CN108997385A - A kind of isomers adsorbent for nitro-chlorobenzene separation - Google Patents
A kind of isomers adsorbent for nitro-chlorobenzene separation Download PDFInfo
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- CN108997385A CN108997385A CN201710422444.8A CN201710422444A CN108997385A CN 108997385 A CN108997385 A CN 108997385A CN 201710422444 A CN201710422444 A CN 201710422444A CN 108997385 A CN108997385 A CN 108997385A
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- adsorbent
- isomers
- chlorobenzene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic System
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic System without C-Metal linkages
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
- C07C63/14—Monocyclic dicarboxylic acids
- C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
- C07C63/26—1,4 - Benzenedicarboxylic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
- C07C63/307—Monocyclic tricarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic System
- C07F1/005—Compounds containing elements of Groups 1 or 11 of the Periodic System without C-Metal linkages
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic System
- C07F11/005—Compounds containing elements of Groups 6 or 16 of the Periodic System compounds without a metal-carbon linkage
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic System
- C07F15/02—Iron compounds
- C07F15/025—Iron compounds without a metal-carbon linkage
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic System
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of metal-organic framework materials, and the separation of nitro-chlorobenzene is realized using suction type.It is bonded together to form by metal ion and organoligand coordination.At least one above-mentioned metal ion and at least one above-mentioned organoligand coordination bond together to form metal-organic framework materials.By controlling the aperture of adsorbent material in 0.8-1.5nm, paranitrochlorobenzene isomer progress adsorbing separation.Adsorbing separation is carried out to isomer using the architectural difference of molecule.Space structure by changing absorbent interior can be generally applicable to the separation of isomers in organic matter, and easily operated, speed is fast, and labor intensity is low, highly-safe.
Description
Technical field
The invention belongs to field of fine chemical, are related to a kind of new adsorbent for nitro-chlorobenzene separation.
Background technique
O-nitrochlorobenzene is one of the intermediate for manufacturing pesticide, o-phenylenediamine can be reduced to through ammonification, then waited through cyclisation
Journey and carbendazim is made；It is also to produce one of intermediate of dyestuff, can through processes such as reduction, methyl oxidation, condensation, couplings
A variety of dyestuffs are made；It can be made into fragrance through processes such as methylation, reduction, hydrolysis, hydroformylations；Through processes such as reduction, vulcanization, closed loops,
Rubber accelerator can be made.
Paranitrochlorobenzene can be derived as paranitroanilinum, p-nitrophenol, para-aminophenol, para aminophenyl ethyl ether, right
Aminoanisole, 4, the Organic chemical products such as 4 '-benzidine ethers, it is widely used in dyestuff intermediate, pesticide, medicine, rubber
The chemical industries such as glue auxiliary agent.
Currently, the country is all made of traditional mixed acid process technique production nitro-chlorobenzene, it is primarily due to law technology maturity height,
Long history.The production process of certain company's nitro-chlorobenzene device mainly includes raw material reception, nitration mixture preparation, Chlorobenzene Nitration, acidity
Nitro chlorobenzene neutralization, washing, extraction, drying, wastewater treatment, rectifying separate and to nitre Crystallization Separation etc..
The domestic method for all using Crystallization Separation substantially of the separation of nitro-chlorobenzene product.Since the said firm is using multiple groups
Small-sized fin type crystallizer, the physical property of nitro-chlorobenzene lead to crystallizer seriously corroded, influence the stabilization of production.
Summary of the invention
The technical problem to be solved by the present invention is to cumbersome, the crystallizers for nitro-chlorobenzene production crystallization process intermittently operated
The problems such as leak is corroded.The present invention proposes a kind of application of the adsorbing separation of isomers adsorbent and its paranitrochlorobenzene, passes through
The parameters such as pore diameter range, the cellular structure of adsorbent are controlled to realize the separation of nitro-chlorobenzene.
Technical solution of the present invention: the isomers adsorbent for nitro-chlorobenzene adsorbing separation, it is characterised in that described
Isomers adsorbent is a kind of metal-organic framework materials, including metal salt and organic ligand；The metal salt is zinc salt, aluminium
One or more of salt, molysite, mantoquita, magnesium salts, chromic salts；Organic ligand be selected from aromatic rings, polycarboxylic acid aromatic ligand, pyridine,
One or more of indoles, quinoline, imidazoles；At least one above-mentioned metal ion is matched at least one above-mentioned organic ligand
Position bonds together to form metal-organic framework materials.
Generally, the metal salt are as follows: the mixture of copper chloride, aluminum nitrate and ferric sulfate.
The organic ligand are as follows: one of pyridine and polycarboxylic acid aromatic ligand.
The polycarboxylic acid aromatic ligand is terephthalic acid (TPA) or trimesic acid.
The present invention is tubular type cellular structure by the inside for controlling adsorbent in metal-organic framework materials preparation process,
Pore diameter range is in 0.8-1.5nm, it can be achieved that nitro-chlorobenzene is the same as the adsorbing separation for dividing enantiomers.
Adsorbing separation is carried out to isomer using the architectural difference of molecule.By the space knot for changing absorbent interior
Structure can be generally applicable to the separation of isomers in organic matter, and easily operated, speed is fast, and labor intensity is low, highly-safe.
Beneficial effects of the present invention: the space knot in the preparation process of adsorbent material through control adsorbent is developed
The parameters such as structure, aperture carry out adsorbing separation to isomer.It is separated using isomers adsorbent paranitrochlorobenzene, it will
Adsorbent is put into nitro-chlorobenzene mixture, stands the regular hour, and o-, m- position nitro-chlorobenzene is adsorbed, improves to nitro
The content of chlorobenzene.To improve the separating effect of paranitrochlorobenzene.It is with a wide range of applications.
Specific embodiment
Below by embodiment, the present invention is further elaborated, but is not limited only to the present embodiment.
Embodiment in the present invention is in a static condition, using isomers adsorbent adsorbing separation nitro-chlorobenzene, will to inhale
Attached dose is put into nitro-chlorobenzene mixture, stands the regular hour, and o-, m- position nitro-chlorobenzene is adsorbed, and guarantees nitro-chlorobenzene
Separating effect.
Embodiment 1
Ready nitro-chlorobenzene is put into beaker, a certain amount of isomers adsorbent is added, is adsorbed 5 hours.It takes out and inhales afterwards
Attached dose, analyze the content of each component of sample in beaker.Analysis is the results show that the concentration of paranitrochlorobenzene can be before absorption
74.3% is increased to 81.2%, and o-nitrochlorobenzene concentration is reduced to 12.6% from 18.5% before absorption, and m-chloronitrobenzene concentration is from suction
5.0% before attached drops to 3.9%.
Embodiment 2
Ready nitro-chlorobenzene is put into beaker, a certain amount of isomers adsorbent is added, is adsorbed 10 hours.It takes out and inhales afterwards
Attached dose, analyze the content of each component of sample in beaker.Analysis is the results show that the concentration of paranitrochlorobenzene can be before absorption
74.3% is increased to 85.2%, and o-nitrochlorobenzene concentration is reduced to 11.2% from 18.5% before absorption, and m-chloronitrobenzene concentration is from suction
5.0% before attached drops to 3.4%.
Embodiment 3
Ready nitro-chlorobenzene is put into beaker, a certain amount of isomers adsorbent is added, 100ml nitro-chlorobenzene, which is added, to be inhaled
Attached dose of 5g is adsorbed 5 hours.After take out adsorbent, analyze the content of each component of sample in beaker.Analysis is the results show that right
The concentration of nitro-chlorobenzene can be increased to 79.0% from 74.3% before absorption, and o-nitrochlorobenzene concentration is reduced from 18.5% before absorption
To 13.1%, m-chloronitrobenzene concentration drops to 4.1% from 5.0% before absorption.
Embodiment 4
Ready nitro-chlorobenzene is put into beaker, a certain amount of isomers adsorbent is added, 100ml nitro-chlorobenzene, which is added, to be inhaled
Attached dose of 5g is adsorbed 10 hours.After take out adsorbent, analyze the content of each component of sample in beaker.Analysis is the results show that right
The concentration of nitro-chlorobenzene can be increased to 82.2% from 74.3% before absorption, and o-nitrochlorobenzene concentration is reduced from 18.5% before absorption
To 11.9%, m-chloronitrobenzene concentration drops to 3.7% from 5.0% before absorption.
Claims (7)
1. a kind of isomers adsorbent for nitro-chlorobenzene adsorbing separation, it is characterised in that the isomers adsorbent is one
Kind metal-organic framework materials, including metal salt and organic ligand；The metal salt is zinc salt, aluminium salt, molysite, mantoquita, magnesium
One or more of salt, chromic salts；Organic ligand is in aromatic rings, polycarboxylic acid aromatic ligand, pyridine, indoles, quinoline, imidazoles
One or more；At least one above-mentioned metal ion, which bonds together to form metal at least one above-mentioned organoligand coordination, to be had
Machine framework material.
2. isomers adsorbent as described in claim 1, which is characterized in that the metal salt are as follows: copper chloride, aluminum nitrate and sulphur
The mixture of sour iron.
3. isomers adsorbent as described in claim 1, which is characterized in that the organic ligand are as follows: pyridine and polycarboxylic acid virtue
One of fragrant ligand.
4. isomers adsorbent as claimed in claim 1 or 3, which is characterized in that the polycarboxylic acid aromatic ligand is to benzene two
Formic acid or trimesic acid.
5. isomers adsorbent as described in claim 1, it is characterised in that absorbent interior microstructure is tubular type cellular structure.
6. isomers adsorbent as claimed in claim 5, it is characterised in that the aperture in absorbent interior tubular type duct are as follows: 0.8-
1.5nm。
7. isomers adsorbent as described in claim 1, it is characterised in that by changing adsorbent space structure and aperture parameters
Adsorbing separation for other isomers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710422444.8A CN108997385A (en) | 2017-06-07 | 2017-06-07 | A kind of isomers adsorbent for nitro-chlorobenzene separation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710422444.8A CN108997385A (en) | 2017-06-07 | 2017-06-07 | A kind of isomers adsorbent for nitro-chlorobenzene separation |
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| Publication Number | Publication Date |
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| CN108997385A true CN108997385A (en) | 2018-12-14 |
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| CN201710422444.8A Pending CN108997385A (en) | 2017-06-07 | 2017-06-07 | A kind of isomers adsorbent for nitro-chlorobenzene separation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205475A (en) * | 2020-02-24 | 2020-05-29 | 陕西师范大学 | Porous COFs block and application thereof in isomer separation |
| CN113354828A (en) * | 2021-05-08 | 2021-09-07 | 沈阳大学 | Preparation and application of novel stable metal organic framework material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631805A (en) * | 2004-11-12 | 2005-06-29 | 南京大学 | Method for separating and recovering nitro chlorobenzene from wastewater by using silanization modified zeolite |
-
2017
- 2017-06-07 CN CN201710422444.8A patent/CN108997385A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1631805A (en) * | 2004-11-12 | 2005-06-29 | 南京大学 | Method for separating and recovering nitro chlorobenzene from wastewater by using silanization modified zeolite |
Non-Patent Citations (2)
| Title |
|---|
| ZHI-LI FANG等: "Tubular metal–organic framework-based capillary gas chromatography column for separation of alkanes and aromatic positional isomers", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 李晓新 等: "金属-有机骨架材料在色谱分离中的应用", 《化学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205475A (en) * | 2020-02-24 | 2020-05-29 | 陕西师范大学 | Porous COFs block and application thereof in isomer separation |
| CN113354828A (en) * | 2021-05-08 | 2021-09-07 | 沈阳大学 | Preparation and application of novel stable metal organic framework material |
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Application publication date: 20181214 |