CN107794767A - A kind of method that metal organic framework compound parcel fiber is prepared using spray-on process - Google Patents
A kind of method that metal organic framework compound parcel fiber is prepared using spray-on process Download PDFInfo
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- CN107794767A CN107794767A CN201710994152.1A CN201710994152A CN107794767A CN 107794767 A CN107794767 A CN 107794767A CN 201710994152 A CN201710994152 A CN 201710994152A CN 107794767 A CN107794767 A CN 107794767A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/687—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing atoms other than phosphorus, silicon, sulfur, nitrogen, oxygen or carbon in the main chain
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B1/00—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating
- D06B1/02—Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by spraying or projecting
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/02—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fibres, slivers or rovings
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The present invention discloses a kind of method that metal organic framework compound parcel fiber is prepared using spray-on process, spray solution is used as using metal cation solution, solution of the organic ligand solution as immersion fiber, metal cation solution to be atomized is entered in sprayer unit by auto injection infusion, it is set to be dispersed into liquid little particle by ultrasonic wave in the showerhead, and sprayed with mist from shower nozzle, solution after atomization falls on the surface for the fiber for soaking organic ligand solution by the even action of gravity, reacted after two kinds of material contacts in fiber surface, construct metal organic framework compound and be wrapped in fiber surface.It is an advantage of the invention that：It is simple to operate, be easy to control and industrialized production；Normal temperature and pressure, experiment condition are gentle, environmental protection and energy saving；Reaction speed is fast, short preparation period；Collection of products method is easy, convenient follow-up use.
Description
Technical field
The present invention relates to chemical field, and in particular to one kind prepares metal organic framework compound parcel fibre using spray-on process
The method of dimension.
Background technology
Metal organic framework compound is a kind of novel nano-pore crystalline material, and its structure is by metal ion or metal
Cluster is formed in the form of strong coordinate bond with reference to diversified organic ligand.Metal organic framework compound has uniform pore diameter, surpassed
The excellent physicochemical properties such as high-specific surface area and stronger absorption affinity.The fiber of metal organic framework compound parcel
It is a kind of compound material, incorporates the advantageous property of metal organic framework compound and fiber, enhances the physics and chemistry of fiber
Matter, extend the application field of fiber.The method of common preparation metal organic framework compound parcel fiber has：Presoma is molten
Direct sedimentation in liquid；Free diffusing method.But these method complex operations, synthesis cycle length, preparation process energy consumption are unsuitable for greatly
Industrial production.
The content of the invention
In order to solve the above technical problems, the present invention prepares metal organic framework using ultrasonic spray technology in fiber surface
Compound, the synthesis of metal organic framework nanometer sheet is the method achieve with being wrapped in the synchronous progress of fiber surface, there is operation
Simply, synthesis cycle is short and is easy to the advantage mass produced in the industry.
Concrete technical scheme is as follows：
A kind of method that metal organic framework compound parcel fiber is prepared using spray-on process, is comprised the following steps：
(1) two kinds of reaction solutions of a kind of configuration in following situations are selected：
Situation one：
The first solution is metal cation solution, and its solute is copper acetate, concentration 0.015mol/L-0.025mol/
L, solvent are that volume ratio is 1:2 DMF and acetonitrile mixture,
Second is organic ligand solution；Its solute is terephthalic acid (TPA), concentration 0.005mol/L-0.015mol/L,
Solvent is that volume ratio is 2:1 N,N-dimethylformamide and acetonitrile mixture；
Situation two：
The first solution is metal cation solution, and its solute is zinc acetate, concentration 0.0055mol/L-
0.0065mol/L, solvent are that volume ratio is 1:2 DMF and acetonitrile mixture,
Second is organic ligand solution；Its solute is terephthalic acid (TPA), concentration 0.005mol/L-0.015mol/L,
Solvent is that volume ratio is 2:1 N,N-dimethylformamide and acetonitrile mixture；
Situation three：
The first solution is metal cation solution, and its solute is cobalt acetate, and concentration 0.15mol/L, solvent is N, N-
Dimethylformamide,
Second is organic ligand solution；Its solute is terephthalic acid (TPA), and concentration 0.15mol/L, solvent is N, N- bis-
NMF；
(2) soak：Basilar fibers is immersed in organic ligand solution, taken out to after being impregnated with；
(3) spray：It is set to be separated into liquid by ultrasonic wave using metal cation solution as in spray solution injection nozzle
Little particle is dripped, is sprayed with mist from shower nozzle；Solution after atomization uniformly fall lower section immersion organic ligand solution
On basilar fibers, two kinds of solution start to construct metal organic framework compound after fiber surface contact, and then obtain metal and have
The fiber of machine framework compound parcel；The fiber of obtained metal organic framework compound parcel by being immersed in N, N- bis- repeatedly
Purifying is washed in NMF.
Further, step (3) is sprayed：The spray solution is by auto injection pump injection nozzle, the ginseng of auto injection pump
Number is arranged to flow 30 μ L/min, spray time 400s.
Further, the basilar fibers is one kind in carbon felt fiber, cotton fiber or organic fiber.
The present invention successfully synthesizes the fiber of metal organic framework compound parcel by spray-on process.At present, metallic framework
The fiber of compound parcel has good application in gas sensing, absorption and catalysis etc..Compared with traditional packaging method
It is compared with the advantages of, the method：(1) it is easy to operate, it is easily controllable, beneficial to industrial production；(2) reacted under normal temperature and pressure, test bar
Part is gentle, energy-conserving and environment-protective；(3) reaction is fast, and the cycle is short；(5) collection of products is convenient, is used beneficial to follow-up.
Brief description of the drawings
Fig. 1 is the solute using Salicylaldoxime as metal cation solution, when concentration is 0.02mol/L, passes through spraying
The SEM photograph of metal organic framework compound parcel carbon felt fiber prepared by method；
Fig. 2 is the solute using Salicylaldoxime as metal cation solution, when concentration is 0.02mol/L, passes through spraying
The situ X-Ray Diffraction spectrogram of metal organic framework compound parcel carbon felt fiber prepared by method；
Fig. 3 is the solute using Salicylaldoxime as metal cation solution, when concentration is 0.02mol/L, passes through spraying
The SEM pictures of metal organic framework compound parcel cotton fiber prepared by method；
Fig. 4 is the solute using Salicylaldoxime as metal cation solution, when concentration is 0.02mol/L, passes through spraying
The SEM pictures of metal organic framework compound parcel nylon measuring fiber prepared by method.Fig. 4 (1) is multiplication factor when being 12000 times
A wide range of figure, Fig. 4 (2) is local parcel figure of multiplication factor when being 80000 times.
Fig. 5 is the solute using acetic anhydride zinc as metal cation solution, when concentration is 0.006mol/L, passes through spraying
The SEM pictures of metal organic framework compound parcel carbon felt fiber prepared by method；
Fig. 6 is the solute using four acetate hydrate cobalts as metal cation solution, when concentration is 0.15mol/L, passes through spray
The SEM pictures of metal organic framework compound parcel carbon felt fiber prepared by mist method.
Embodiment
Embodiment 1
(1) two kinds of reaction solutions are prepared：The first is acetic acid copper solution, and concentration 0.015mol/L, solute matter is anhydrous
Copper acetate, solvent are 1 that volume ratio is:2N, dinethylformamide and acetonitrile mixed solvent；Second is that terephthalic acid (TPA) is molten
Liquid, concentration 0.005mol/L, solute are terephthalic acid (TPA)s, and solvent is that volume ratio is 2:1 N,N-dimethylformamide and second
Nitrile mixed solvent.
(2) immersion process：2 × 2cm carbon felt fiber is immersed in terephthalic acid solution, is taken out completely after moistening standby
With；
(3) spray process：Spray is injected by the syringe of auto injection pump using acetic anhydride copper solution as spray solution
In the shower nozzle of mist device, it is dispersed into liquid little particle by ultrasonic wave in the showerhead, sprayed with mist from shower nozzle；Mist
Solution after change falls in the carbon felt for soaking terephthalic acid (TPA) by the even action of self gravitation, and two kinds of materials are fine in carbon felt
Start to construct copper-terephthalic acid metal organic framework compounds after the contact of dimension table face；The parameter setting of auto injection pump：
Flow：30μL/min
Distribute number:10 times
Distribute the time：100s
Distribute liquid measure:50μL
Interval time:0.1min
Syringe selects：4.25mm
(4) purifying of the fiber of metal organic framework compound parcel：The carbon felt of obtained copper-terephthalic acid (TPA) parcel is fine
Dimension washs purifying by being immersed in repeatedly in N,N-dimethylformamide.
Embodiment 2
Acetic acid copper concentration in embodiment 1 is changed to 0.025mol/L, corresponding P-phthalic acid at concentration is changed to
0.015mol/L, other processes are same as Example 1.
Embodiment 3
Acetic acid copper concentration in embodiment 1 is changed to 0.02mol/L, corresponding P-phthalic acid at concentration is changed to 0.01mol/
L, other processes are same as Example 1.
Embodiment 4
The fiber of immersion is changed to cotton, other processes are same as Example 1.
Embodiment -5
The fiber of immersion is changed to cotton, other processes are same as Example 2.
Embodiment 6
The fiber of immersion is changed to cotton, other processes are same as Example 3.
Embodiment 7
The fiber of immersion is changed to nylon cloth, other processes are same as Example 1.
Embodiment 8
The fiber of immersion is changed to nylon cloth, other processes are same as Example 2.
Embodiment 9
The fiber of immersion is changed to nylon cloth, other processes are same as Example 3.
Embodiment 10
(1) two kinds of reaction solutions are prepared：The first is zinc acetate solution, and concentration 0.0055mol/L, solute is anhydrous vinegar
Sour zinc, solvent are 1 that volume ratio is:2N, dinethylformamide and acetonitrile mixed solvent；Second is that terephthalic acid (TPA) is molten
Liquid, concentration 0.05mol/L, solute are terephthalic acid (TPA)s, and solvent is that volume ratio is 2:1 N,N-dimethylformamide and acetonitrile
Mixed solvent；
(2) immersion process：2 × 2cm carbon felt fiber is immersed in terephthalic acid solution, is taken out completely after moistening standby
With；
(3) spray process：Spray is injected by the syringe of auto injection pump using acetic anhydride zinc solution as spray solution
In the shower nozzle of mist device, it is dispersed into liquid little particle by ultrasonic wave in the showerhead, sprayed with mist from shower nozzle；Mist
Solution after change falls in the carbon felt for soaking terephthalic acid (TPA) by the even action of self gravitation, and two kinds of materials are fine in carbon felt
Start to construct zinc-terephthalic acid metal organic framework compounds after the contact of dimension table face；The parameter setting of auto injection pump：
Flow：30μL/min
Distribute number:10 times
Distribute the time：100s
Distribute liquid measure:50μL
Interval time:0.1min
Syringe selects：4.25mm
(4) purifying of the fiber of metal organic framework compound parcel：The carbon felt of obtained zinc-terephthalic acid (TPA) parcel is fine
Dimension washs purifying by being immersed in repeatedly in N,N-dimethylformamide.
Embodiment 11
Acetic acid zinc concentration in embodiment 10 is changed to 0.0065mol/L, the concentration of corresponding terephthalic acid (TPA) is changed to
0.015mol/L, other processes are same as in Example 10.
Embodiment 12
Acetic acid zinc concentration in embodiment 10 is changed to 0.006mol/L, the concentration of corresponding terephthalic acid (TPA) is changed to
0.01mol/L, other processes are same as in Example 10.
Embodiment 13
(1) two kinds of reaction solutions are prepared：The first is acetic acid cobalt liquor, and concentration 0.15mol/L, solute is four hydration second
Sour cobalt, solvent are DMFs；Second is terephthalic acid solution, and concentration 0.15mol/L, solute is to benzene
Dioctyl phthalate, solvent are DMFs.
(2) immersion process：2 × 2cm carbon felt fiber is immersed in terephthalic acid solution, is taken out completely after moistening standby
With；
(3) spray process：Filled using acetic acid cobalt liquor as spray solution by the syringe spray injection of auto injection pump
In the shower nozzle put, it is dispersed into liquid little particle by ultrasonic wave in the showerhead, sprayed with mist from shower nozzle；After atomization
Solution fall by the even action of self gravitation in the carbon felt for soaking terephthalic acid (TPA), two kinds of materials are in carbon felt fiber table
Start to construct copper-terephthalic acid metal organic framework compounds after the contact of face；The parameter setting of auto injection pump：
Flow：30μL/min
Distribute number:10 times
Distribute the time：100s
Distribute liquid measure:50μL
Interval time:0.1min
Syringe selects：4.25mm
(4) purifying of the fiber of metal organic framework compound parcel：The carbon felt of obtained zinc-terephthalic acid (TPA) parcel is fine
Dimension washs purifying by being immersed in repeatedly in N,N-dimethylformamide.
In conjunction with accompanying drawing, the present invention will be described, and Fig. 1 is that concentration is using Salicylaldoxime as metal cation solution
During 0.02mol/L, the SEM photograph of the metal organic framework compound wrap carbon fiber prepared by spray-on process, as illustrated, spray
Metal organic framework compound wrap carbon fiber prepared by mist method is uniform.
Fig. 2 is using Salicylaldoxime as metal cation solution, when concentration is 0.02mol/L, is prepared by spray-on process
Metal organic framework compound wrap carbon fiber situ X-Ray Diffraction spectrogram.
Fig. 3 is using Salicylaldoxime as metal cation solution, when concentration is 0.02mol/L, is prepared by spray-on process
Metal organic framework compound parcel cotton fiber SEM photograph, as illustrated, spray-on process prepare metal organic framework chemical combination
Thing parcel cotton fiber is uniform.
Fig. 4 is using Salicylaldoxime as metal cation solution, when concentration is 0.02mol/L, is prepared by spray-on process
Metal organic framework compound parcel nylon fiber SEM photograph, as illustrated, spray-on process prepare metal organic framework
Compound parcel nylon fiber is uniform.
Fig. 5 is using zinc acetate as metal cation solution, when concentration is 0.006mol/L, passes through the gold of spray-on process preparation
Belong to the SEM photograph of organic framework compounds wrap carbon fiber, as illustrated, metal organic framework compound bag prepared by spray-on process
It is uniform to wrap up in carbon fiber.
Fig. 6 is using cobalt acetate as metal cation solution, when concentration is 0.15mol/L, passes through the gold of spray-on process preparation
Belong to the SEM photograph of organic framework compounds wrap carbon fiber, as illustrated, metal organic framework compound bag prepared by spray-on process
It is uniform to wrap up in carbon fiber.
Claims (3)
- A kind of 1. method that metal organic framework compound parcel fiber is prepared using spray-on process, it is characterised in that including as follows Step：(1) two kinds of reaction solutions of a kind of configuration in following situations are selected：Situation one：The first solution is metal cation solution, and its solute is copper acetate, concentration 0.015mol/L-0.025mol/L, molten Agent is that volume ratio is 1:2 DMF and acetonitrile mixture,Second is organic ligand solution；Its solute is terephthalic acid (TPA), concentration 0.005mol/L-0.015mol/L, solvent It is that volume ratio is 2:1 N,N-dimethylformamide and acetonitrile mixture；Situation two：The first solution is metal cation solution, and its solute is zinc acetate, concentration 0.0055mol/L-0.0065mol/L, Solvent is that volume ratio is 1:2 DMF and acetonitrile mixture,Second is organic ligand solution；Its solute is terephthalic acid (TPA), concentration 0.005mol/L-0.015mol/L, solvent It is that volume ratio is 2:1 N,N-dimethylformamide and acetonitrile mixture；Situation three：The first solution is metal cation solution, and its solute is cobalt acetate, concentration 0.15mol/L, and solvent is N, N- diformazans Base formamide,Second is organic ligand solution；Its solute is terephthalic acid (TPA), concentration 0.15mol/L, and solvent is N, N- dimethyl Formamide；(2) soak：Basilar fibers is immersed in organic ligand solution, taken out to after being impregnated with；(3) spray：Metal cation solution is small as making it be separated into drop by ultrasonic wave in spray solution injection nozzle Particle, sprayed with mist from shower nozzle；Solution after atomization uniformly fall lower section immersion organic ligand solution substrate On fiber, two kinds of solution start to construct metal organic framework compound after fiber surface contact, and then obtain the organic bone of metal The fiber of frame compound parcel；The fiber of obtained metal organic framework compound parcel by being immersed in N, N- dimethyl repeatedly Purifying is washed in formamide.
- 2. the method according to claim 1 that metal organic framework compound parcel fiber is prepared using spray-on process, it is special Sign is：For the spray solution by auto injection pump injection nozzle, the parameter of auto injection pump is the μ L/min of flow 30, during spraying Between be 400s.
- 3. the method according to claim 1 or 2 that metal organic framework compound parcel fiber is prepared using spray-on process, its It is characterised by：The basilar fibers is one kind in carbon felt fiber, cotton fiber or organic fiber.
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| CN201710994152.1A CN107794767B (en) | 2017-10-23 | 2017-10-23 | Method for preparing metal organic framework compound coated fibers by using spraying method |
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| CN201710994152.1A CN107794767B (en) | 2017-10-23 | 2017-10-23 | Method for preparing metal organic framework compound coated fibers by using spraying method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113437279A (en) * | 2021-08-26 | 2021-09-24 | 河南师范大学 | Preparation method of MOFs-coated high-conductivity multi-wall carbon nanotube composite material and application of MOFs-coated high-conductivity multi-wall carbon nanotube composite material in potassium ion battery |
| US11840057B2 (en) | 2021-03-02 | 2023-12-12 | Embry-Riddle Aeronautical University, Inc. | Metal organic framework modifications of structural fibers |
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| CN105133317A (en) * | 2015-08-16 | 2015-12-09 | 哈尔滨工业大学宜兴环保研究院 | Method for modification of carbon fiber surface by use of metal organic framework |
| CN107022095A (en) * | 2017-04-27 | 2017-08-08 | 东北大学 | A kind of method that utilization spray-on process prepares metal organic framework film |
| CN107201645A (en) * | 2017-04-28 | 2017-09-26 | 东华大学 | A kind of metal organic frame/carbon nano-fiber composite film material and preparation method thereof |
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2017
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| CN105133317A (en) * | 2015-08-16 | 2015-12-09 | 哈尔滨工业大学宜兴环保研究院 | Method for modification of carbon fiber surface by use of metal organic framework |
| CN107022095A (en) * | 2017-04-27 | 2017-08-08 | 东北大学 | A kind of method that utilization spray-on process prepares metal organic framework film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11840057B2 (en) | 2021-03-02 | 2023-12-12 | Embry-Riddle Aeronautical University, Inc. | Metal organic framework modifications of structural fibers |
| CN113437279A (en) * | 2021-08-26 | 2021-09-24 | 河南师范大学 | Preparation method of MOFs-coated high-conductivity multi-wall carbon nanotube composite material and application of MOFs-coated high-conductivity multi-wall carbon nanotube composite material in potassium ion battery |
| CN113437279B (en) * | 2021-08-26 | 2021-11-16 | 河南师范大学 | Preparation method of MOFs-coated high-conductivity multi-wall carbon nanotube composite material and application of MOFs-coated high-conductivity multi-wall carbon nanotube composite material in potassium ion battery |
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