phosphate salt that the core-shell silica of surface modification is coated.
In above-mentioned steps (1), nonionogenic tenside is Span-80 and Tween-80 is (3 ~ 5) according to mass ratio: 1 formulated mixed solution.
In above-mentioned steps (1), the mass concentration of phosphoric acid is higher than 85%.
In above-mentioned steps (2), nonionogenic tenside is Span-80 and Tween-80 is (2 ~ 4) according to mass ratio: 1 formulated mixed solution.
In above-mentioned steps (2), weak ammonia is NH
3content be 25 ~ 28% ammoniacal liquor and ethanol in mass ratio for 1:(1 ~ 1.25) formulated solution.
In above-mentioned steps (4), the hexane solution of tetraethoxy is tetraethoxy and normal hexane is 2:(1 ~ 4 in mass ratio) formulated solution.
In above-mentioned steps (5), silane coupling agent is one or more in the silane coupling agents such as vinyltriethoxysilane, aminopropyl triethoxysilane, Y-(2,3-epoxy third oxygen) propyl trimethoxy silicane.
In above-mentioned steps (5), the hexane solution of silane coupling agent is silane coupling agent and normal hexane is 2:(1 ~ 4 in mass ratio) formulated solution.
In above-mentioned steps (5), breakdown of emulsion is add 10 ~ 50g acetone or alcohol in former dispersion liquid after, then stirs, and obtains muddy emulsion.
The coated ammonium phosphate salt of the core-shell silica that the present invention prepares can be used as a kind of fire retardant of superior performance.Silicon-dioxide is nontoxic, non-stimulated, to the mankind and environment without harm, and high, the water-fast protection against the tide of thermostability, after coated with silica ammonium phosphate salt, can obviously reduce the water-soluble of product, if carry out surface treatment to the ammonium phosphate salt particulate silane coupling agent of coated with silica again, not only can reduce the contact angle of particle and water, by selecting different silane coupling agents, the consistency with macromolecular material can also be increased.In addition; usually can there is the phenomenons such as migration and bloom due to ammonium phosphate salt based flame retardant; the flame retardant properties of material can be had influence on; the present invention has carried out coated process to ammonium phosphate salt; can problems be solved, moreover, the pungent taste of ammonium phosphate salt can also be shielded like this; reduce the release of toxic ingredient in polymer processing in fire retardant, avoid environmental pollution and actual bodily harm.Finally, the temperature of initial decomposition of product after coated with silica ammonium phosphate salt, can be improved, expand the use range of fire retardant.The synergistic effect of nitrogen phosphorus silicon three kinds of ignition-proof elements can improve the flame retardant properties of product better, thus reduces the usage quantity of product, energy-conserving and environment-protective more.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the coated with silica ammonium phosphate salt that embodiment 1 step (4) obtains;
Fig. 2 is the XRD figure spectrum of the coated with silica ammonium phosphate salt that embodiment 1 step (4) obtains.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment 1:
In the present embodiment, the preparation method of hud typed coated with silica ammonium phosphate salt carries out in the steps below:
(1) under normal temperature condition, get 4g normal hexane, 2.4gSpan-80 and 0.6gTween-80, after mixing, stir 15min, then add 1g phosphoric acid, after stirring 15min, add 0.9g Pentyl alcohol, after continuing to stir 0.5h, obtain transparent reverse micro emulsion A;
(2) under normal temperature condition, get 3g normal hexane, 1.7gSpan-80 and 0.6gTween-80, after mixing, stir 15min, then add the weak ammonia prepared by 0.7g ammoniacal liquor and 0.7g ethanol, after continuing to stir 0.5h, obtain transparent reverse micro emulsion B;
(3) temperature controls is 10 DEG C, and poured in the four-hole bottle with agitator by reverse micro emulsion A, stirring velocity is set as 350r/min, keep 10min, then be added drop-wise in four-hole bottle by reverse micro emulsion B, rate of addition is 3 ~ 4mL/min, after stirring 2.5h, obtain the dispersion liquid of nanoparticle;
(4) temperature controls is 10 DEG C, after 0.6g tetraethoxy is dissolved in 0.4g normal hexane, be added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, stirring velocity is still 350r/min, after keeping 4h, obtains the dispersion liquid of the coated ammonium phosphate salt of core-shell silica, wherein: as shown in Figure 1, the XRD figure spectrum of coated with silica ammonium phosphate salt as shown in Figure 2 for the scanning electron microscope (SEM) photograph of coated with silica ammonium phosphate salt;
(5) temperature controls is 0 ~ 20 DEG C, after 0.1g vinyltriethoxysilane is dissolved in 0.1g normal hexane, be added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, stirring velocity is still 350r/min, after keeping 15h, then after the process such as breakdown of emulsion, separation and drying, finally obtain the ammonium phosphate salt that the core-shell silica of surface modification is coated.
Embodiment 2:
In the present embodiment, the preparation method of hud typed coated with silica ammonium phosphate salt carries out in the steps below:
(1) under normal temperature condition, get 4g normal hexane, 2.4gSpan-80 and 0.6gTween-80, after mixing, stir 15min, then add 1g phosphoric acid, after stirring 15min, add 0.9g Pentyl alcohol, after continuing to stir 0.5h, obtain transparent reverse micro emulsion A;
(2) under normal temperature condition, get 3.2g normal hexane, 1.8gSpan-80 and 0.6gTween-80, after mixing, stir 15min, then add the weak ammonia prepared by 0.75g ammoniacal liquor and 0.75g ethanol, after continuing to stir 0.5h, obtain transparent reverse micro emulsion B;
(3) temperature controls is 0 ~ 20 DEG C, reverse micro emulsion A is poured in the four-hole bottle with agitator, stirring velocity is set as 300r/min, keep 10min, again reverse micro emulsion B is added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, after stirring 3h, obtains the dispersion liquid of nanoparticle;
(4) temperature controls is 5 DEG C, after 0.75g tetraethoxy is dissolved in 0.5g normal hexane, is added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, stirring velocity is still 300r/min, after keeping 6h, obtains the dispersion liquid of the coated ammonium phosphate salt of core-shell silica;
(5) temperature controls is 5 DEG C, after 0.1g aminopropyl triethoxysilane is dissolved in 0.1g normal hexane, be added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, stirring velocity is still 300r/min, after keeping 20h, then through breakdown of emulsion, be separated after waiting process with drying, finally obtain the ammonium phosphate salt that the core-shell silica of surface modification is coated.
Claims (10)
1. prepare a method for the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method, it is characterized in that described method steps is as follows:
(1) under normal temperature condition, get 3 ~ 5g normal hexane and 2.5 ~ 3.5g nonionogenic tenside, after mixing, stir 10 ~ 20min, add 1 ~ 2g phosphoric acid again, add 0.8 ~ 1g Pentyl alcohol after stirring 10 ~ 20min, after continuing stirring 0.5 ~ 1h, obtain transparent reverse micro emulsion A;
(2) under normal temperature condition, get 2 ~ 5g normal hexane and 2.0 ~ 3.5g nonionogenic tenside, stir 10 ~ 20min after mixing, then add 1.0 ~ 2.8g weak ammonia, after continuing stirring 0.5 ~ 1h, obtain transparent reverse micro emulsion B;
(3) temperature controls is 0 ~ 20 DEG C, reverse micro emulsion A is poured in the four-hole bottle with agitator, stirring velocity is set as 300 ~ 400r/min, after keeping 5 ~ 15min, again reverse micro emulsion B is added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, after stirring 2 ~ 3h, obtains the dispersion liquid of nanoparticle;
(4) temperature controls is 0 ~ 20 DEG C, be added drop-wise in four-hole bottle by the hexane solution of 0.5 ~ 4.0g tetraethoxy, rate of addition is 3 ~ 4mL/min, and stirring velocity is 300 ~ 400r/min, after keeping 2 ~ 6h, obtain the dispersion liquid of the coated ammonium phosphate salt of core-shell silica;
(5) temperature controls is 0 ~ 20 DEG C, the hexane solution of 0.1 ~ 1.5g silane coupling agent is added drop-wise in four-hole bottle, rate of addition is 3 ~ 4mL/min, stirring velocity is 300 ~ 400r/min, after keeping 12 ~ 24h, again after breakdown of emulsion, separation and drying treatment, finally obtain the ammonium phosphate salt that the core-shell silica of surface modification is coated.
2. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 1, it is characterized in that in described step (1), nonionogenic tenside is Span-80 and Tween-80 is (3 ~ 5) according to mass ratio: 1 formulated mixed solution.
3. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 1, is characterized in that in described step (1), the mass concentration of phosphoric acid is higher than 85%.
4. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 1, it is characterized in that in described step (2), nonionogenic tenside is Span-80 and Tween-80 is (2 ~ 4) according to mass ratio: 1 formulated mixed solution.
5. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 1, it is characterized in that in described step (2), weak ammonia is ammoniacal liquor and ethanol is 1:(1 ~ 1.25 in mass ratio) formulated solution.
6. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 5, is characterized in that NH in described ammoniacal liquor
3content is 25 ~ 28%.
7. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 1, it is characterized in that in described step (4), the hexane solution of tetraethoxy is tetraethoxy and normal hexane is 2:(1 ~ 4 in mass ratio) formulated solution.
8. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 1, it is characterized in that in described step (5), silane coupling agent is one or more in vinyltriethoxysilane, aminopropyl triethoxysilane, Y-(2,3-epoxy third oxygen) propyl trimethoxy silicane.
9. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 1 or 8, it is characterized in that in described step (5), the hexane solution of silane coupling agent is silane coupling agent and normal hexane is 2:(1 ~ 4 in mass ratio) formulated solution.
10. the method preparing the coated ammonium phosphate salt of core-shell silica based on reverse microemulsion method according to claim 1, it is characterized in that in described step (5), breakdown of emulsion is add 10 ~ 50g acetone or alcohol in former dispersion liquid after, then stirs, and obtains muddy emulsion.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108570246A (en) * | 2018-01-24 | 2018-09-25 | 北京化工大学 | A kind of preparation method of the ammonium polyphosphate with activity of cross-linking reaction group |
| CN112430417A (en) * | 2020-11-20 | 2021-03-02 | 兰州理工大学白银新材料研究院 | Preparation method of ammonium polyphosphate microspheres |
| CN115517979A (en) * | 2022-09-30 | 2022-12-27 | 中国日用化学研究院有限公司 | Preparation of ZnO @ SiO based on narrow distribution AEO3-AEO9 reversed microemulsion 2 Method for producing nanoparticles |
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| 杨汉民等: "反相微乳液中LaPO_4纳米粒子的制备", 《中南民族大学学报(自然科学版)》 * |
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| CN108570246A (en) * | 2018-01-24 | 2018-09-25 | 北京化工大学 | A kind of preparation method of the ammonium polyphosphate with activity of cross-linking reaction group |
| CN108570246B (en) * | 2018-01-24 | 2019-08-02 | 北京化工大学 | A kind of preparation method of the ammonium polyphosphate with activity of cross-linking reaction group |
| CN112430417A (en) * | 2020-11-20 | 2021-03-02 | 兰州理工大学白银新材料研究院 | Preparation method of ammonium polyphosphate microspheres |
| CN115517979A (en) * | 2022-09-30 | 2022-12-27 | 中国日用化学研究院有限公司 | Preparation of ZnO @ SiO based on narrow distribution AEO3-AEO9 reversed microemulsion 2 Method for producing nanoparticles |
| CN115517979B (en) * | 2022-09-30 | 2024-01-30 | 中国日用化学研究院有限公司 | Preparation of ZnO@SiObased on narrow-distribution AEO3-AEO9 inverse microemulsion 2 Method of nanoparticle |
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