CN107243303A - A kind of method for preparing phosphorus alkene hydrogel material - Google Patents
A kind of method for preparing phosphorus alkene hydrogel material Download PDFInfo
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- CN107243303A CN107243303A CN201710494870.2A CN201710494870A CN107243303A CN 107243303 A CN107243303 A CN 107243303A CN 201710494870 A CN201710494870 A CN 201710494870A CN 107243303 A CN107243303 A CN 107243303A
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- Prior art keywords
- phosphorus alkene
- hydrogel material
- nitrogen
- containing compound
- phosphorus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
Abstract
The invention discloses a kind of method for preparing phosphorus alkene hydrogel material, including：Phosphorus alkene and nitrogen-containing compound are together placed in solution and be uniformly dispersed, the consumption of phosphorus alkene accounts for the 5%~95% of phosphorus alkene and nitrogen-containing compound gross mass, so that phosphorus alkene/nitrogen-containing compound mixed solution is made；Phosphorus alkene/nitrogen-containing compound the mixed solution is placed in water heating kettle, and 1~72h hydro-thermal reaction is carried out under conditions of 50~220 DEG C, room temperature is then cooled to, so that phosphorus alkene hydrogel material is made.The present invention can not only effectively prepare phosphorus alkene hydrogel material, 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 phosphorus alkene field of compound material, more particularly to a kind of method for preparing phosphorus alkene hydrogel material.
Background technology
Phosphorus alkene material is new 2D nano lamellar materials, and it has wide answer in fields such as electronic communication, communications and transportation
Use prospect.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.Existing phosphorus alkene material is usually film or powdered, and it can significantly be limited when different field is applied.
In the prior art, the phosphorus alkene material specific surface area of preparation is smaller, and mechanical performance is also weaker, in addition to the layer of phosphorus alkene
Folded phenomenon and the shortcoming for being oxidized easily erosion do not have good processing method, and phosphorus alkene hydrogel material and its conjunction do not occur
Into method.
The content of the invention
For above-mentioned weak point of the prior art, the invention provides a kind of side for preparing phosphorus alkene hydrogel material
Method, can not only effectively prepare phosphorus alkene hydrogel material, and simple to operate, low for equipment requirements, good product quality, yield
Height, is very suitable for carrying out large-scale production.The phosphorus alkene hydrogel material is a kind of phosphorus alkene material based on three-dimensional porous structure, tool
There are huge specific surface area and good electric conductivity and heat conductivility, not only can effectively prevent the lamella of phosphorus alkene from stacking,
And can effectively suppress the erosion of oxygen and water to phosphorus alkene, it is ensured that the special performance of phosphorus alkene is not destroyed, therefore can be answered extensively
For fields such as electrochemical energy storage, electronic communications.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method for preparing phosphorus alkene hydrogel material, comprises the following steps：
Step A, phosphorus alkene and nitrogen-containing compound is together placed in solution and be uniformly dispersed, the consumption of phosphorus alkene accounts for phosphorus alkene and contained
The 5%~95% of nitrogen compound gross mass, so that phosphorus alkene/nitrogen-containing compound mixed solution is made；
Step B, the phosphorus alkene/nitrogen-containing compound mixed solution is placed in water heating kettle, and under conditions of 50~220 DEG C
1~72h hydro-thermal reaction is carried out, room temperature is then cooled to, so that phosphorus alkene hydrogel material is made.
Preferably, described nitrogen-containing compound be glucose, urea, phytic acid, reduced glutathione, ethylenediamine in extremely
Few one kind.
Preferably, the solution be water, methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride, acetonitrile, ether,
Petroleum ether, pentane, hexane, carbon disulfide, dichloromethane, dichloroethanes, chloroform, trichloroethanes, ethyl acetate, butanone,
Benzene,toluene,xylene, hexamethylene, N,N-dimethylformamide, formaldehyde, sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid, ammoniacal liquor, water
Close at least one of hydrazine, 1-METHYLPYRROLIDONE.
Preferably, scattered described in step A is the ultrasonic disperse that 1~360min is carried out using ultrasonic device.
As seen from the above technical solution provided by the invention, the phosphorus alkene hydrogel material provided by the present invention of preparing
Method carries out hydro-thermal process to the mixed solution of phosphorus alkene and nitrogen-containing compound, and by phosphorus alkene and nitrogen-containing compound ratio, water
Thermal response temperature, the hydro-thermal reaction time are controlled, so as to effectively prepare phosphorus alkene hydrogel material；The phosphorus alkene hydrogel material
It is a kind of phosphorus alkene material based on three-dimensional porous structure, with huge specific surface area and good electric conductivity and thermal conductivity
Can, it not only can effectively prevent the lamella of phosphorus alkene from stacking, and can effectively suppress the erosion of oxygen and water to phosphorus alkene, it is ensured that phosphorus
The special performance of alkene is not destroyed, therefore can be widely used for the fields such as electrochemical energy storage, electronic communication.The phosphorus is prepared in the present invention
The method of alkene hydrogel material is simple to operate, low for equipment requirements, good product quality, yield are high, is very suitable for carrying out 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 method provided by the present invention for preparing phosphorus alkene hydrogel material is described in detail below.
A kind of method for preparing phosphorus alkene hydrogel material, comprises the following steps：
Step A, phosphorus alkene and nitrogen-containing compound is together placed in solution, the consumption of phosphorus alkene accounts for phosphorus alkene and nitrogen-containing compound is total
The 5%~95% of quality, then the ultrasonic disperse for carrying out 1~360min using ultrasonic device are allowed to be uniformly dispersed, so that phosphorus is made
Alkene/nitrogen-containing compound mixed solution.Wherein, described nitrogen-containing compound be glucose, urea, phytic acid, reduced glutathione,
At least one of ethylenediamine.The 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,toluene,xylene, hexamethylene, N,N-dimethylformamide, formaldehyde, sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid, ammoniacal liquor,
At least one of hydrazine hydrate, 1-METHYLPYRROLIDONE.
Step B, the phosphorus alkene/nitrogen-containing compound mixed solution is placed in water heating kettle, and under conditions of 50~220 DEG C
1~72h hydro-thermal reaction is carried out, room temperature is then cooled to, so that phosphorus alkene hydrogel material is made.
Specifically, mixing of the method provided by the present invention for preparing phosphorus alkene hydrogel material to phosphorus alkene and nitrogen-containing compound
Solution carries out hydro-thermal process, and by being controlled to phosphorus alkene and nitrogen-containing compound ratio, hydrothermal temperature, the hydro-thermal reaction time
System, so as to effectively prepare phosphorus alkene hydrogel material；The phosphorus alkene hydrogel material is a kind of phosphorus alkene based on three-dimensional porous structure
Material, with huge specific surface area and good electric conductivity and heat conductivility, not only can effectively prevent the piece of phosphorus alkene
Layer is stacked, and can effectively suppress the erosion of oxygen and water to phosphorus alkene, it is ensured that the special performance of phosphorus alkene is not destroyed, therefore can
It is widely used in the fields such as electrochemical energy storage, electronic communication.The method operation letter of the phosphorus alkene hydrogel material is prepared in the present invention
Single, low for equipment requirements, good product quality, yield are high, are 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 method that what body embodiment was provided the embodiment of the present invention prepare phosphorus alkene hydrogel material is described in detail.
Embodiment 1
A kind of method for preparing phosphorus alkene hydrogel material, comprises the following steps：
Step a1,1g phosphorus alkene and 10g urea is together placed in water, and carries out using ultrasonic device 5min ultrasonic disperse
It is allowed to be uniformly dispersed, so that phosphorus alkene/nitrogen-containing compound mixed solution is made.
Step b1, the phosphorus alkene/nitrogen-containing compound mixed solution is placed in water heating kettle, and carried out under conditions of 65 DEG C
72h hydro-thermal reaction, is then cooled to room temperature, so that phosphorus alkene hydrogel material as shown in Figure 1 is made.
Embodiment 2
A kind of method for preparing phosphorus alkene hydrogel material, comprises the following steps：
Step a2,1g phosphorus alkene and 3g glucose is together placed in ethanol, and carries out using ultrasonic device 60min ultrasound
It is scattered to be allowed to be uniformly dispersed, so that phosphorus alkene/nitrogen-containing compound mixed solution is made.
Step b2, the phosphorus alkene/nitrogen-containing compound mixed solution is placed in water heating kettle, and entered under conditions of 100 DEG C
Row 48h hydro-thermal reaction, is then cooled to room temperature, so that phosphorus alkene hydrogel material is made.
Embodiment 3
A kind of method for preparing phosphorus alkene hydrogel material, comprises the following steps：
Step a3,1g phosphorus alkene and 1g phytic acid is together placed in acetone, and carries out using ultrasonic device 120min ultrasound
It is scattered to be allowed to be uniformly dispersed, so that phosphorus alkene/nitrogen-containing compound mixed solution is made.
Step b3, the phosphorus alkene/nitrogen-containing compound mixed solution is placed in water heating kettle, and entered under conditions of 150 DEG C
Row 12h hydro-thermal reaction, is then cooled to room temperature, so that phosphorus alkene hydrogel material is made.
Embodiment 4
A kind of method for preparing phosphorus alkene hydrogel material, comprises the following steps：
Step a4,1g phosphorus alkene and 0.2g ethylenediamines and urea admixture is together placed in petroleum ether and cyclohexane solution,
And carry out 240min ultrasonic disperse and be allowed to be uniformly dispersed, so that phosphorus alkene/nitrogen-containing compound mixed solution is made.
Step b4, the phosphorus alkene/nitrogen-containing compound mixed solution is placed in water heating kettle, and entered under conditions of 180 DEG C
Row 6h hydro-thermal reaction, is then cooled to room temperature, so that phosphorus alkene hydrogel material is made.
Embodiment 5
A kind of method for preparing phosphorus alkene hydrogel material, comprises the following steps：
Step a5,1g phosphorus alkene and 0.09g glucose and reduced glutathione mixture is together placed in ammoniacal liquor and acetic acid
In ethyl ester solution, and carry out 360min ultrasonic disperse and be allowed to be uniformly dispersed, so that it is molten that phosphorus alkene/nitrogen-containing compound mixing is made
Liquid.
Step b5, the phosphorus alkene/nitrogen-containing compound mixed solution is placed in water heating kettle, and entered under conditions of 210 DEG C
Row 1.5h hydro-thermal reaction, is then cooled to room temperature, so that phosphorus alkene hydrogel material is made.
As fully visible, the embodiment of the present invention can not only effectively prepare phosphorus alkene hydrogel material, and simple to operate, right
Equipment requirement is low, good product quality, yield high, is very suitable for carrying out large-scale production.The phosphorus alkene hydrogel material is a kind of base
In the phosphorus alkene material of three-dimensional porous structure, with huge specific surface area and good electric conductivity and heat conductivility, not only
Can effectively prevent the lamella of phosphorus alkene from stacking, and can effectively suppress the erosion of oxygen and water to phosphorus alkene, it is ensured that phosphorus alkene it is only
Characteristic can not be destroyed, therefore can be widely applied to the fields such as electrochemical energy storage, electronic communication.
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 (4)
1. a kind of method for preparing phosphorus alkene hydrogel material, it is characterised in that comprise the following steps：
Step A, phosphorus alkene and nitrogen-containing compound is together placed in solution and be uniformly dispersed, the consumption of phosphorus alkene accounts for phosphorus alkene and nitrogen
The 5%~95% of compound gross mass, so that phosphorus alkene/nitrogen-containing compound mixed solution is made；
Step B, the phosphorus alkene/nitrogen-containing compound mixed solution is placed in water heating kettle, and carried out under conditions of 50~220 DEG C
1~72h hydro-thermal reaction, is then cooled to room temperature, so that phosphorus alkene hydrogel material is made.
2. the method according to claim 1 for preparing phosphorus alkene hydrogel material, it is characterised in that described nitrogen-containing compound
For at least one of glucose, urea, phytic acid, reduced glutathione, ethylenediamine.
3. the method according to claim 1 or 2 for preparing phosphorus alkene hydrogel material, it is characterised in that the solution be water,
Methanol, ethanol, propyl alcohol, acetone, tetrahydrofuran, carbon tetrachloride, acetonitrile, ether, petroleum ether, pentane, hexane, carbon disulfide, two
Chloromethanes, dichloroethanes, chloroform, trichloroethanes, ethyl acetate, butanone, benzene,toluene,xylene, hexamethylene, N, N- bis-
At least one in NMF, formaldehyde, sulfuric acid, hydrochloric acid, nitric acid, acetic acid, propionic acid, ammoniacal liquor, hydrazine hydrate, 1-METHYLPYRROLIDONE
Kind.
4. the method according to claim 1 or 2 for preparing phosphorus alkene hydrogel material, it is characterised in that described in step A
Scattered is the ultrasonic disperse for being carried out using ultrasonic device 1~360min.
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| CN201710494870.2A CN107243303A (en) | 2017-06-26 | 2017-06-26 | A kind of method for preparing phosphorus alkene hydrogel material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110947344A (en) * | 2019-12-11 | 2020-04-03 | 哈尔滨工程大学 | Hydrogel and preparation method thereof and application of hydrogel in preparation of sensing chip |
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| CN104310389A (en) * | 2014-10-22 | 2015-01-28 | 福州大学 | Compressive graphene hydrogel and preparation method thereof |
| CN105535971A (en) * | 2015-12-22 | 2016-05-04 | 苏州大学 | A black phosphorus nanometer particle with biocompatibility, a preparing method thereof and applications of the black phosphorus nanometer particle |
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| CN102849731A (en) * | 2012-09-07 | 2013-01-02 | 中国科学技术大学 | Nitrogen-doped graphene hydrogel, preparation method and applications thereof |
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Application publication date: 20171013 |