CN107266682A - A kind of preparation method of phosphorus alkene poly-dopamine composite - Google Patents
A kind of preparation method of phosphorus alkene poly-dopamine composite Download PDFInfo
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- CN107266682A CN107266682A CN201710494302.2A CN201710494302A CN107266682A CN 107266682 A CN107266682 A CN 107266682A CN 201710494302 A CN201710494302 A CN 201710494302A CN 107266682 A CN107266682 A CN 107266682A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0666—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0672—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a kind of preparation method of phosphorus alkene poly-dopamine composite, including：Phosphorus alkene is placed in the solution that pH value is 7~10,0.1~48h of ultrasonic disperse obtains phosphorus alkene solution；Dopamine hydrochloride is placed in the phosphorus alkene solution and ultrasonic disperse, precursor solution is obtained；The precursor solution is carried out to 1~72h hydro-thermal process under conditions of 50~150 DEG C, separation of solid and liquid is then carried out, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene poly-dopamine composite is made.The present invention can not only effectively prepare the phosphorus alkene poly-dopamine material for having both phosphorus alkene and poly-dopamine advantages concurrently, and simple to operate, low for equipment requirements, good product quality, yield are high, be very suitable for carrying out large-scale production.
Description
Technical field
The present invention relates to the preparation side of phosphorus alkene field of compound material, more particularly to a kind of phosphorus alkene-poly-dopamine composite
Method.
Background technology
Phosphorus alkene material be by the tightly packed new phosphorus nano material into bi-dimensional cellular shape lattice structure of individual layer phosphorus atoms, its
Special stable micro-structure makes it have excellent chemical property and heat-conductive characteristic, therefore phosphorus alkene material is logical in electronics
The fields such as letter, communications and transportation have broad prospect of application.
Phosphorus alkene material because phosphorus atoms interlayer have stronger Van der Waals force, it is prone to stratification and form similar film
Laminated structure, this structure can cause specific surface area significantly to reduce, thus can the distinctive absorption of heavy losses phosphorus alkene, it is conductive,
The excellent properties such as heat conduction.In addition, the stronger chemism of phosphorus alkene makes it easily be corroded by materials such as oxygen gas and waters and lose original property
Energy.The water-oil separating performance of phosphorus alkene is poor, can lose separating property because environment is different when in use.
In the prior art, the phosphorus alkene material specific surface area of preparation is smaller, and water-oil separating performance is weaker, in addition to phosphorus alkene
Stratification does not have good processing method with the shortcoming for being oxidized easily erosion, and it is compound phosphorus alkene-poly-dopamine do not occur
Material and its synthetic method.
The content of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of phosphorus alkene-poly-dopamine composite
Preparation method, can not only effectively prepare the phosphorus alkene-poly-dopamine material for having both phosphorus alkene and poly-dopamine advantages concurrently, and
Simple to operate, low for equipment requirements, good product quality, yield are high, are very suitable for carrying out large-scale production.The phosphorus alkene-poly- DOPA
Amine material has good mechanical performance and excellent adhesion property and gas liquid separating property, can be widely applied to gas-liquid
The field such as isolate and purify.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of phosphorus alkene-poly-dopamine composite, comprises the following steps：
Step A, phosphorus alkene is placed in the solution that pH value is 7~10,0.1~48h of ultrasonic disperse obtains phosphorus alkene solution；
Step B, Dopamine hydrochloride is placed in the phosphorus alkene solution and ultrasonic disperse, obtains precursor solution；
Step C, the hydro-thermal process that the precursor solution is carried out to 1~72h under conditions of 50~150 DEG C, Ran Houjin
Row separation of solid and liquid, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite is made.
Preferably, described solution is water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride, acetonitrile, second
Ether, petroleum ether, pentane, hexane, carbon disulfide, dichloromethane, dichloroethanes, chloroform, trichloroethanes, ethyl acetate, fourth
Ketone, benzene, hexamethylene, N,N-dimethylformamide, formaldehyde, sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid, ammoniacal liquor, hydrazine hydrate, N- first
At least one of base pyrrolidones.
Preferably, it is described by phosphorus alkene be placed in pH value be 7~10 solution include：When the pH value of solution is not 7~10
When, Tris-HCl buffer solutions regulation pH value is added into the solution, until the pH value of the solution is 7~10.
As seen from the above technical solution provided by the invention, phosphorus alkene-poly-dopamine composite wood provided by the present invention
Phosphorus alkene is placed in the solution that pH value is 7~10 by the preparation method of material, and is adding the laggard water-filling heat treatment of Dopamine hydrochloride, is led to
Reaction time and the reaction temperature of control hydro-thermal process are crossed, so that phosphorus alkene-poly-dopamine composite has been made；The phosphorus alkene-poly-
Dopamine material has that the two-fold advantage of phosphorus alkene and poly-dopamine, specific surface area be big, good mechanical property, and with good gas
Body, the stalling characteristic of liquid and excellent stability and flexibility, can be widely applied to the fields such as gas-liquid separation purifying.The present invention
The preparation method of the phosphorus alkene-poly-dopamine composite provided is simple to operate, low for equipment requirements, good product quality, yield
Height, is very suitable for carrying out large-scale production.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is the electron scanning micrograph of the N doping phosphorus alkene prepared by the embodiment of the present invention 1.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
The preparation method to phosphorus alkene-poly-dopamine composite provided by the present invention is described in detail below.
A kind of preparation method of phosphorus alkene-poly-dopamine composite, comprises the following steps：
Step A, phosphorus alkene is placed in the solution that pH value is 7~10,0.1~48h of ultrasonic disperse obtains phosphorus alkene solution.Its
In, when the pH value of solution is not 7~10, Tris-HCl buffer solutions regulation pH value can be added into the solution, until molten
The pH value of liquid is 7~10.Described solution is water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride, acetonitrile, second
Ether, petroleum ether, pentane, hexane, carbon disulfide, dichloromethane, dichloroethanes, chloroform, trichloroethanes, ethyl acetate, fourth
Ketone, benzene, hexamethylene, N,N-dimethylformamide, formaldehyde, sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid, ammoniacal liquor, hydrazine hydrate, N- first
At least one of base pyrrolidones.
Step B, Dopamine hydrochloride is placed in the phosphorus alkene solution and ultrasonic disperse, obtains precursor solution.
Step C, the hydro-thermal process that the precursor solution is carried out to 1~72h under conditions of 50~150 DEG C, Ran Houjin
Row separation of solid and liquid, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite is made.
Specifically, it is 7 that phosphorus alkene is placed in pH value by the preparation method of phosphorus alkene-poly-dopamine composite provided by the present invention
In~10 solution, and Dopamine hydrochloride laggard water-filling heat treatment is being added, by controlling reaction time of hydro-thermal process and anti-
Temperature is answered, so that phosphorus alkene-poly-dopamine composite has been made；Phosphorus alkene-poly-dopamine the material has phosphorus alkene and poly-dopamine
Two-fold advantage, specific surface area is big, good mechanical property, and with good gas, the stalling characteristic of liquid and excellent
Stability and flexibility, can be widely applied to the fields such as gas-liquid separation purifying.Phosphorus alkene-poly-dopamine composite wood provided by the present invention
The preparation method of material is simple to operate, low for equipment requirements, good product quality, yield are high, is very suitable for carrying out large-scale production.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with tool
The preparation method for phosphorus alkene-poly-dopamine composite that body embodiment is provided the embodiment of the present invention is described in detail.
Embodiment 1
A kind of preparation method of phosphorus alkene-poly-dopamine composite, comprises the following steps：
Step a1,0.1g phosphorus alkene is placed in the water that pH value is 7.5, ultrasonic disperse 0.5h obtains phosphorus alkene solution.
Step b1,0.1g Dopamine hydrochlorides are placed in the phosphorus alkene solution and ultrasonic disperse, obtain precursor solution.
Step c1, the hydro-thermal process that the precursor solution is carried out to 72h under conditions of 60 DEG C, then carry out solid-liquid point
From, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite as shown in Figure 1 is made.
Embodiment 2
A kind of preparation method of phosphorus alkene-poly-dopamine composite, comprises the following steps：
Step a2,0.1g phosphorus alkene is placed in the water and alcohol mixed solution that pH value is 8, ultrasonic disperse 5h obtains phosphorus alkene
Solution.
Step b2,0.5g Dopamine hydrochlorides are placed in the phosphorus alkene solution and ultrasonic disperse, obtain precursor solution.
Step c2, the hydro-thermal process that the precursor solution is carried out to 50h under conditions of 80 DEG C, then carry out solid-liquid point
From, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite is made.
Embodiment 3
A kind of preparation method of phosphorus alkene-poly-dopamine composite, comprises the following steps：
Step a3,0.1g phosphorus alkene is placed in the DMF solution that pH value is 8.5, ultrasonic disperse 24h is obtained
To phosphorus alkene solution.
Step b3,1g Dopamine hydrochlorides are placed in the phosphorus alkene solution and ultrasonic disperse, obtain precursor solution.
Step c3, the hydro-thermal process that the precursor solution is carried out to 24h under conditions of 100 DEG C, then carry out solid-liquid
Separation, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite is made.
Embodiment 4
A kind of preparation method of phosphorus alkene-poly-dopamine composite, comprises the following steps：
Step a4,0.1g phosphorus alkene is placed in the ethyl acetate solution that pH value is 9.5, ultrasonic disperse 48h obtains phosphorus alkene molten
Liquid.
Step b4,1.5g Dopamine hydrochlorides are placed in the phosphorus alkene solution and ultrasonic disperse, obtain precursor solution.
Step c4, the hydro-thermal process that the precursor solution is carried out to 1.5h under conditions of 150 DEG C, then carry out solid-liquid
Separation, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite is made.
As fully visible, the embodiment of the present invention can not only effectively prepare the phosphorus for having both phosphorus alkene and poly-dopamine advantages concurrently
Alkene-poly-dopamine material, and simple to operate, low for equipment requirements, good product quality, yield are high, are very suitable for carry out scale
Metaplasia is produced.Phosphorus alkene-poly-dopamine the material has good mechanical performance and excellent adhesion property and gas liquid separation
Performance, can be widely applied to the fields such as gas-liquid separation purifying.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (3)
1. a kind of preparation method of phosphorus alkene-poly-dopamine composite, it is characterised in that comprise the following steps：
Step A, phosphorus alkene is placed in the solution that pH value is 7~10,0.1~48h of ultrasonic disperse obtains phosphorus alkene solution；
Step B, Dopamine hydrochloride is placed in the phosphorus alkene solution and ultrasonic disperse, obtains precursor solution；
Step C, the hydro-thermal process that the precursor solution is carried out to 1~72h under conditions of 50~150 DEG C, are then consolidated
Liquid is separated, and the solid that separation of solid and liquid is obtained is dried, so that phosphorus alkene-poly-dopamine composite is made.
2. the preparation method of phosphorus alkene-poly-dopamine composite according to claim 1, it is characterised in that described is molten
Liquid is water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride, acetonitrile, ether, petroleum ether, pentane, hexane, two sulphur
Change carbon, dichloromethane, dichloroethanes, chloroform, trichloroethanes, ethyl acetate, butanone, benzene, hexamethylene, N, N- dimethyl methyls
At least one of acid amides, formaldehyde, sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid, ammoniacal liquor, hydrazine hydrate, 1-METHYLPYRROLIDONE.
3. the preparation method of phosphorus alkene-poly-dopamine composite according to claim 1, it is characterised in that described general
Phosphorus alkene, which is placed in the solution that pH value is 7~10, to be included：When the pH value of solution is not 7~10, Tris- is added into the solution
HCl buffer solutions adjust pH value, until the pH value of the solution is 7~10.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254916A (en) * | 2015-09-30 | 2016-01-20 | 西南交通大学 | Preparation method for oxidized graphene-poly-dopamine composite aerogel |
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- 2017-06-26 CN CN201710494302.2A patent/CN107266682A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254916A (en) * | 2015-09-30 | 2016-01-20 | 西南交通大学 | Preparation method for oxidized graphene-poly-dopamine composite aerogel |
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Application publication date: 20171020 |