CN109369925A - A kind of chance water discoloration covalent organic framework material and its preparation method and application - Google Patents
A kind of chance water discoloration covalent organic framework material and its preparation method and application Download PDFInfo
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- CN109369925A CN109369925A CN201811188065.8A CN201811188065A CN109369925A CN 109369925 A CN109369925 A CN 109369925A CN 201811188065 A CN201811188065 A CN 201811188065A CN 109369925 A CN109369925 A CN 109369925A
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- organic framework
- framework material
- covalent organic
- chance water
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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
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/81—Indicating humidity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
Abstract
The present invention relates to a kind of chance water discoloration covalent organic framework materials and its preparation method and application.Covalent organic framework material is synthesized by indoor temperature solid phase method using p-phenylenediamine and trifonnyl phenol as synthon first.Covalent organic framework material specific surface area of the invention is big, pore structure is abundant, it is by forming hydrogen bond to change it to energy level between hydrone, to change its color, the application new in catalytic field of covalent organic framework material is expanded, and preparation method has simple process, easy repetitive operation, structure-controllable, it is suitable for mass production the advantages that.
Description
Technical field
The invention belongs to porous material technical field, in particular to a kind of preparation for meeting water discoloration covalent organic framework material
Method, and expand the potential application of covalent organic framework material.
Background technique
Covalent organic framework material is the porous material of crystalline form formed with light elements such as C, N, O, B, Si by Covalent bonding together
Material, since COF has high stability, structural regularity, hole adjustability, easily functionality, to apply in gas storage, drug
The fields such as release, catalysis and photoelectricity.
In the recent period, covalent organic framework material is as a kind of novel porous carbon sill of sheet due to its unique performance such as rigidity
Structure (two dimension or three-dimensional), lower density, high stability and large specific surface area and gap etc. are concerned, these are special
Point makes it be expected to solve the defects of non-metallic catalyst activity is low, stability is poor.The common synthesis side of covalent organic framework material
Method has solvent-thermal method, ionothermal synthesis, microwave heating method etc..CN103755588A discloses a kind of novel covalent organic framework light and urges
Agent and preparation method thereof, with equal benzene trioxin and 2,5- bis- (N, N- dimethyl) amino-two hydrazides of Isosorbide-5-Nitrae-benzene is to close for the invention
Covalent organic framework material is made using solvent-thermal method at monomer, this method generated time is long, the difficult regulation of reaction, is unfavorable for advising greatly
Mould synthesis.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention utilizes settled process, synthesizes under room temperature and open system
A kind of covalent organic framework material.This synthetic method is with the reaction time is short, low energy consumption, non-volatility organic pollution, behaviour
Make the advantages that simple, while obtained covalent organic framework material has the performance for meeting water discoloration.
The technical solution adopted by the present invention is that: a kind of chance water discoloration covalent organic framework material, preparation method includes following
Step: organic solvent and glacial acetic acid are dispersed in distilled water, form mixed solution；By p-phenylenediamine and trifonnyl phenol point
It is dispersed in and is formed by mixed solution, at room temperature after uniform stirring 0.1-0.5h, stand, filtering, obtained solid powder is successively used
After tetrahydrofuran and acetone washing, 12 are dried in vacuo in 80 DEG C, target product is obtained and meets water discoloration covalent organic framework material.
Further, above-mentioned a kind of chance water discoloration covalent organic framework material, in molar ratio, p-phenylenediamine: three formyls
Base phenol=2:3.
Further, a kind of above-mentioned chance water changes colour covalent organic framework material, the organic solvent be tetrahydrofuran,
One or two or more kinds of mixing of 1,3,5- trimethylbenzene, toluene, dioxane, ethyl alcohol, n-butanol and o-dichlorohenzene.
Further, above-mentioned a kind of chance water discoloration covalent organic framework material, the organic solvent is dioxy six
The mixing of ring and 1,3,5- trimethylbenzene or toluene or the mixing of dioxane and tetrahydrofuran or n-butanol and o-dichlorohenzene
Mixing.
Further, above-mentioned a kind of chance water discoloration covalent organic framework material, the organic solvent is dioxy six
The mixing of ring and 1,3,5- trimethylbenzene；By volume, 1,3,5- trimethylbenzenes: dioxane: glacial acetic acid=1:1:0.01~
1:1:0.5。
A kind of application of the above-mentioned chance water discoloration covalent organic framework material in ambient humidity detection field.Method is such as
Under: dry above-mentioned chance water discoloration covalent organic framework material is placed in container, 10min under the conditions of different humidity is placed in
In after, take out meet water discoloration covalent organic framework material tested in ultraviolet-visible spectrum tester.
The beneficial effects of the present invention are: a kind of covalent organic framework material of chance water discoloration, the material prepared by the present invention
Material can show color change under water body or different humidity, and its color change is attributed to its material itself and hydrone shape
At hydrogen bond, energy level is caused to change, using such material property, has in ambient humidity detection field and potentially apply valence
Value.
Detailed description of the invention
Fig. 1 is a kind of PXRD of the covalent organic framework material of chance water discoloration prepared by the present invention.
Fig. 2 is a kind of scanning electron microscope (SEM) photograph of the covalent organic framework material of chance water discoloration prepared by the present invention.
Fig. 3 is a kind of UV-visible spectrum of the covalent organic framework material of chance water discoloration prepared by the present invention.
Fig. 4 is a kind of color camera of the covalent organic framework material of chance water discoloration prepared by the present invention.
Specific embodiment
The following examples will be further described the present invention, but not thereby limiting the invention.Following realities
Experimental method described in example is applied, is conventional method unless otherwise specified；The reagent and material, unless otherwise specified,
It obtains from commercial channels.
A kind of covalent organic framework material for meeting water discoloration of embodiment 1
(1) preparation method
1,3,5- trimethylbenzene of 1mL, 1mL dioxane and 0.5mL glacial acetic acid are dispersed in 0.3mL distilled water, formed
Mixed solution.It is molten that 21.6mg (1mmol) p-phenylenediamine and 10.8mg (1.5mmol) trifonnyl phenol are dispersed in above-mentioned mixing
In liquid, at room temperature after uniform stirring 0.5h, stand, filtering, after obtained solid powder successively uses tetrahydrofuran and acetone washing, in
80 DEG C of vacuum drying 12h, obtain yellow powder, to meet water discoloration covalent organic framework material.
(2) it detects
Fig. 1 is the XRD diffracting spectrum of product and the XRD diffraction pattern of analog product, as seen from Figure 1, analogue spectrums and product
Spectrogram be it is identical, illustrate that prepared material structure is correct, and be pure phase.
Fig. 2 is the scanning electron microscope (SEM) photograph of product, from Figure 2 it can be seen that the material shows column cross-linked state, to generate multistage
Pore structure.
A kind of discoloration for the covalent organic framework material for meeting water discoloration of embodiment 2
Method: it weighs covalent organic framework material prepared by 100mg embodiment 1 and is placed under different humidity and place 10min
Afterwards, the test of solid uv-vis spectra is carried out.
Fig. 3 is the UV-visible spectrum of the covalent organic framework material for meeting water discoloration prepared by embodiment 1, in difference
Humidity under, a degree of change occurs for the ultraviolet-visible spectrum of material, from figure it can be found that under influence of moisture, material
Ultraviolet-ray visible absorbing of the ultraviolet-visible spectrum of material at 500nm-750nm is remarkably reinforced, so as to cause color change, but
Under the damp condition that moisture is 6%, ultraviolet-ray visible absorbing variation is unobvious, and significantly variation is generated under remaining humidity.
Fig. 4 is the color camera of the covalent organic framework material for meeting water discoloration prepared by embodiment 1.From fig. 4, it can be seen that into
Before and after row Humidity Detection, the color of material becomes black (wet sample) from rufous (drying sample).
After test, the covalent organic framework material of recycling is activated at 120 DEG C, material restores itself color.
Claims (7)
- The covalent organic framework material 1. a kind of chance water changes colour, which is characterized in that preparation method includes the following steps: organic solvent It is dispersed in distilled water with glacial acetic acid, forms mixed solution；P-phenylenediamine and trifonnyl phenol are dispersed in be formed by it is mixed It closes in solution, at room temperature after uniform stirring 0.1-0.5h, stands, filtering, obtained solid powder successively uses tetrahydrofuran and acetone It after washing, is dried in vacuo in 80 DEG C, obtains target product and meet water discoloration covalent organic framework material.
- The covalent organic framework material 2. a kind of chance water according to claim 1 changes colour, it is characterised in that: in molar ratio, right Phenylenediamine: trifonnyl phenol=2:3.
- The covalent organic framework material 3. a kind of chance water according to claim 1 changes colour, it is characterised in that: described is organic molten Agent be tetrahydrofuran, 1,3,5- trimethylbenzene, toluene, dioxane, ethyl alcohol, n-butanol and o-dichlorohenzene one kind or two kinds with On mixing.
- The covalent organic framework material 4. a kind of chance water according to claim 3 changes colour, it is characterised in that: described is organic molten Agent is dioxane and 1, the mixing of 3,5- trimethylbenzenes or toluene or the mixing of dioxane and tetrahydrofuran or n-butanol With the mixing of o-dichlorohenzene.
- The covalent organic framework material 5. a kind of chance water according to claim 4 changes colour, it is characterised in that: described is organic molten Agent is dioxane and 1, the mixing of 3,5- trimethylbenzenes；By volume, 1,3,5- trimethylbenzenes: dioxane: glacial acetic acid= 1:1:0.01~1:1:0.5.
- 6. a kind of application for meeting water discoloration covalent organic framework material in ambient humidity detection described in claim 1.
- 7. application according to claim 6, which is characterized in that method is as follows: by dry chance water described in claim 1 Discoloration covalent organic framework material is placed in container, after being placed under the conditions of different humidity in 10min, takes out that meet water discoloration covalent Organic framework material is tested in ultraviolet-visible spectrum tester.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114395549A (en) * | 2022-01-19 | 2022-04-26 | 北京化工大学 | Enzyme in-situ packaging method based on hollow covalent organic framework material |
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| CN114395549A (en) * | 2022-01-19 | 2022-04-26 | 北京化工大学 | Enzyme in-situ packaging method based on hollow covalent organic framework material |
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