CN105200477A - Equipment for preparing MOF (Metal organic framework) membrane by multielectrode electrodeposition - Google Patents
Equipment for preparing MOF (Metal organic framework) membrane by multielectrode electrodeposition Download PDFInfo
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- CN105200477A CN105200477A CN201510569727.6A CN201510569727A CN105200477A CN 105200477 A CN105200477 A CN 105200477A CN 201510569727 A CN201510569727 A CN 201510569727A CN 105200477 A CN105200477 A CN 105200477A
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Abstract
The invention discloses equipment for preparing an MOF (Metal organic framework) membrane by a multielectrode electrodeposition method. The equipment comprises a structural combined rack, anodes, cathodes and the like, wherein the structural combined rack consists of two polytetrafluoroethylene circular plates, i.e., an upper polytetrafluoroethylene circular plate and a lower polytetrafluoroethylene circular plate, polytetrafluoroethylene connectors and polytetrafluoroethylene cylinders; the anodes are cylindrical anodes, pore passages and grooves, which are used for embedding the cylindrical anodes, are formed in the upper and lower polytetrafluoroethylene circular plates in the whole structural combined rack, the distribution of the cylindrical anodes is determined according to actual demands on the distance from the anodes to the cathodes and the distance among the cylindrical anodes, and the cylindrical anodes are made from high-purity red-copper bars; the cathodes are tubular carbon materials or other conductive materials and are embedded in the annular grooves of the lower polytetrafluoroethylene circular plate through the hole passages in the upper polytetrafluoroethylene circular plate, and the tubular cathodes are uniformly distributed in a circular electric field formed by the anodes. The equipment has the characteristics of simplicity in preparation, convenience in assembly, high working efficiency and the like and has an important application value in growing the MOF membrane on the surface of a tubular material by the electrodeposition method.
Description
Technical field
The present invention relates to a kind of galvanic deposit equipment, is that MOF film equipment is prepared in a kind of multi-electrode galvanic deposit specifically.
Background technology
Metal-organic framework materials (MOF), be often referred to metal ion or metal cluster and organic ligand and formed the crystalline material with periodically infinite network structure by self assembling process, a member is obtained as emerging porous material, many advantages of MOF collection of material inorganic porous material and porous material, as good mechanical stability, higher voidage, larger specific surface area, higher rate of permeation, with excellent proton conductivity etc., it is had broad application prospects, becomes the focus of scientific research.Nowadays, the laboratory of MOF film is prepared major part and is rested on hydrothermal method and all kinds of Improving ways.But hydrothermal method can the feature such as uncontrollability and cycle length make MOF production efficiency not high, and electrodip process grows MOF and has bibliographical information on copper mesh, and relative to the carrier of sheet, the surface-area of tubulose is large, is easily assembled into assembly, has higher using value.Tubular material, due to own form problem, makes stressed uneven on its surface, is difficult to the film obtaining dense uniform.Form uniform electric field by galvanic deposit way, tubing each several part uniform force, more easily forms high quality, firmly MOF film.
Summary of the invention
The object of the invention is: for prior art vacancy, research and develop a kind of multi-electrode galvanic deposit and prepare MOF film equipment, the present invention makes simply, combined and instant, working efficiency high; Significant application value is had at tubular material surface growth MOF film for by galvanic deposit way.
In order to solve the problem, technical scheme of the present invention is: a kind of multi-electrode electrodip process prepares the equipment of MOF film, comprise textural association frame, anode, negative electrode etc., textural association frame is made up of upper and lower two polytetrafluoro plectanes, polytetrafluoro linker, polytetrafluoro cylinder; Anode is cylindrical anode, the duct and groove that can be used for intercalation cylindrical anode is provided with in the plectane of polytetrafluoro up and down of total combined bay, the arrangement of cylindrical anode by cathode spacing from and each cylindrical anode spacing actual needs determine, cylindrical anode is processed by high-purity red copper bar; Negative electrode is tubulose carbon material or other electro-conductive materials, its by polytetrafluoro plectane (on) duct intercalation polytetrafluoro plate (under) annular recesses in, sleeve cathode is evenly distributed in the circular electric field of anodic formation.
Described cylindrical anode is film forming material donor, and described sleeve cathode is the carrier of film forming material.
Described cylindrical anode is high purity red copper (copper content >=99.9%) and processes, diameter 5-6mm, height 65-70mm, distance sleeve cathode center 14-15mm.
Described sleeve cathode is conductive carbon pipe, and carbon tube-surface is distributed with the hole of 10-30 μm.
The smooth surface or coarse of described sleeve cathode.
Described textural association frame material is polytetrafluoro sheet material or acid and alkali-resistance rubber.
Described annular recesses diameter is identical with sleeve cathode diameter, and the degree of depth is 3-4mm.
The gap formed between 5 described polytetrafluoro cylinders can hold the magneton of magnetic agitation.
Described polytetrafluoro body diameter 6-8mm, degree of depth 10mm.
The present invention has the following advantages: 1) this equipment makes simple, and combined and instant is with low cost.2) adopt multianode electrode to be evenly distributed on around cathode tube, form uniform electric field, uniform current density around negative electrode, is conducive to the complete plating of cathode.3) be provided with magneton stirring system between device 5 pillar, the effective concentration polarization eliminated in electrolytic solution, substantially increases the higher limit of cathode current density, coating is flattened.4) using polytetrafluoro or acid and alkali-resistance rubber as the integral frame of whole equipment, anode and cathode is convenient to extract, and the replacing especially for anode consumptive material is significant.5) circular anode and sleeve cathode experimentally need to carry out replacement of function, and namely circular anode serves as negative electrode, and sleeve cathode serves as anode, and this plays an important role for deposition MOF, reduces the cost of experiment simultaneously.6) this device also can be used for the preparation of other associated metal title complexs.
Accompanying drawing explanation
Below in conjunction with practical examples and accompanying drawing, apparatus of the present invention are further illustrated:
Fig. 1 is the local structure view that MOF film equipment is prepared in multi-electrode galvanic deposit;
Fig. 2 is the local structure view of combined electrical deposition MOF film equipment;
Fig. 3 is the three-dimensional arrangement view of combined electrical deposition MOF film equipment;
Fig. 4 is through the environmental scanning figure of the Cu-BTC film of combined electrical deposition MOF film equipment deposition.
In figure: 1, polytetrafluoro plectane (on); 2, polytetrafluoro plectane (under); 3, polytetrafluoro cylinder; 4, polytetrafluoro linker; 5, duct; 6, cylindrical anode; 7, annular recesses; 8, groove; 9, polytetrafluoro plectane (on) duct; 10, sleeve cathode.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail: as shown in Figure 1, 2, 3, the present invention relates to the equipment that a kind of multi-electrode electrodip process prepares MOF film, comprise textural association frame, anode, negative electrode etc., textural association frame is made up of upper and lower two polytetrafluoro plectanes 1 and 2,4 polytetrafluoro linkers, 4,5 polytetrafluoro cylinders 3; Anode is that 12 cylindrical anodes 6 combine, the duct 5 and groove 8 that can be used for intercalation cylindrical anode is provided with in the plectane of polytetrafluoro up and down 1 and 2 of total combined bay, the arrangement of cylindrical anode 6 by cathode spacing from and each cylindrical anode spacing actual needs determine, cylindrical anode 6 is processed by high-purity red copper bar; Negative electrode 10 is tubulose carbon material or other electro-conductive materials, its by polytetrafluoro plectane (on) duct 9 intercalation polytetrafluoro plate (under) annular recesses 7 in, sleeve cathode 10 be evenly distributed on anode 6 formed circular electric field in.
Described cylindrical anode 6 is film forming material donor, and described sleeve cathode 10 is the carrier of film forming material.
Described cylindrical anode 6 is high purity red copper (copper content >=99.9%) and processes, diameter 5-6mm, height 65-70mm, distance sleeve cathode 10 center 14-15mm.
Described sleeve cathode 10 is conductive carbon pipe, and carbon tube-surface is distributed with the hole of 10-30 μm.
The smooth surface or coarse of described sleeve cathode 10.
Described textural association frame 1,2,3,4 material is polytetrafluoro sheet material or acid and alkali-resistance rubber.
Described annular recesses 7 diameter is identical with sleeve cathode (10) diameter, and the degree of depth is 3-4mm.
The gap formed between 5 described polytetrafluoro cylinders 3 can hold the magneton of magnetic agitation.
Described polytetrafluoro cylinder 3 diameter 6-8mm, degree of depth 10mm.
Below in conjunction with specific embodiment, device of the present invention is described:
Multi-electrode electrodip process prepares an equipment for MOF film, by cylindrical anode 6 with sleeve cathode 10 is equidistantly evenly distributed combines; Described cylindrical anode 6 is high purity red copper (copper content >=99.9%) and processes, diameter 5-6mm, height 65-70mm, distance sleeve cathode center 14-15mm; Described sleeve cathode 10 is conductive carbon pipe, and carbon tube-surface is distributed with the hole of 10-30 μm; Described cylindrical anode 6 is film forming material donor, and described sleeve cathode 10 is the carrier of film forming material.Textural association frame is by upper and lower two polytetrafluoro plectanes 1,2, and 4 polytetrafluoro linkers, 4,5 polytetrafluoro cylinders 3 form, and are provided with the duct 5 and groove 8 that can be used for intercalation cylindrical anode in the plectane of polytetrafluoro up and down 1 and 2 of total combined bay.12 described cylindrical anode passing hole channels 5 are intercalated in groove 8, circular electric field is formed with the sleeve cathode 10 being embedded in lower polytetrafluoro plectane 2 annular recesses 7, the smooth surface or coarse of described sleeve cathode 10, described annular recesses 7 diameter is identical with sleeve cathode (10) diameter, and the degree of depth is 3-4mm.The gap formed between 5 described polytetrafluoro cylinders 3 can hold the magneton of magnetic agitation.Described polytetrafluoro cylinder 3 diameter 6-8mm, degree of depth 10mm.
During work, first copper facing on sleeve cathode 10, in the copper sulfate bath adding apparatus of preparation 2.5-5g/L, puts magneton and opens stirring; Arranging voltage is 1.5V, electric current 0.1A, and electroplating time is 20-30min; After copper facing terminates, washing unit; The trimesic acid adding apparatus of preparation 16mg/mL, make anode with the sleeve cathode 10 plating layers of copper, 12 cylindrical anodes 6 are now as negative electrode, and voltage 2.0V, electric current 0.05A, temperature 50-55 degree Celsius, depositing time 20min, obtains Cu-BTC film.
As shown in Figure 4, be the environmental scanning figure of the Cu-BTC film of deposition obtained above.
Above-described embodiment is only for illustration of technological thought of the present invention and feature, its object is to enable those skilled in the art understand device of the present invention and principle and implement according to this, only can not limit the scope of the claims of the present invention with the present embodiment, namely the equal change done of all disclosed spirit or modification, still drop in the scope of the claims of the present invention.
Claims (9)
1. MOF film equipment is prepared in a multi-electrode galvanic deposit, comprise textural association frame, anode, negative electrode etc., it is characterized in that textural association frame is made up of upper and lower two polytetrafluoro plectanes (1) (2), 4 polytetrafluoro linkers (4), 5 polytetrafluoro cylinders (3); Anode is 12 cylindrical anode (6) combinations, the duct (5) that can be used for intercalation cylindrical anode and groove (8) is provided with in the plectane of polytetrafluoro up and down (1) (2) of total combined bay, the arrangement of cylindrical anode (6) by cathode spacing from and each cylindrical anode spacing actual needs determine, cylindrical anode (6) is processed by high-purity red copper bar; Negative electrode (10) is tubulose carbon material or other electro-conductive materials, its by polytetrafluoro plectane (on) duct (9) intercalation polytetrafluoro plate (under) annular recesses (7) in, sleeve cathode (10) is evenly distributed in the circular electric field that anode (6) formed.
2. MOF film equipment is prepared in a kind of multi-electrode galvanic deposit according to claim 1, it is characterized in that, by cylindrical anode (6) with sleeve cathode (10) is equidistantly evenly distributed combines.
3. MOF film equipment is prepared in a kind of multi-electrode galvanic deposit according to claim 1, it is characterized in that, by cylindrical anode (6) with sleeve cathode (10) is equidistantly evenly distributed combines; Described circular anode is high purity red copper (copper content >=99.9%) and processes, diameter 5-6mm, height 65-70mm, distance sleeve cathode center 14-15mm.
4. MOF film equipment is prepared in a kind of multi-electrode galvanic deposit according to claim 1, and it is characterized in that, sleeve cathode (10) is conductive carbon pipe, and carbon tube-surface is distributed with the hole of 10-30 μm.
5. MOF film equipment is prepared in a kind of multi-electrode galvanic deposit according to claim 1, it is characterized in that, the smooth surface or coarse of described sleeve cathode (10).
6. MOF film equipment is prepared in a kind of multi-electrode galvanic deposit according to claim 1, and it is characterized in that, textural association frame material is polytetrafluoro sheet material or acid and alkali-resistance rubber.
7. MOF film equipment is prepared in a kind of multi-electrode galvanic deposit according to claim 1, and it is characterized in that, described annular recesses (7) diameter is identical with sleeve cathode diameter, and the degree of depth is 3-4mm.
8. MOF film equipment is prepared in a kind of multi-electrode galvanic deposit according to claim 1, and it is characterized in that, the gap formed between described 5 polytetrafluoro cylinders (3) can hold the magneton of magnetic agitation.
9. MOF film equipment is prepared in a kind of multi-electrode galvanic deposit according to claim 1 and 8, it is characterized in that, polytetrafluoro cylinder (3) diameter 6-8mm, degree of depth 10mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510569727.6A CN105200477A (en) | 2015-09-07 | 2015-09-07 | Equipment for preparing MOF (Metal organic framework) membrane by multielectrode electrodeposition |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498447A (en) * | 2016-11-23 | 2017-03-15 | 北京建筑大学 | The batch electrochemistry formated device and method of metal-organic framework materials |
| CN107574465A (en) * | 2017-08-14 | 2018-01-12 | 哈尔滨理工大学 | A kind of preparation method of the films of hollow IRMOF 3 |
| CN107620114A (en) * | 2017-11-10 | 2018-01-23 | 中航飞机起落架有限责任公司 | A kind of electroplating anode device and chrome-plating method |
| CN108220619A (en) * | 2018-01-26 | 2018-06-29 | 宁波华成阀门有限公司 | A kind of high-purity red copper and its manufacturing method |
| CN108614026A (en) * | 2018-05-02 | 2018-10-02 | 重庆大学 | Electrochemistry teaching or testing equipment and its assemble method |
| CN109046473A (en) * | 2018-09-07 | 2018-12-21 | 中南大学 | A kind of transition metal modification TiO2The combination electrode and the preparation method and application thereof of-MOFs film |
| CN110029382A (en) * | 2019-05-22 | 2019-07-19 | 电子科技大学 | A kind of process of surface treatment and its related directly electroplating technology for being directly electroplated |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104073863A (en) * | 2014-07-22 | 2014-10-01 | 天津工业大学 | Combined type device for plating MOF film through electrodeposition method |
-
2015
- 2015-09-07 CN CN201510569727.6A patent/CN105200477A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104073863A (en) * | 2014-07-22 | 2014-10-01 | 天津工业大学 | Combined type device for plating MOF film through electrodeposition method |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498447A (en) * | 2016-11-23 | 2017-03-15 | 北京建筑大学 | The batch electrochemistry formated device and method of metal-organic framework materials |
| CN107574465A (en) * | 2017-08-14 | 2018-01-12 | 哈尔滨理工大学 | A kind of preparation method of the films of hollow IRMOF 3 |
| CN107574465B (en) * | 2017-08-14 | 2019-04-12 | 哈尔滨理工大学 | A kind of preparation method of hollow IRMOF-3 film |
| CN107620114A (en) * | 2017-11-10 | 2018-01-23 | 中航飞机起落架有限责任公司 | A kind of electroplating anode device and chrome-plating method |
| CN107620114B (en) * | 2017-11-10 | 2019-07-19 | 中航飞机起落架有限责任公司 | A kind of electroplating anode device and chrome-plating method |
| CN108220619A (en) * | 2018-01-26 | 2018-06-29 | 宁波华成阀门有限公司 | A kind of high-purity red copper and its manufacturing method |
| CN108614026A (en) * | 2018-05-02 | 2018-10-02 | 重庆大学 | Electrochemistry teaching or testing equipment and its assemble method |
| CN109046473A (en) * | 2018-09-07 | 2018-12-21 | 中南大学 | A kind of transition metal modification TiO2The combination electrode and the preparation method and application thereof of-MOFs film |
| CN109046473B (en) * | 2018-09-07 | 2021-03-05 | 中南大学 | Transition metal modified TiO2Composite electrode of MOFs film and preparation method and application thereof |
| CN110029382A (en) * | 2019-05-22 | 2019-07-19 | 电子科技大学 | A kind of process of surface treatment and its related directly electroplating technology for being directly electroplated |
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