CN101798390A - Preparation method of quaternary ammonium salt and halogenated lithium-containing fractal aggregate - Google Patents
Preparation method of quaternary ammonium salt and halogenated lithium-containing fractal aggregate Download PDFInfo
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Abstract
The invention belongs to the field of material and fractal, in particular to a preparation method of quaternary ammonium salt and halogenated lithium-containing fractal aggregate. The method comprises the steps of: firstly inserting dimethyl diallyl ammonium chloride monomers among montmorillonite layers to obtain dimethyl diallyl ammonium-montmorillonite; dispersing the dimethyl diallyl ammonium-montmorillonite into hydrosolvent to have in situ polymerization so as to obtain poly-dimethyl diallyl ammonium-montmorillonite; dispersing the poly-dimethyl diallyl ammonium-montmorillonite into tetrahydrofuran solvent; extracting poly-dimethyl diallyl ammonium-halogenated lithium with tetrahydrofuran solution of lithium chloride to obtain composite micelle of poly-dimethyl diallyl ammonium-lithium chloride; and dropping the poly-dimethyl diallyl ammonium-lithium chloride onto a cleaning substrate, and naturally volatilizing the solvent in room-temperature air to obtain the aggregate with fractal pattern. The method synthesizes polymer and inorganic salt-containing fractal aggregate with a simple chemical method, the reaction conditions can be controlled, the price of the raw materials is low, the experimental facility is simple, and the repeatability is high.
Description
Technical field
The invention belongs to material and fractal field, relating in particular to a kind of is the preparation method that the template preparation contains the fractal aggregate of quaternary ammonium salt and lithium halide with the polynite.
Background technology
Fractal how much of the Nature that is called, the object or the phenomenon that are seen everywhere and have fractal characteristic at occurring in nature.But utilize the technology of artificial means controlledly synthesis and preparation fractal also rare.That has reported mostly is the particularly preparation of the fractal of metallic substance of inorganic materials, and wherein requirement for experiment condition harshness, device are comparatively complicated.
For example: utilize sol-gel process to prepare Yin-Jin nuclear-core/shell nanoparticles 2-dimensional mesoscopic fractal aggregate.(China, open day: 2002.07.17, the patent No.: CN01140157.5, the preparation method of patent name: Yin-Jin nuclear-core/shell nanoparticles 2-dimensional mesoscopic fractal aggregate.)
Adopt electrodip process on natural fractal body material, to obtain a kind of fractal metallic substance.(China, open day: 2002.10.02, the patent No.: CN01106178.2, patent name: a kind of preparation method of shape classified structure metal material.) do raw material with ZnO powder, Graphite Powder 99 and the copper powder of commodity, with the N that is easy to get
2Be source of the gas, in the horizontal tube growth furnace, adopt on substrate, the grow macroscopic ZnO monocrystal material of tree-shaped fractal structure of thermal evaporation.(China, open day: 2007.12.26, the patent No.: CN200710039173.4, patent name: macroscopic ZnO monocrystal material of a kind of tree-shaped fractal structure and preparation method thereof.)
Also have Xylo-Mucine dissolved in the cationic polyelectrolyte solution to form complex compound, be dissolved in the mixed solvent that alkali lye and organic solvent be made into, obtain fractal aggregate through suitable aftertreatment.(China, open day: 2009.02.11, the patent No.: CN200810161594.9, patent name: the preparation method who includes carboxymethyl cellulose complex compound with fractal characteristic pattern aggregate.) be the preparation method who rarely contains the organic components fractal at present.The technology for preparing the fractal that contains organic/inorganic compounding composition in the experiment is still rare.
Summary of the invention
Purpose of the present invention provides a kind of and adopts simple chemical process to prepare the organic/inorganic composite parts, the preparation method of the fractal aggregate that contains quaternary ammonium salt and lithium halide that raw material is cheap and easy to get, repeatability is strong.
A kind of preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide of the present invention: this method may further comprise the steps:
Step 1: with concentration be 65% dimethyldiallylammonchloride chloride monomer and sodium-based montmorillonite by mass ratio X: 1,0.2≤X≤3 preparations, be scattered in the deionized water, in 20 ℃-30 ℃, continue mechanical stirring after 24 hours; Centrifugal, the washing, the oven dry, obtain dimethyldiallylammonium-polynite;
Step 2: with the dimethyldiallylammonium-polynite that makes, be scattered in concentration and be in the aqueous solution of ammonium persulphate of 10wt%, at 55 ℃ of lasting mechanical stirring 6-60 hours, and then centrifugal, washing, oven dry, make poly dimethyl allyl ammonium-polynite;
Step 3: the poly dimethyl allyl ammonium-polynite that makes is scattered in the tetrahydrofuran solvent, after 24 hours, adds lithium halide/tetrahydrofuran solution, follow 20 ℃ of-30 ℃ of lasting magnetic agitation after 48 hours 20 ℃ of-30 ℃ of lasting magnetic agitation; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium halide;
Step 4: the composite micelle that will gather resulting dimethyldiallylammonium-lithium halide with sebific duct drops on the clean substrate, behind the solvent flashing, obtains containing the fractal aggregate of quaternary ammonium salt and lithium halide in 20 ℃ of-30 ℃ of air atmospheres.
Described lithium halide is lithiumbromide or lithium chloride.
The invention has the beneficial effects as follows: owing to adopt technique scheme, synthesize the fractal aggregate that contains polymkeric substance and inorganic salt by simple chemical process, reaction conditions is controlled, raw material is cheap and easy to get, experimental installation is simple, repeatability is strong.
Description of drawings:
Fig. 1 is poly dimethyl allyl ammonium-lithium chloride fractal aggregate scanned photograph that 24 hours conditions of different monomers amount of the present invention, polymerization make: a) 2.6ml, b) 5.2ml, c) 13.0ml, d) 26.0ml.
Fig. 2 is 13.0ml for amount of monomer of the present invention, the poly dimethyl allyl ammonium that different polymerization times make-lithium chloride fractal aggregate scanned photograph: a) 6 hours, and b) 12 hours, c) 60 hours, d) poly dimethyl allyl ammonium-lithiumbromide fractal aggregate.
Embodiment:
Example one:
Step 1: with concentration is that 65% dimethyldiallylammonchloride chloride monomer 2.6ml and sodium-based montmorillonite 10.0g are scattered in the 200ml deionized water, 20 ℃ of lasting mechanical stirring after 24 hours; Centrifugal then, the washing, the oven dry, obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, 55 ℃ of lasting mechanical stirring after 24 hours, centrifugal then, the washing, the oven dry, obtain poly dimethyl allyl ammonium-polynite;
Step 3: with the poly dimethyl allyl ammonium-polynite that makes, be scattered in the tetrahydrofuran solvent of 30.0ml, under 25 ℃, continue magnetic agitation after 24 hours, lithium chloride/the tetrahydrofuran solution that adds 50.0ml, follow 25 ℃ of lasting magnetic agitation after 48 hours, again supernatant liquor is poured in the petroleum ether solvent after centrifugal, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 20 ℃, air atmosphere, behind the solvent flashing, obtain poly dimethyl allyl ammonium-lithium chloride fractal aggregate and (see Fig. 1 a).
Example two:
Step 1: with concentration is that 65% dimethyldiallylammonchloride chloride monomer 5.2ml and sodium-based montmorillonite 10.0g are scattered in the deionized water of 200.0ml, 25 ℃ of lasting mechanical stirring after 24 hours; Centrifugal again, the washing, the oven dry, obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, 55 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, the washing, the oven dry, obtain poly dimethyl allyl ammonium-polynite;
Step 3: described poly dimethyl allyl ammonium-polynite is scattered in the tetrahydrofuran solvent of 30.0ml, adds lithiumbromide/tetrahydrofuran solution of 50.0ml after 24 hours 25 ℃ of lasting magnetic agitation, then 25 ℃, continue magnetic agitation after 48 hours; In the petroleum ether solvent of after centrifugal supernatant liquor being poured into, obtain the composite micelle of poly dimethyl allyl ammonium-lithiumbromide;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithiumbromide is dropped on the clean substrate, in 25 ℃, air atmosphere, behind the solvent flashing, obtain containing the fractal aggregate of quaternary ammonium salt and lithiumbromide.Obtain poly dimethyl allyl ammonium-lithium chloride fractal aggregate (seeing Fig. 1 b).
Example three:
Step 1: step 1: getting concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, and sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 30 ℃, continued mechanical stirring 24 hours.Centrifugal, the washing, the oven dry, obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, and 55 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, add lithium chloride/tetrahydrofuran solution of 50.0ml after 24 hours, then 25 ℃ of lasting magnetic agitation after 48 hours 25 ℃ of lasting magnetic agitation; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 30 ℃, air atmosphere, behind the solvent flashing, obtain poly dimethyl allyl ammonium-lithium chloride fractal aggregate (seeing Fig. 1 c).
Example four:
Step 1: getting concentration is 65% dimethyldiallylammonchloride chloride monomer 26.0ml, sodium-based montmorillonite 10.0g is scattered in the 200.0ml deionized water, after 24 hours,, obtain dimethyldiallylammonium-polynite 25 ℃ of lasting mechanical stirring in centrifugal, washing, oven dry;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, and 55 ℃ of lasting mechanical stirring after 2 hours, centrifugal again, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, add lithiumbromide/tetrahydrofuran solution of 50.0ml after 24 hours, then 25 ℃ of lasting magnetic agitation 48 hours 25 ℃ of lasting magnetic agitation; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 25 ℃, air atmosphere, behind the solvent flashing, obtain poly dimethyl allyl ammonium-lithium chloride fractal aggregate (seeing Fig. 1 d).
Example five:
Step 1: getting concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 25 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, and 55 ℃ of lasting mechanical stirring after 6 hours, centrifugal again, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, 25 ℃, continue magnetic agitation adds 50.0ml after 24 hours lithium chloride/tetrahydrofuran solution, then 25 ℃, lasting magnetic agitation 48 hours; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 25 ℃ of air atmospheres, behind the solvent flashing, obtain poly dimethyl allyl ammonium-lithium chloride fractal aggregate and (see Fig. 2 a).
Example six:
Step 1: with concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 25 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain dimethyldiallylammonium-polynite;
Step 2: the dimethyldiallylammonium-polynite that makes is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, 55 ℃ of lasting mechanical stirring after 12 hours, centrifugal again, the washing, the oven dry, obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, 25 ℃, continue magnetic agitation adds 50.0ml after 24 hours lithium chloride/tetrahydrofuran solution, follow 25 ℃ of lasting magnetic agitation 48 hours; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 25 ℃, air atmosphere, behind the solvent flashing, obtain poly dimethyl allyl ammonium-lithium chloride fractal aggregate (seeing Fig. 2 b).
Example seven:
Step 1: with concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 25 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, and 55 ℃ of lasting mechanical stirring after 60 hours, centrifugal again, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, add lithium chloride/tetrahydrofuran solution of 50.0ml after 24 hours, then 25 ℃ of lasting magnetic agitation after 48 hours 25 ℃ of lasting magnetic agitation; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 25 ℃, air atmosphere, behind the solvent flashing, obtain poly dimethyl allyl ammonium-lithium chloride fractal aggregate (seeing Fig. 2 c).
Example eight:
Step 1: with concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 25 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, and 55 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, 25 ℃, continue magnetic agitation adds 50.0ml after 24 hours lithiumbromide/tetrahydrofuran solution, then 25 ℃, lasting magnetic agitation 48 hours; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithiumbromide;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 25 ℃ air atmosphere, behind the solvent flashing, obtain poly dimethyl allyl ammonium-lithiumbromide fractal aggregate (seeing Fig. 2 d).
Claims (10)
1. preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide: it is characterized in that this method may further comprise the steps:
Step 1: with concentration be 65% dimethyldiallylammonchloride chloride monomer and sodium-based montmorillonite by mass ratio X: 1,0.2≤X≤3 preparations, be scattered in the deionized water, in 20 ℃-30 ℃, continue mechanical stirring after 24 hours; Centrifugal, the washing, the oven dry, obtain dimethyldiallylammonium-polynite;
Step 2: with prepared dimethyldiallylammonium-polynite, be scattered in the aqueous solution that concentration is the 10wt% ammonium persulphate, at 55 ℃ of lasting mechanical stirring 6-60 hours, and then centrifugal, the washing, the oven dry, make poly dimethyl allyl ammonium-polynite;
Step 3: prepared poly dimethyl allyl ammonium-polynite is scattered in the tetrahydrofuran solvent, after 24 hours, adds lithium halide/tetrahydrofuran solution, follow 20 ℃ of-30 ℃ of lasting magnetic agitation after 48 hours 20 ℃ of-30 ℃ of lasting magnetic agitation; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium halide;
Step 4: the composite micelle that will gather resulting dimethyldiallylammonium-lithium halide with sebific duct drops on the clean substrate, behind the solvent flashing, obtains containing the fractal aggregate of quaternary ammonium salt and lithium halide in 20 ℃ of-30 ℃ of air atmospheres.
2. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that, described lithium halide is lithium chloride or lithiumbromide.
3. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that,
Step 1: with concentration is that 65% dimethyldiallylammonchloride chloride monomer 2.6ml and sodium-based montmorillonite 10.0g are scattered in the 200ml deionized water, 20 ℃ of lasting mechanical stirring after 24 hours; Centrifugal then, the washing, the oven dry, obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, 55 ℃ of lasting mechanical stirring after 24 hours, centrifugal then, the washing, the oven dry, obtain poly dimethyl allyl ammonium-polynite;
Step 3: with the poly dimethyl allyl ammonium-polynite that makes, be scattered in the tetrahydrofuran solvent of 30.0ml, under 25 ℃, continue magnetic agitation after 24 hours, lithium chloride/the tetrahydrofuran solution that adds 50.0ml, follow 25 ℃ of lasting magnetic agitation after 48 hours, again supernatant liquor is poured in the petroleum ether solvent after centrifugal, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 20 ℃, air atmosphere, behind the solvent flashing, obtain containing the fractal aggregate of quaternary ammonium salt and lithium chloride.
4. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that, this method may further comprise the steps:
Step 1: with concentration is that 65% dimethyldiallylammonchloride chloride monomer 5.2ml and sodium-based montmorillonite 10.0g are scattered in the deionized water of 200.0ml, 25 ℃ of lasting mechanical stirring after 24 hours; Centrifugal again, the washing, the oven dry, obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, 55 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, the washing, the oven dry, obtain poly dimethyl allyl ammonium-polynite;
Step 3: described poly dimethyl allyl ammonium-polynite is scattered in the tetrahydrofuran solvent of 30.0ml, adds lithium chloride/tetrahydrofuran solution of 50.0ml after 24 hours 25 ℃ of lasting magnetic agitation, then 25 ℃, continue magnetic agitation after 48 hours; In the petroleum ether solvent of after centrifugal supernatant liquor being poured into, obtain the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithiumbromide is dropped on the clean substrate, in 25 ℃, air atmosphere, behind the solvent flashing, obtain containing the fractal aggregate of quaternary ammonium salt and lithium chloride.
5. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that, this method may further comprise the steps:
Step 1: getting concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, and sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 30 ℃, continued mechanical stirring 24 hours.Centrifugal, the washing, the oven dry, obtain dimethyldiallylammonium-polynite;
Step 2: the dimethyldiallylammonium-polynite that makes is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, 55 ℃, continue mechanical stirring 24 hours, centrifugal, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, add lithium chloride/tetrahydrofuran solution of 50.0ml after 24 hours, then 25 ℃ of lasting magnetic agitation after 48 hours 25 ℃ of lasting magnetic agitation; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 30 ℃, air atmosphere, behind the solvent flashing, obtain containing the fractal aggregate of quaternary ammonium salt and lithium chloride.
6. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that, this method may further comprise the steps:
Step 1: getting concentration is 65% dimethyldiallylammonchloride chloride monomer 26.0ml, sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, after 24 hours,, obtain dimethyldiallylammonium-polynite 25 ℃ of lasting mechanical stirring in centrifugal, washing, oven dry;
Step 2: the dimethyldiallylammonium-polynite that makes is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, 55 ℃ of lasting mechanical stirring after 26 hours, centrifugal again, the washing, the oven dry, obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, add lithium chloride/tetrahydrofuran solution of 50.0ml after 24 hours, then 25 ℃ of lasting magnetic agitation 48 hours 25 ℃ of lasting magnetic agitation; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 30 ℃, air atmosphere, behind the solvent flashing, obtain containing the fractal aggregate of quaternary ammonium salt and lithium chloride.
7. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that, this method may further comprise the steps:
Step 1: getting concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 30 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, and 55 ℃ of lasting mechanical stirring after 6 hours, centrifugal again, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, 25 ℃, continue magnetic agitation adds 50.0ml after 24 hours lithium chloride/tetrahydrofuran solution, then 25 ℃, lasting magnetic agitation 48 hours; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 25 ℃ of air atmospheres, behind the solvent flashing, obtain containing the fractal aggregate of quaternary ammonium salt and lithium chloride.
8. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that, this method may further comprise the steps:
Step 1: with concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, sodium-based montmorillonite 10.0g is scattered in the 200.0ml deionized water, 25 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain dimethyldiallylammonium-polynite;
Step 2: the dimethyldiallylammonium-polynite that makes is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, 55 ℃ of lasting mechanical stirring after 12 hours, centrifugal again, the washing, the oven dry, obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, 25 ℃, continue magnetic agitation adds 50.0ml after 24 hours lithium chloride/tetrahydrofuran solution, follow 25 ℃ of lasting magnetic agitation 48 hours; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 25 ℃, air atmosphere, behind the solvent flashing, obtain poly dimethyl allyl ammonium-lithium chloride fractal aggregate
9. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that, this method may further comprise the steps:
Step 1: with concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 25 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of ammonium persulphate that 200.0ml concentration is 10wt%, and 55 ℃ of lasting mechanical stirring after 60 hours, centrifugal again, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, add lithium chloride/tetrahydrofuran solution of 50.0ml after 24 hours, then 25 ℃ of lasting magnetic agitation after 48 hours 25 ℃ of lasting magnetic agitation; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithium chloride;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithium chloride is dropped on the clean substrate, in 25 ℃, air atmosphere, behind the solvent flashing, obtain containing the fractal aggregate of quaternary ammonium salt and lithium chloride
10. the preparation method who contains the fractal aggregate of quaternary ammonium salt and lithium halide according to claim 1 is characterized in that,
Step 1: with concentration is 65% dimethyldiallylammonchloride chloride monomer 13.0ml, sodium-based montmorillonite 10.0g is scattered in the deionized water of 200.0ml, 25 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain dimethyldiallylammonium-polynite;
Step 2: described dimethyldiallylammonium-polynite is scattered in the aqueous solution of peracid ammonium that 200.0ml concentration is 10wt%, and 55 ℃ of lasting mechanical stirring after 24 hours, centrifugal again, washing, oven dry obtain poly dimethyl allyl ammonium-polynite;
Step 3: with described poly dimethyl allyl ammonium-polynite, be scattered in the tetrahydrofuran solvent of 30.0ml, 25 ℃, continue magnetic agitation adds 50.0ml after 24 hours lithiumbromide/tetrahydrofuran solution, then 25 ℃, lasting magnetic agitation 48 hours; After centrifugal supernatant liquor is poured in the petroleum ether solvent, obtained the composite micelle of poly dimethyl allyl ammonium-lithiumbromide;
Step 4: the composite micelle of described poly dimethyl allyl ammonium-lithiumbromide is dropped on the clean substrate, in 25 ℃ air atmosphere, behind the solvent flashing, obtain containing the fractal aggregate of quaternary ammonium salt and lithiumbromide.
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| CN110282715A (en) * | 2019-07-16 | 2019-09-27 | 闽江学院 | A kind of preparation and application of polyquaternium In-situ reaction improved PFS |
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| US4833009A (en) * | 1988-03-25 | 1989-05-23 | E. I. Du Pont De Nemours And Company | Purification of condensation products |
| JPH04503223A (en) * | 1989-01-24 | 1992-06-11 | ザ・ダウ・ケミカル・カンパニー | Aggregates or clusters of water-swellable polymers that have a greater hydration rate than unassociated water-swellable polymers |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104148667A (en) * | 2014-08-14 | 2014-11-19 | 青岛大学 | Method for preparing fractal aggregate with gas sensitivity and reversibility of metal nanoparticles |
| CN104148667B (en) * | 2014-08-14 | 2016-04-20 | 青岛大学 | The preparation method of the reversible fractal aggregate of a kind of vapor sensitivity metal nanoparticle |
| CN110282715A (en) * | 2019-07-16 | 2019-09-27 | 闽江学院 | A kind of preparation and application of polyquaternium In-situ reaction improved PFS |
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