CN107486155A - One kind pollution acetonitrile treatment agent and its application process - Google Patents
One kind pollution acetonitrile treatment agent and its application process Download PDFInfo
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- CN107486155A CN107486155A CN201710758477.XA CN201710758477A CN107486155A CN 107486155 A CN107486155 A CN 107486155A CN 201710758477 A CN201710758477 A CN 201710758477A CN 107486155 A CN107486155 A CN 107486155A
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- Prior art keywords
- acetonitrile
- pollution
- treatment agent
- acetonitrile treatment
- yuan
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
Abstract
It is by ten yuan of melon rings and [Cd the invention discloses one kind pollution acetonitrile treatment agent and its application process4Cl16]8‑Mixing, self-assembly porous framework solid powder is made, that is, pollutes acetonitrile treatment agent.Pollution acetonitrile treatment agent is put into organic guest molecule in pollution acetonitrile in absorption effluent, realizes pollution acetonitrile treatment.The present invention has the machine guest molecule that can be adsorbed in pollution acetonitrile, the characteristics of for purifying contaminated acetonitrile, extends the research of ten yuan of melon rings；In addition, the present invention has the characteristics of pollution acetonitrile treatment agent preparation technology is simple, and processing cost is low, and organic guest molecule species of absorption is more, and treatment effeciency is high.
Description
Technical field
The present invention relates to one kind pollution acetonitrile treatment agent and its application process, particularly one kind to be based on ten yuan of melon ring supermolecules
The pollution acetonitrile treatment agent of the porous framework structure solid powder of self assembly and its application process.
Background technology
Melon ring（Cucurbit[n]uril）, also known as Cucurbituril,（Abbreviation CB [n] or Q [n]）, because structure obtains like pumpkin
Name, is the new caged host compound of another class after the macrocyclic compound such as crown ether, cyclodextrin, calixarenes, from structural
From the point of view of in matter, melon ring has the hydrophobic cavity and both ends open and the carbonylic oxygen atom for being covered with polarity of a high degree of symmetry,
The feature of this structure can be selective under solution state inclusion size dimension it is suitable organic and inorganic and biological
The small molecules such as molecule at port again or with hydrophilic complex effect occurs with dipole or ionic compound, with research
The deep progress of work, melon ring are applied to organic synthesis, molecular recognition, nano material, catalysis, separation etc. gradually.Ten yuan
Melon ring relatively low product of the content during as melon cyclization, reported first in the form of Q [5]@Q [10] in Day seminar in 2002
Road, but because content is low, the factor such as hardly possible separation, limit its development and application.And it is applied in the contaminated acetonitrile of removing
The pollution acetonitrile treatment agent of organic guest molecule, which has no, to be had been reported that.
Meanwhile the species of existing pollution acetonitrile treatment agent is a lot, but preparation technology complexity be present, processing cost is high, inhales
The defects of attached organic guest molecule species is few, and treatment effeciency is low.
The content of the invention
It is an object of the present invention to provide one kind pollution acetonitrile treatment agent and its application process.The present invention has and can inhaled
Organic guest molecules in attached contaminated acetonitrile, the characteristics of for purifying contaminated acetonitrile, extend the application of ten yuan of melon rings；This
Outside, the present invention is simple with pollution acetonitrile treatment agent preparation technology, and processing cost is low, and organic guest molecule species of absorption is more,
The characteristics for the treatment of effeciency is high.
Technical scheme：One kind pollution acetonitrile treatment agent, is by ten yuan of melon rings and [Cd4Cl16]8-Mixing, it is heavy to obtain
Starch, dried after sediment is filtered out, pollution acetonitrile treatment agent is made.
Foregoing pollution acetonitrile treatment agent, the molecular formula of the sediment are：C60H222N40O92Cd4Cl18, structural formula is for example attached
Shown in Fig. 1.
Foregoing pollution acetonitrile treatment agent, described ten yuan of melon rings and [Cd4Cl16]8-Mol ratio be 1：4.
Foregoing pollution acetonitrile treatment agent, the drying are using 50-70 DEG C of vacuum drying 1-2 hour.
Foregoing pollution acetonitrile treatment agent, the drying are dried in vacuo 1.5 hours using 60 DEG C.
Foregoing pollution acetonitrile treatment agent, the specific preparation method of the pollution acetonitrile treatment agent are as follows：
A. ten yuan of melon rings are added in 6-12M hydrochloric acid, concussion, makes its dissolving, obtain A product；
B. by CdCl2Add in 6-12M hydrochloric acid, concussion, make its dissolving, obtain B product（That is [Cd4Cl16]8-）；
C. A product are mixed into obtain mixed liquor with B product, to white precipitate is no longer produced, filtered, drying, you can obtain polluting at acetonitrile
Manage agent.
A kind of application process according to foregoing pollution acetonitrile treatment agent, method comprise the following steps：
A. the pollution acetonitrile treatment agent is put into the contaminated acetonitrile containing organic guest molecule, in absorption pollution acetonitrile
Organic guest molecule, the ratio for being contaminated amount of the acetonitrile amount with polluting acetonitrile treatment agent is 1L：50-100g；
B. 5-10 minutes are stood, filtering precipitate, obtains pure acetonitrile；
The application process of foregoing pollution acetonitrile treatment agent, organic guest molecule include rhodamine B, pyrene methylamine, bathocuproine,
Carbendazim, Ofloxacin, Norfloxacin, Hydroxycoumarin, quinoline, thioflavine T, methyl blue, acridine orange, pyronin, ferrosin,
Naphthols, anthracene, cumarin aldehyde, pyridine ethene, pyrene and pyrene aldehyde.
Beneficial effects of the present invention：
1st, the present invention is by using ten yuan of melon rings and [Cd4Cl16]8-Self-assembly porous framework solid powder is mixed to prepare, that is, is polluted
Acetonitrile treatment agent.The pollution acetonitrile treatment agent can adsorb organic guest molecule in pollution acetonitrile, reach purifying contaminated acetonitrile
Effect, extend the research of ten yuan of melon rings.
2nd, pollution acetonitrile treatment agent preparation technology of the invention is simple, and when acetonitrile is polluted in processing, processing cost is low；And it is pair
A kind of extension of acetonitrile treatment has been polluted at present, and the application value to exploring melon ring is great, before there is extensive development
Scape.
3rd, the adsorbable organic guest molecule species of pollution acetonitrile treatment agent of the invention is more, and can disposably adsorb a variety of has
Machine guest molecule, greatly reduces processing cost, improves treatment effeciency.
Brief description of the drawings
Fig. 1 is the structure chart of the self-assembly porous framework of the present invention；
Fig. 2 is the structure chart and crystal detail view of the self-assembly porous framework of the present invention（C-axis direction）；
Fig. 3 is the topology diagram schematic diagram of the self-assembly porous framework of the present invention；
Fig. 4 is the crystal structure figure of a parallelepiped cage unit of the self-assembly porous framework of the present invention；
Fig. 5 is ten yuan of melon rings and four [Cd4Cl16]8-Binding mode detail view；
Fig. 6 is four ten yuan of melon rings and [a Cd4Cl16]8-Binding mode detail view.
To further illustrate the effect of the present invention, following experiment has been done：
Experimental example 1, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing Luo Dan
In bright B pollution acetonitrile sample, rock, red solution lighter can be observed, white solid powder is changed into pink, explanation
Porous framework has adsorbed rhodamine B.
Experimental example 2, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing pyrene
In the pollution acetonitrile sample of methylamine, rock, solution fluorescence, which can be observed, under 365nm ultraviolet lights dies down, and non-blooming white is solid
Body powder sends green fluorescence, illustrates that porous framework has adsorbed pyrene methylamine.
Experimental example 3, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing bath
In the pollution acetonitrile sample of copper spirit, rock, yellow solution lighter can be observed, white solid powder is changed into yellow, explanation
Porous framework has adsorbed bathocuproine.
Experimental example 4, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing more
Bacterium spirit pollution acetonitrile sample in, rock, can be observed under 365nm ultraviolet lights non-blooming white solid powder send it is orange glimmering
Light, illustrate that porous framework has adsorbed carbendazim.
Experimental example 5, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing aerobic
In the pollution acetonitrile sample of Flucloxacillin, rock, yellow solution lighter can be observed, white solid powder is changed into yellow, says
Bright porous framework has adsorbed Ofloxacin.
Experimental example 6, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing promise
In the pollution acetonitrile sample of Flucloxacillin, rock, non-blooming white solid powder can be observed under 365nm ultraviolet lights and send green grass or young crops
Color fluorescence, illustrate that porous framework has adsorbed Norfloxacin.
Experimental example 7, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing first
In the blue pollution acetonitrile sample of base, rock, blue solution lighter can be observed, white solid powder is changed into black-and-blue, said
Bright porous framework has adsorbed methyl blue.
Experimental example 8, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing pyrene
Pollution acetonitrile sample in, rock, yellow solution lighter can be observed, white solid powder is changed into yellow, illustrates porous
Framework has adsorbed pyrene.
Experimental example 9, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework is poured into containing pyrene
In the pollution acetonitrile sample of aldehyde, rock, yellow solution lighter can be observed, white solid powder is changed into yellow, illustrates more
Hole framework has adsorbed pyrene aldehyde.
Experimental example 10, by ten yuan of melon rings of 15.0mg and [Cd4Cl16]8-The solid powder of self-assembly porous framework pour into containing
In the pollution acetonitrile sample of thioflavine T, rock, yellow solution lighter can be observed, white solid powder is changed into yellow, says
Bright porous framework has adsorbed thioflavine T.
Embodiment
With reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiments of the invention
Embodiment 1, a kind of pollution acetonitrile treatment agent, its preparation method are as follows：
A. ten yuan of melon rings are added in 8M hydrochloric acid, concussion, makes its dissolving, obtain A product；
B. by CdCl2Add in 8M hydrochloric acid, concussion, make its dissolving, obtain B product（That is [Cd4Cl16]8-）；
C. A product are mixed into obtain mixed liquor with B product, adjusts ten yuan of melon rings and [Cd in B product in A product4Cl16]8-Proportioning be 1:4,
To ten yuan of melon rings to white precipitate is no longer produced, white precipitate is filtered out into rear 60 DEG C of vacuum dryings 1.5 hours, you can polluted
Acetonitrile sewage-treating agent；
The application process of above-mentioned pollution acetonitrile treatment agent：
A. the pollution acetonitrile treatment agent solid powder is put into the contaminated acetonitrile containing organic guest molecule, absorption pollution
Organic guest molecule in acetonitrile, the ratio for polluting acetonitrile amount and the amount of inorganic agent is 1L：50g；
B. 10 minutes are stood, filters the sediment in acetonitrile, obtain pure acetonitrile.
Embodiment 2, a kind of pollution acetonitrile treatment agent, its preparation method are as follows：
A. ten yuan of melon rings are added in 6M hydrochloric acid, concussion, makes its dissolving, obtain A product；
B. by CdCl2Add in 8M hydrochloric acid, concussion, make its dissolving, obtain B product（That is [Cd4Cl16]8-）；
C. A product are mixed into obtain mixed liquor with B product, adjusts ten yuan of melon rings and [Cd in B product in A product4Cl16]8-Proportioning be 1:4,
To ten yuan of melon rings to white precipitate is no longer produced, white precipitate is filtered out into rear 50 DEG C of vacuum dryings 2 hours, you can obtain polluting second
Nitrile sewage-treating agent；
The application process of above-mentioned pollution acetonitrile treatment agent：
A. the pollution acetonitrile treatment agent solid powder is put into the contaminated acetonitrile containing organic guest molecule, absorption pollution
Organic guest molecule in acetonitrile, the ratio for polluting acetonitrile amount and the amount of inorganic agent is 1L：80g；
B. 7 minutes are stood, filters the sediment in acetonitrile, obtain pure acetonitrile.
Embodiment 3, a kind of pollution acetonitrile treatment agent, its preparation method are as follows：
A. ten yuan of melon rings are added in 12M hydrochloric acid, concussion, makes its dissolving, obtain A product；
B. by CdCl2Add in 8M hydrochloric acid, concussion, make its dissolving, obtain B product（That is [Cd4Cl16]8-）；
C. A product are mixed into obtain mixed liquor with B product, adjusts ten yuan of melon rings and [Cd in B product in A product4Cl16]8-Proportioning be 1:4,
To ten yuan of melon rings to white precipitate is no longer produced, white precipitate is filtered out into rear 70 DEG C of vacuum dryings 1 hour, you can obtain polluting second
Nitrile sewage-treating agent；
The application process of above-mentioned pollution acetonitrile treatment agent：
A. the pollution acetonitrile treatment agent solid powder is put into the contaminated acetonitrile containing organic guest molecule, absorption pollution
Organic guest molecule in acetonitrile, the ratio for polluting acetonitrile amount and the amount of inorganic agent is 1L：100g；
B. 5 minutes are stood, filters the sediment in acetonitrile, obtain pure acetonitrile.
Organic guest molecule described in above-described embodiment is rhodamine B, pyrene methylamine, bathocuproine, carbendazim, oxygen fluorine are husky
Star, Norfloxacin, Hydroxycoumarin, quinoline, thioflavine T, methyl blue, acridine orange, pyronin, ferrosin, naphthols, anthracene, tonka-bean
Plain aldehyde, pyridine ethene, pyrene and pyrene aldehyde.
Claims (8)
1. one kind pollution acetonitrile treatment agent, it is characterised in that：It is by ten yuan of melon rings and [Cd4Cl16]8-Mixing, obtains sediment, will be heavy
Starch is dried after filtering out, and pollution acetonitrile treatment agent is made.
2. pollution acetonitrile treatment agent according to claim 1, it is characterised in that：The molecular formula of the sediment is：
C60H222N40O92Cd4Cl18, structural formula is：
3. pollution acetonitrile treatment agent according to claim 1, it is characterised in that：Described ten yuan of melon rings and [Cd4Cl16]8-'s
Mol ratio is 1：4.
4. pollution acetonitrile treatment agent according to claim 1, it is characterised in that：The drying is to use 50-70 DEG C of vacuum
Dry 1-2 hours.
5. pollution acetonitrile treatment agent according to claim 4, it is characterised in that：The drying is using 60 DEG C of vacuum drying
1.5 hour.
6. the pollution acetonitrile treatment agent according to claim any one of 1-5, it is characterised in that：The pollution acetonitrile treatment agent
Preparation method it is as follows：
A. ten yuan of melon rings are added in 6-12M hydrochloric acid, concussion, makes its dissolving, obtain A product；
B. by CdCl2Add in 6-12M hydrochloric acid, concussion, make its dissolving, obtain B product；
C. A product are mixed into obtain mixed liquor with B product, to white precipitate is no longer produced, filtered, drying, you can obtain polluting at acetonitrile
Manage agent.
A kind of 7. application process of pollution acetonitrile treatment agent according to claim any one of 1-5, it is characterised in that：Method
Comprise the following steps：
A. the pollution acetonitrile treatment agent is put into the contaminated acetonitrile containing organic guest molecule, in absorption pollution acetonitrile
Organic guest molecule, the ratio for being contaminated amount of the acetonitrile amount with polluting acetonitrile treatment agent is 1L：50-100g；
B. 5-10 minutes are stood, filtering precipitate, obtains pure acetonitrile.
8. the application process of pollution acetonitrile treatment agent according to claim 7, it is characterised in that：Organic guest molecule
Including rhodamine B, pyrene methylamine, bathocuproine, carbendazim, Ofloxacin, Norfloxacin, Hydroxycoumarin, quinoline, thioflavine T, first
Base indigo plant, acridine orange, pyronin, ferrosin, naphthols, anthracene, cumarin aldehyde, pyridine ethene, pyrene and pyrene aldehyde.
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Cited By (2)
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| CN109187476A (en) * | 2018-09-18 | 2019-01-11 | 贵州大学 | A kind of application of the supermolecule frame material based on ten yuan of melon rings in pyridine detection |
| CN110484242A (en) * | 2019-08-28 | 2019-11-22 | 贵州大学 | The fluorescence probe of ferric ion and its preparation and detection method in a kind of detection water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187476A (en) * | 2018-09-18 | 2019-01-11 | 贵州大学 | A kind of application of the supermolecule frame material based on ten yuan of melon rings in pyridine detection |
| CN109187476B (en) * | 2018-09-18 | 2021-02-02 | 贵州大学 | Application of ten-element cucurbituril-based super-molecular framework material in pyridine detection |
| CN110484242A (en) * | 2019-08-28 | 2019-11-22 | 贵州大学 | The fluorescence probe of ferric ion and its preparation and detection method in a kind of detection water |
| CN110484242B (en) * | 2019-08-28 | 2022-05-17 | 贵州大学 | Fluorescent probe for detecting ferric ions in water and preparation and detection methods thereof |
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Application publication date: 20171219 |