CN106222718B - A kind of electro-deposition method of carboxymethyl cellulose - Google Patents
A kind of electro-deposition method of carboxymethyl cellulose Download PDFInfo
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Abstract
The present invention relates to a kind of electro-deposition methods of carboxymethyl cellulose.A kind of electro-deposition method of carboxymethyl cellulose, which is characterized in that it includes the following steps:1)Prepare carboxymethyl cellulose electrodeposit liquid;2)The preparation of metal electrode material:Using the anode metal material of metallic copper or metallic cobalt as carboxymethyl cellulose electro-deposition, using cathodic metal material of the platinized platinum as carboxymethyl cellulose electro-deposition;3)The electro-deposition of carboxymethyl cellulose:Anode and cathode are immersed in simultaneously in the container equipped with carboxymethyl cellulose electrodeposit liquid, and anode and cathode are connected to DC power supply, carry out the electro-deposition of carboxymethyl cellulose, sedimentation time is 3~10 minutes, obtains being electrodeposited in the carboxymethyl cellulose deposition layer of anode metal electrodes material surface.This method electro-deposition can form carboxymethyl cellulose deposition layer on metal electrode, have the advantages that preparation condition is mild, simple to operate, easily controllable, instrument and equipment is simple, environmentally protective, favorable repeatability, of low cost.
Description
Technical field
The invention belongs to fields such as high molecular material, biological macromolecule material, electrochemistry, Coordinative Chemistry, more particularly to
A kind of electro-deposition method of carboxymethyl cellulose.
Background technology
Electro-deposition techniques can provide method simply and easily, controllable to cause big point of the biology with stimulating responsive
The assembling of son, and formed on metal electrode sedimentary [Biosensors and Bioelectronics, 2016,80:222-
229].Conducting polymer thin film, biological devices, large biological molecule gel etc. can be built by electro-deposition techniques, can also be led to
Cross the method being co-deposited realize nano material, biological substance etc. on the electrode assembling [Polymers, 2015,7:1-46].Electricity
Deposition technique has accurate space time selectivity and controllability, and Simultaneous Electrodeposition technology has easy to operate, mild condition,
A variety of large biological molecules can be realized in different types of electrode and substrate surface electro-deposition using the technology, therefore are passed in biology
The fields such as sensor, drug release have a good application prospect.
Large biological molecule is stored in extensively in nature in animals and plants and microorganism, the high molecular material phase with chemical synthesis
Than, large biological molecule have the advantages that many performance characteristics and, such as material source is extensive, good biocompatibility, biology drop
Xie Xing, environment friendly and recyclability etc.;And there are many contain some reaction active groups (such as carboxylic in large biological molecule
The groups such as base, amino and hydroxyl), therefore can be modified to prepare the material of different demands by the methods of chemistry, physics
Material.Carboxymethyl cellulose is a kind of water soluble anion polysaccharide [Carbohydrate having no toxic and side effect to human body
Polymers, 2014,112:32-38] and use scope is most wide at present, cellulose derivative of dosage maximum;Carboxymethyl is fine
Dimension element is white or micro- yellowish fiber element powder, have it is odorless, tasteless, nontoxic, be dissolved in the performance characteristics such as water, be widely used
In the materials such as biology, medicine, hydrogel, such as film forming agent, binder and emulsion stabilizer.In addition, carboxymethyl is fine
Dimension element has metal ion stronger coordination ability [Biomacromolecules 2007,8,2762-2767], such as carboxylic first
Base cellulose has coordination to copper ion, and coordination product can directly be precipitated in the solution, and precipitate is flocculent deposit.
In summary, if it is possible to be directly realized by carboxymethyl cellulose in electro-deposition on the metal material, will build
The gel of large biological molecule or natural polymer carboxymethyl derivant, film, electrode modified material, biosensor, detector,
Bioelectrode etc. has good application value.However, phase is had no about the electro-deposition method of carboxymethyl cellulose at present
Close document and patent report.
Invention content
The technical problem to be solved by the present invention is to:There is provided a kind of electro-deposition method of carboxymethyl cellulose, this method can be
Electro-deposition forms carboxymethyl cellulose deposition layer on metal electrode, and can easily be removed from surface of metal electrode, also holds
Easily obtaining has certain thickness carboxymethyl cellulose deposition layer;This method have preparation condition it is mild, it is simple to operate,
It is easily controllable, instrument and equipment is simple, environmentally protective, favorable repeatability, it is of low cost the advantages of.
The technical solution that there is provided to solve above-mentioned technical problem of the present invention is:A kind of electro-deposition side of carboxymethyl cellulose
Method, which is characterized in that it includes the following steps:
1) carboxymethyl cellulose electrodeposit liquid is prepared:Carboxymethyl cellulose powder is added in, quality percentage is prepared in distilled water
Specific concentration is 1%~3% cmc soln, carries out magnetic agitation at 15~30 DEG C until carboxymethyl cellulose powder
Last fully dissolving, then by the decompression of the cmc soln of configuration filter 1~2 time (vacuum degree that decompression filters for-
0.03MPa~-0.08MPa), remove undissolved carboxymethyl cellulose completely, be prepared mass percent concentration for 1%~
3% carboxymethyl cellulose electrodeposit liquid;
2) preparation of metal electrode material (cathode and anode):Using metallic copper or metallic cobalt as carboxymethyl cellulose electricity
The anode metal material (anode metal materials such as copper or cobalt sheet metal of different shapes, wire, metal bar) of deposition, first uses sand
Paper is to carefully carrying out polishing until flat smooth at the out-of-flatness on the surface and edge of anode metal material, then by anode metal material
Material is cleaned by ultrasonic 5~15 minutes respectively in distilled water, absolute ethyl alcohol, acetone, distilled water successively, and (ultrasonic power is 50-60
Watt), then this anode metal material is cleaned by ultrasonic in the hydrochloric acid solution of 0.5~2.0M 1~3 minute (ultrasonic power is 50-
60 watts), it is then again dipped into distilled water and is cleaned by ultrasonic 5~15 minutes (ultrasonic power is 50-60 watts), obtain required sun
Pole metal electrode material, it is spare;
Using cathodic metal material of the platinized platinum as carboxymethyl cellulose electro-deposition, by platinized platinum successively in absolute ethyl alcohol, third
It is cleaned by ultrasonic respectively in ketone, distilled water 5~15 minutes (ultrasonic power is 50-60 watts), it is spare;
3) electro-deposition of carboxymethyl cellulose:20~30mL of carboxymethyl cellulose electrodeposit liquid prepared by step 1) is taken to add
Enter container (such as:Small beaker) in, ultrasonic de-soak 3~5 minutes (ultrasonic power is 50-60 watts);Then using accurate in step 2)
For the anode metal electrodes material (copper or cobalt metal material) got ready as anode, cathodic metal material (platinized platinum), will as cathode
Anode and cathode are immersed in the container equipped with carboxymethyl cellulose electrodeposit liquid (such as simultaneously:Small beaker) in, and by anode and the moon
Pole is connected to DC power supply (high precision DC power supply), and DC power supply is adjusted to constant voltage mode, and voltage is set as 0.5~1.5V,
The electro-deposition of carboxymethyl cellulose is carried out, sedimentation time is 3~10 minutes;DC power supply is closed after electro-deposition, takes out table
Face electro-deposition has the anode of carboxymethyl cellulose deposition layer, cleans anode surface 5~15 times with distilled water, is electrodeposited in
The carboxymethyl cellulose deposition layer on anode metal electrodes material (copper or cobalt metal material) surface.
A kind of connected applications of the electro-deposition method of carboxymethyl cellulose of the present invention also for electronic technology and biotechnology carry
Supplied effective ways and approach, can be applied to biosensor, detector, chip lab, biomedical metal material modification, with
And the fields such as co-deposition for realizing nano material and biological substance.A kind of electro-deposition method of carboxymethyl cellulose of the present invention,
It can be applied to carry out other large biological molecules or the electricity of natural polymer carboxymethyl derivant (such as carboxymethyl chitosan) sink
Product has in the gel of structure large biological molecule or natural polymer carboxymethyl derivant, film, electrode modified material etc.
Good application value.
The technical principle of the present invention:It, can be with copper ion, cobalt containing groups such as carboxyls in the strand of carboxymethyl cellulose
Coordination occurs for the metal ions such as ion, forms the complex of carboxymethyl cellulose and metal ion.In electro-deposition
Cheng Zhong, after voltage is applied on metal electrode, the anode electrochemical oxidation reaction that metal electrode occurs forms metal ion;Such as
When using metallic copper as anode, the electrochemical oxidation reactions of anode form copper ion, when using metallic cobalt as anode,
The electrochemical oxidation reactions of anode form cobalt ions;Then these metal ions further with the carboxymethyl cellulose in electrodeposit liquid
Coordination occurs for element, so as to form carboxymethyl cellulose deposition layer in surface of metal electrode electro-deposition.The present invention while profit
The electrochemical oxidation reactions occurred with anode can form metal ion with coordination ability and carboxymethyl cellulose can be with
The characteristics of coordination occurs with metal ion, it is heavy so as to fulfill the direct electricity that carboxymethyl cellulose is carried out on metal electrode
Product.
The beneficial effects of the invention are as follows:
1) the present invention provides a kind of electro-deposition method of carboxymethyl cellulose, this method is utilized in electrodeposition process,
Metal electrode can generate metal ion in the electrochemical oxidation reactions that anode occurs, these metal ions can be with carboxymethyl cellulose
Coordination occurs for element, and so as to fulfill electro-deposition of the carboxymethyl cellulose on metal electrode, being that one kind is novel can realize
The method of the direct electro-deposition of carboxymethyl cellulose.
2) a kind of electro-deposition method of carboxymethyl cellulose of the present invention, prepared carboxymethyl cellulose deposition layer appearance
Flat smooth, surface bubble-free, and can easily be removed from surface of metal electrode, it is also easy to get with certain thickness carboxylic
Methylcellulose deposition layer.
3) a kind of electro-deposition method of carboxymethyl cellulose of the present invention, the carboxymethyl cellulose used in this method have source
Extensively, good biocompatibility, nontoxicity, biodegradability, environment friendly and green it is renewable the features such as and advantage,
Therefore it is advantageous to application of the prepared carboxymethyl cellulose electrodeposited material in bio-medical field.
4) a kind of electro-deposition method of carboxymethyl cellulose of the present invention, have preparation condition it is mild, it is easy to operate, be easy to control
System, instrument and equipment are simple, favorable repeatability, it is environmentally protective, of low cost the features such as and advantage, this method be also equipped with space and when
Between selectivity and the features such as controllability.
Description of the drawings
Fig. 1 is photo of the embodiment of the present invention 1 in metallic copper on piece electro-deposition carboxymethyl cellulose deposition layer.
Fig. 2 is the photo that the embodiment of the present invention 2 powers on deposition carboxymethyl cellulose deposition layer in metal copper wire.
Fig. 3 is that the embodiment of the present invention 3 is ultraviolet at 254 nanometers in metallic cobalt on piece electro-deposition carboxymethyl cellulose deposition layer
Fluorescence photo under lamp.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples, and certain following embodiments should not be construed as pair
The limitation of the present invention.
The present invention provides a kind of electro-deposition method of carboxymethyl cellulose, with reference to specific embodiment prepared by the present invention
Method is described further, but does not limit the present invention.
Embodiment 1
A kind of electro-deposition method of carboxymethyl cellulose, it is comprised the following specific steps that:
1) carboxymethyl cellulose electrodeposit liquid is prepared:Carboxymethyl cellulose powder is (limited from Chinese medicines group chemical reagent
Company buys) cmc soln for preparing that mass percent concentration is 1% is added in distilled water, magnetic is carried out at 15 DEG C
Power stirring is fully dissolved up to carboxymethyl cellulose powder, then filters the decompression of the cmc soln of configuration 1 time, complete
Remove entirely undissolved carboxymethyl cellulose (cmc soln of the mass percent concentration 1% in order to obtain, with
During cmc soln processed, can suitably add into some carboxymethyl cellulose solid samples), mass percent is prepared
A concentration of 1% carboxymethyl cellulose electrodeposit liquid;
2) preparation of metal electrode material (cathode and anode):Using metal copper sheet as carboxymethyl cellulose electro-deposition
Anode metal material, will first with sand paper to carefully carrying out polishing at the out-of-flatness on the surface and edge of copper sheet up to flat smooth
Anode metal material after polishing is cleaned by ultrasonic 5 minutes respectively in distilled water, absolute ethyl alcohol, acetone, distilled water successively, then will
This anode metal material is cleaned by ultrasonic 3 minutes in the hydrochloric acid solution of 0.5M, is then again dipped into distilled water and is cleaned by ultrasonic 5 points
Clock obtains required anode metal electrodes material, spare;
Using cathodic metal material of the platinized platinum as carboxymethyl cellulose electro-deposition, by platinized platinum successively in absolute ethyl alcohol, third
It is cleaned by ultrasonic respectively in ketone, distilled water 5 minutes, it is spare;
3) electro-deposition of carboxymethyl cellulose:The carboxymethyl cellulose electrodeposit liquid 20mL prepared by step 1) is taken to add in small
In beaker, ultrasonic de-soak 3 minutes;Then using ready copper sheet in step 2) as anode, platinized platinum is as cathode, by anode
It is immersed in simultaneously with cathode in the small beaker equipped with carboxymethyl cellulose electrodeposit liquid, and anode and cathode is connected to direct current
Source (high precision DC power supply), DC power supply are adjusted to constant voltage mode, and voltage is set as 0.5, carry out the electricity of carboxymethyl cellulose
Deposition, sedimentation time are 10 minutes;DC power supply is closed after electro-deposition, taking out surface electro-deposition has carboxymethyl cellulose electricity
The copper sheet of sedimentary, anode surface is carefully cleaned with distilled water 5 times, obtains being electrodeposited in the carboxymethyl cellulose on metal copper sheet surface
Plain deposition layer.
Fig. 1 is photo of the embodiment of the present invention 1 in metallic copper on piece electro-deposition carboxymethyl cellulose deposition layer.By Fig. 1
It can be found that when using metal copper sheet as anode metal material, one layer of apparent carboxylic is formed on copper sheet surface after electro-deposition
Methylcellulose deposition layer, the carboxymethyl cellulose deposition layer have certain thickness gel mould, flat appearance in blue
It is smooth, surface bubble-free, and can easily be removed from metal copper plate electrode surface, film has certain intensity;Above-mentioned knot
Fruit illustrates, using a kind of electro-deposition method of carboxymethyl cellulose of the present invention, can obtain carboxymethyl cellulose in metallic copper on piece
Plain deposition layer.
Embodiment 2
A kind of electro-deposition method of carboxymethyl cellulose, it is comprised the following specific steps that:
1) carboxymethyl cellulose electrodeposit liquid is prepared:Carboxymethyl cellulose powder is added in, quality percentage is prepared in distilled water
Specific concentration is 3% cmc soln, carries out magnetic agitation at 30 DEG C until carboxymethyl cellulose powder is fully molten
Then the decompression of the cmc soln of configuration is filtered 2 times, removes undissolved carboxymethyl cellulose completely, prepared by solution
Obtain the carboxymethyl cellulose electrodeposit liquid that mass percent concentration is 3%;
2) preparation of metal electrode material (cathode and anode):Using metal copper wire as carboxymethyl cellulose electro-deposition
Anode metal material, first with sand paper to carefully carrying out polishing at the out-of-flatness on the surface of copper wire up to flat smooth, after polishing
Anode metal material be cleaned by ultrasonic respectively in distilled water, absolute ethyl alcohol, acetone, distilled water 15 minutes successively, then by this sun
Pole metal material is cleaned by ultrasonic 1 minute in the hydrochloric acid solution of 2.0M, is then again dipped into distilled water and is cleaned by ultrasonic 15 minutes
Required anode metal electrodes material is obtained, it is spare;
Using cathodic metal material of the platinized platinum as carboxymethyl cellulose electro-deposition, by platinized platinum successively in absolute ethyl alcohol, third
It is cleaned by ultrasonic respectively in ketone, distilled water 15 minutes, it is spare;
3) electro-deposition of carboxymethyl cellulose:The carboxymethyl cellulose electrodeposit liquid 30mL prepared by step 1) is taken to add in small
In beaker, ultrasonic de-soak 5 minutes;Then using ready copper wire in step 2) as anode, platinized platinum is as cathode, by anode
It is immersed in simultaneously with cathode in the small beaker equipped with carboxymethyl cellulose electrodeposit liquid, and anode and cathode is connected to direct current
Source (high precision DC power supply), DC power supply are adjusted to constant voltage mode, and voltage is set as 1.5V, carry out the electricity of carboxymethyl cellulose
Deposition, sedimentation time are 3 minutes;DC power supply is closed after electro-deposition, taking out surface electro-deposition has carboxymethyl cellulose electricity
The copper wire of sedimentary, anode surface is carefully cleaned with distilled water 15 times, and the carboxymethyl for obtaining being electrodeposited in metallic copper silk table face is fine
The plain deposition layer of dimension.
Fig. 2 is the photo that the embodiment of the present invention 2 powers on deposition carboxymethyl cellulose deposition layer in metal copper wire.By Fig. 2
It can be found that formd when using metal copper wire as anode metal material, after electro-deposition in metallic copper silk table face one layer it is bright
Aobvious carboxymethyl cellulose deposition layer, the carboxymethyl cellulose deposition layer have certain thickness gel mould, film in blue
Flat appearance, the smooth bubble-free in surface;The above results illustrate, utilize a kind of electro-deposition side of carboxymethyl cellulose of the present invention
Method can obtain carboxymethyl cellulose deposition layer on metal copper wire.
Embodiment 3
A kind of electro-deposition method of carboxymethyl cellulose, it is comprised the following specific steps that:
1) carboxymethyl cellulose electrodeposit liquid is prepared:Carboxymethyl cellulose powder is added in, quality percentage is prepared in distilled water
Specific concentration is 2% cmc soln, carries out magnetic agitation at 20 DEG C until carboxymethyl cellulose powder is fully molten
Then the decompression of the cmc soln of configuration is filtered 2 times, removes undissolved carboxymethyl cellulose completely, prepared by solution
Obtain the carboxymethyl cellulose electrodeposit liquid that mass percent concentration is 2%;
2) preparation of metal electrode material (cathode and anode):Using metallic cobalt piece as carboxymethyl cellulose electro-deposition
Anode metal material, will first with sand paper to carefully carrying out polishing at the out-of-flatness on the surface and edge of cobalt piece up to flat smooth
Anode metal material after polishing is cleaned by ultrasonic 10 minutes respectively in distilled water, absolute ethyl alcohol, acetone, distilled water successively, then
This anode metal material in the hydrochloric acid solution of 1.0M is cleaned by ultrasonic 2 minutes, is then again dipped into distilled water and is cleaned by ultrasonic
Required anode metal electrodes material is obtained within 10 minutes, it is spare;
Using cathodic metal material of the platinized platinum as carboxymethyl cellulose electro-deposition, by platinized platinum successively in absolute ethyl alcohol, third
It is cleaned by ultrasonic respectively in ketone, distilled water 10 minutes, it is spare;
3) electro-deposition of carboxymethyl cellulose:The carboxymethyl cellulose electrodeposit liquid 25mL prepared by step 1) is taken to add in small
In beaker, ultrasonic de-soak 4 minutes;Then using ready cobalt metal material in step 2) as anode, platinized platinum as cathode,
Anode and cathode are immersed in the small beaker equipped with carboxymethyl cellulose electrodeposit liquid, and anode and cathode are connected to simultaneously
DC power supply (high precision DC power supply), DC power supply are adjusted to constant voltage mode, and voltage is set as 1V, carries out carboxymethyl cellulose
Electro-deposition, sedimentation time be 6 minutes;DC power supply is closed after electro-deposition, taking out surface electro-deposition has carboxymethyl cellulose
The anode of plain deposition layer, anode surface is carefully cleaned with distilled water 10 times, obtains being electrodeposited in the carboxylic first on metallic cobalt piece surface
Base cellulose deposition layer.
Fig. 3 is that the embodiment of the present invention 3 is ultraviolet at 254 nanometers in metallic cobalt on piece electro-deposition carboxymethyl cellulose deposition layer
Fluorescence photo under lamp.The fluorescent staining method of carboxymethyl cellulose deposition layer is:In the carboxylic that mass percent concentration is 2%
Rhodamine 6G is added in for 0.1% according to mass percent concentration in methylcellulose electrodeposit liquid and carry out fluorescent staining, so as to make
The carboxymethyl cellulose deposition layer obtained in metallic cobalt on piece electro-deposition has fluorescence, then to it under 254 nanometers of ultraviolet lamps
Fluorescence is observed.By Fig. 3 it can be found that when using metallic cobalt piece as anode metal material, in metallic cobalt after electro-deposition
Piece surface forms carboxymethyl cellulose deposition layer, which sends out under 254 nanometers of ultraviolet lamps
Apparent fluorescence, flat appearance, the smooth bubble-free in surface;Illustrating can be in anode conducting metal material cobalt on piece using this method
Obtain carboxymethyl cellulose deposition layer;The above results illustrate, using a kind of electro-deposition method of carboxymethyl cellulose of the present invention,
Carboxymethyl cellulose deposition layer can be obtained in metallic cobalt on piece.
It should be noted that it will be understood by those of ordinary skill in the art that, technical scheme of the present invention can be carried out
Modification or equivalent replacement without departing from the objective and range of technical solution of the present invention, should all cover the right in the present invention
In claimed range.
Claims (3)
1. a kind of electro-deposition method of carboxymethyl cellulose, which is characterized in that it includes the following steps:
1)Prepare carboxymethyl cellulose electrodeposit liquid:It is dense that carboxymethyl cellulose powder is added in into preparation mass percent in distilled water
The cmc soln for 1%~3% is spent, carries out magnetic agitation at 15~30 DEG C until carboxymethyl cellulose powder is abundant
Then the decompression of the cmc soln of configuration is filtered 1~2 time, removes undissolved carboxymethyl cellulose completely by dissolving,
The carboxymethyl cellulose electrodeposit liquid that mass percent concentration is 1%~3% is prepared;
2)The preparation of metal electrode material:Using the anode metal material of metallic copper or metallic cobalt as carboxymethyl cellulose electro-deposition
Material, first with sand paper to carefully carrying out polishing at the out-of-flatness on the surface and edge of anode metal material up to flat smooth, then will
Anode metal material is cleaned by ultrasonic 5~15 minutes respectively in distilled water, absolute ethyl alcohol, acetone, distilled water successively, then this is positive
Pole metal material is cleaned by ultrasonic 1~3 minute in the hydrochloric acid solution of 0.5~2.0M, and it is clear to be then again dipped into ultrasound in distilled water
It washes 5~15 minutes, obtains required anode metal electrodes material, it is spare;
Using cathodic metal material of the platinized platinum as carboxymethyl cellulose electro-deposition, by platinized platinum successively in absolute ethyl alcohol, acetone, steaming
It is cleaned by ultrasonic respectively in distilled water 5~15 minutes, it is spare;
3)The electro-deposition of carboxymethyl cellulose:Take step 1)Prepared 20~30mL of carboxymethyl cellulose electrodeposit liquid, which is added in, to be held
In device, ultrasonic de-soak 3~5 minutes;Then step 2 is used)In ready anode metal electrodes material as anode, cathode gold
Belong to material as cathode, anode and cathode are immersed in simultaneously in the container equipped with carboxymethyl cellulose electrodeposit liquid, and will be positive
Pole and cathode are connected to DC power supply, and DC power supply is adjusted to constant voltage mode, and voltage is set as 0.5~1.5V, carries out carboxymethyl
The electro-deposition of cellulose, sedimentation time are 3~10 minutes;DC power supply is closed after electro-deposition, taking out surface electro-deposition has
The anode of carboxymethyl cellulose deposition layer cleans anode surface 5~15 times with distilled water, obtains being electrodeposited in anode metal electricity
The carboxymethyl cellulose deposition layer of pole material surface.
A kind of 2. electro-deposition method of carboxymethyl cellulose according to claim 1, which is characterized in that step 1)In, subtract
The vacuum degree that pressure filters is -0.03MPa~-0.08MPa.
3. the electro-deposition method of a kind of carboxymethyl cellulose according to claim 1, which is characterized in that ultrasonic power is
50-60 watts.
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