CN108586793A - A kind of preparation method of high conductivity compound hydrogel material - Google Patents

A kind of preparation method of high conductivity compound hydrogel material Download PDF

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CN108586793A
CN108586793A CN201810412212.9A CN201810412212A CN108586793A CN 108586793 A CN108586793 A CN 108586793A CN 201810412212 A CN201810412212 A CN 201810412212A CN 108586793 A CN108586793 A CN 108586793A
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hydrogel material
solution
stirred
hydrogel
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沈春霞
蒋益
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Foshan Nine Mo Science And Technology Information Consulting Co Ltd
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    • C08J2201/00—Foams characterised by the foaming process
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    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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Abstract

The present invention relates to a kind of preparation methods of high conductivity compound hydrogel material, belong to hydrogel material technical field.Technical solution of the present invention is adsorbed by rice bran-fiber and by carbon nanotube loaded to inside fibrous material, it is coated by cyclodextrin material and carries out preparing hydrogel material using sodium carboxymethylcellulose as raw material, make aniline be inhaled to bear in the hydrogel with microcosmic porous structure since hydrogel material is swollen in aniline monomer solution, through potassium peroxydisulfate modification, the aniline side group of aniline monomer and gel is graft-polymerized, to effectively improve the electric conductivity of conductive compound hydrogel material, and the present invention loads carbon nanotube by rice bran-fiber and passes through gel coating modification, since coating modification makes it form protective film in composite fiber surface, carbon nanotube particulate and air exclusion are opened, by fiber-loaded continuous performance and it is made uniformly to be filled in gel rubber material, further improve the conductive stable performance of material.

Description

A kind of preparation method of high conductivity compound hydrogel material
Technical field
The present invention relates to a kind of preparation methods of high conductivity compound hydrogel material, belong to hydrogel material technology neck Domain.
Background technology
Hydrogel is a kind of polymer possessing cross-linked network, can absorb a large amount of moisture in water and then occurs molten It is swollen, and can still keep its original structure without dissolving after swelling.And in external environmental factor such as temperature, pH Under the stimulation of value, ion, electric field, magnetic field, solvent, reactant, light or stress etc., itself property such as volume, shape, reaction speed Also the corresponding such hydrogel for generating variation is known as intelligent aqueous gel for rate, recognition performance and electric conductivity etc..Conductive hydrogel is wide It is general to be used in real life, such as drug delivery system, the purification of waste water and biobattery.And using CMC as the conductivity water of matrix The research of gel rubber material is fewer, and the step of preparing hydrogel is more complicated and toxic crosslinking is used in preparation process more Agent（Such as ECH, MBA etc.）, in conjunction with the practical application request of conductive hydrogel（Currently, rank needed for a large amount of biomaterial is KPa grade, such as the nasal cartilages of people（234kPa±27kPa）, pig thoracic aorta（43.2kPa±15kPa）, dog kidney skin Layer and medullary substance（About 10kPa）, embryo nucleus pulposus and ocular tissue（About 1kPa）Deng）.
As a kind of emerging functional material, conductive hydrogel has caused the concern of numerous scholars.By the more than ten years R and D, conductive hydrogel not only has good electric conductivity and stability, while also having considerable mechanical property concurrently, this Sample hydrogel just has prodigious actual application value.Conductive hydrogel is mainly used in electrochemical actuator, sensor, biological material Material, artificial muscle, chemical valve, conductive coating or film etc..According to the situation that hydrogel now develops, conductive hydrogel is substantially Four major class can be divided into：Polyelectrolyte conductive hydrogel, acid doping conducting hydrogel, inorganic matter add conductive hydrogel and lead The polymer-based conductive hydrogel of electricity.In recent years, conductive hydrogel is extensive by people as a member of intelligent aqueous gel family Concern, from the polyelectrolyte conductive hydrogel of starting, gradually transition is that inorganic matter addition is conductive to the research hotspot of conductive hydrogel Hydrogel and conductive polymer subbase conductive hydrogel, the machinery that this is primarily due to single polyelectrolyte conductive hydrogel are strong Degree and stability are all not fully up to expectations, so it is necessary how to prepare a kind of composite hydrogel of high conductivity stable type.
Invention content
The technical problems to be solved by the invention：For the polyelectrolyte composition of existing conductive hydrogel bill of materials one, lead The mechanical strength of conductive hydrogel and the problem that stability is all not fully up to expectations are caused, a kind of high conductivity composite hydrogel is provided The preparation method of material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）Count in parts by weight, respectively weigh 45~50 parts of absolute ethyl alcohols, 25~30 parts of ethyl orthosilicates, 45~50 parts go from Sub- water and 3~5 parts of hydrochloric acid are stirred, heating water bath, standing is cooled to room temperature to obtain hydrolyzate, in mass ratio 1:8, by boric acid Tributyl solution is added dropwise in hydrolyzate, is stirred and is stood, and modified gel liquid is obtained；
（2）In mass ratio 1:5, carbon nanotube is added in modified gel liquid, grinding distribution, obtains dispersion liquid, in parts by weight Meter weighs 45~50 parts of 0.5% hydrochloric acid solutions of mass fraction, 10~15 parts of cyclodextrin, 10~15 parts of dispersion liquids, 10~15 respectively Part rice bran-fiber and 6~8 parts of carbon nanotubes are placed in blender, are stirred to obtain mixed liquor；
（3）In mass ratio 1:8,20% glutaraldehyde solution of mass fraction is added dropwise in mixed liquor, after being added dropwise to complete, adjusts pH To 7.5, be stirred and stand and be cooled to room temperature filtering and collect filter cake, washing it is dry modified covered fiber；
（4）It counts in parts by weight, weighs 45~50 parts of sodium carboxymethylcelluloses, 3~5 parts of 1% sodium hydroxides of mass fraction respectively Solution, 3~5 parts of propylene glycol diglycidyl ethers and 10~15 parts of modified covered fibers are placed in blender, are stirred and are crosslinked Processing, standing are cooled to room temperature, and must stand gel and in mass ratio 1:10, it will stand in soak to aniline solution, then It is impregnated in potassium persulfate solution, collects to obtain cross-linking modified hydrogel and vacuum freeze drying, you can be prepared into a kind of high conductivity Compound hydrogel material.
Step（1）The butyl borate solution drop rate is 2~3mL/min.
Step（3）The glutaraldehyde solution time for adding is 10~15min.
Step（3）The adjusting pH is using 0.5mol/L sodium hydroxide solutions.
Compared with other methods, advantageous effects are the present invention：
（1）Technical solution of the present invention is adsorbed by rice bran-fiber and by carbon nanotube loaded to inside fibrous material, is pasted by ring Smart material is coated and is carried out preparing hydrogel material using sodium carboxymethylcellulose as raw material, since hydrogel material is in aniline monomer Being swollen in solution, which makes aniline be inhaled, bears in the hydrogel with microcosmic porous structure, through potassium peroxydisulfate modification, aniline list The aniline side group of body and gel is graft-polymerized, to effectively improve the electric conductivity of conductive compound hydrogel material；
（2）Technical solution of the present invention is by rice bran-fiber load carbon nanotube and by gel coating modification, due to coating modification So that it is formed protective film in composite fiber surface, carbon nanotube particulate and air exclusion is opened, to improve carbon nanotube particulate Antioxygenic property have no effect on the electric conductivity of copper powder simultaneously, by fiber-loaded continuous performance and make it in gel rubber material Uniformly filling further improves the conductive stable performance of material.
Specific implementation mode
Count in parts by weight, respectively weigh 45~50 parts of absolute ethyl alcohols, 25~30 parts of ethyl orthosilicates, 45~50 parts go from Sub- water and 3~5 parts of 5% hydrochloric acid of mass fraction are placed in beaker, be stirred be placed in heating water bath 15 at 45~55 DEG C~ 20min, standing are cooled to room temperature to obtain hydrolyzate, in mass ratio 1:8,1% butyl borate solution of mass fraction is added dropwise to water It solves in liquid, control butyl borate solution drop rate is 2~3mL/min, is stirred and stands 6~8h, obtain modified gel Liquid；In mass ratio 1:5, carbon nanotube is added in modified gel liquid, 2~3h of grinding distribution obtains dispersion liquid, in parts by weight Meter weighs 45~50 parts of 0.5% hydrochloric acid solutions of mass fraction, 10~15 parts of cyclodextrin, 10~15 parts of dispersion liquids, 10~15 respectively Part rice bran-fiber and 6~8 parts of carbon nanotubes are placed in blender, are stirred to obtain mixed liquor, in mass ratio 1:8, by quality point Several 20% glutaraldehyde solutions are added dropwise in mixed liquor, and control time for adding is 10~15min, after being added dropwise to complete, then is used 0.5mol/L sodium hydroxide solutions adjust pH to 7.5, are stirred and stand and are cooled to room temperature filtering and collect filter cake and with third Ketone rinses 3~5 times, and vacuum freeze drying must be modified covered fiber；It counts in parts by weight, weighs 45~50 parts of carboxymethyl fibres respectively The plain sodium of dimension, 3~5 parts of 1% sodium hydroxide solutions of mass fraction, 3~5 parts of propylene glycol diglycidyl ethers and 10~15 parts of modified claddings Fiber is placed in blender, is stirred and is placed in crosslinking Treatment 20 at 35~45 DEG C~for 24 hours, standing is cooled to room temperature, and is obtained quiet Set gel and in mass ratio 1:10, will stand 20 in soak to 1% aniline solution of mass fraction~for 24 hours, then in quality point Impregnate 20 in several 1% potassium persulfate solutions~for 24 hours, it collects to obtain cross-linking modified hydrogel and vacuum freeze drying, you can be prepared into A kind of high conductivity compound hydrogel material.
It counts in parts by weight, weighs 45 parts of absolute ethyl alcohols, 25 parts of ethyl orthosilicates, 45 parts of deionized waters and 3 parts of matter respectively Amount 5% hydrochloric acid of score is placed in beaker, is stirred and is placed in heating water bath 15min at 45 DEG C, and standing is cooled to room temperature to obtain water Solution liquid, in mass ratio 1:8,1% butyl borate solution of mass fraction is added dropwise in hydrolyzate, butyl borate solution is controlled Drop rate is 2mL/min, is stirred and stands 6h, obtains modified gel liquid；In mass ratio 1:5, carbon nanotube is added to In modified gel liquid, grinding distribution 2h obtains dispersion liquid, counts in parts by weight, and it is molten to weigh 45 parts of 0.5% hydrochloric acid of mass fraction respectively Liquid, 10 parts of cyclodextrin, 10 parts of dispersion liquids, 10 parts of rice bran-fibers and 6~8 parts of carbon nanotubes are placed in blender, are stirred Mixed liquor, in mass ratio 1:8,20% glutaraldehyde solution of mass fraction is added dropwise in mixed liquor, control time for adding is 10min adjusts pH to 7.5 after being added dropwise to complete, then with 0.5mol/L sodium hydroxide solutions, is stirred and stands and be cooled to room Temperature filters and collects filter cake and with acetone rinsing 3 times, and vacuum freeze drying must be modified covered fiber；It counts in parts by weight, respectively 45 parts of sodium carboxymethylcelluloses of weighing, 3 parts of 1% sodium hydroxide solutions of mass fraction, 3 parts of propylene glycol diglycidyl ethers and 10 parts change Property covered fiber is placed in blender, is stirred and is placed in crosslinking Treatment 20 at 35 DEG C~for 24 hours, standing is cooled to room temperature, and is obtained Stand gel and in mass ratio 1:10,20h in soak to 1% aniline solution of mass fraction will be stood, then in mass fraction 20h is impregnated in 1% potassium persulfate solution, collects to obtain cross-linking modified hydrogel and vacuum freeze drying, you can be prepared into a kind of high Electric conductivity compound hydrogel material.
It counts in parts by weight, weighs 47 parts of absolute ethyl alcohols, 28 parts of ethyl orthosilicates, 47 parts of deionized waters and 4 parts of matter respectively Amount 5% hydrochloric acid of score is placed in beaker, is stirred and is placed in heating water bath 17min at 50 DEG C, and standing is cooled to room temperature to obtain water Solution liquid, in mass ratio 1:8,1% butyl borate solution of mass fraction is added dropwise in hydrolyzate, butyl borate solution is controlled Drop rate is 2mL/min, is stirred and stands 7h, obtains modified gel liquid；In mass ratio 1:5, carbon nanotube is added to In modified gel liquid, grinding distribution 2h obtains dispersion liquid, counts in parts by weight, and it is molten to weigh 47 parts of 0.5% hydrochloric acid of mass fraction respectively Liquid, 12 parts of cyclodextrin, 12 parts of dispersion liquids, 12 parts of rice bran-fibers and 7 parts of carbon nanotubes are placed in blender, are stirred to obtain mixing Liquid, in mass ratio 1:8,20% glutaraldehyde solution of mass fraction is added dropwise in mixed liquor, control time for adding is 12min, is waited for After being added dropwise to complete, then with 0.5mol/L sodium hydroxide solutions adjust pH to 7.5, be stirred and stand be cooled to room temperature filtering simultaneously It collects filter cake and with acetone rinsing 4 times, vacuum freeze drying must be modified covered fiber；It counts in parts by weight, weighs 47 parts respectively The modified cladding of sodium carboxymethylcellulose, 4 parts of 1% sodium hydroxide solutions of mass fraction, 4 parts of propylene glycol diglycidyl ethers and 12 parts is fine Dimension is placed in blender, is stirred and is placed in crosslinking Treatment 22h, standing at 40 DEG C and is cooled to room temperature, must stand gel and by Mass ratio 1:10,22h in soak to 1% aniline solution of mass fraction will be stood, then molten in 1% potassium peroxydisulfate of mass fraction 22h is impregnated in liquid, collects to obtain cross-linking modified hydrogel and vacuum freeze drying, you can be prepared into a kind of high conductivity compound water congealing Glue material.
It counts in parts by weight, weighs 50 parts of absolute ethyl alcohols, 30 parts of ethyl orthosilicates, 50 parts of deionized waters and 5 parts of matter respectively Amount 5% hydrochloric acid of score is placed in beaker, is stirred and is placed in heating water bath 20min at 55 DEG C, and standing is cooled to room temperature to obtain water Solution liquid, in mass ratio 1:8,1% butyl borate solution of mass fraction is added dropwise in hydrolyzate, butyl borate solution is controlled Drop rate is 3mL/min, is stirred and stands 8h, obtains modified gel liquid；In mass ratio 1:5, carbon nanotube is added to In modified gel liquid, grinding distribution 3h obtains dispersion liquid, counts in parts by weight, and it is molten to weigh 50 parts of 0.5% hydrochloric acid of mass fraction respectively Liquid, 15 parts of cyclodextrin, 15 parts of dispersion liquids, 15 parts of rice bran-fibers and 8 parts of carbon nanotubes are placed in blender, are stirred to obtain mixing Liquid, in mass ratio 1:8,20% glutaraldehyde solution of mass fraction is added dropwise in mixed liquor, control time for adding is 15min, is waited for After being added dropwise to complete, then with 0.5mol/L sodium hydroxide solutions adjust pH to 7.5, be stirred and stand be cooled to room temperature filtering simultaneously It collects filter cake and with acetone rinsing 5 times, vacuum freeze drying must be modified covered fiber；It counts in parts by weight, weighs 50 parts respectively The modified cladding of sodium carboxymethylcellulose, 5 parts of 1% sodium hydroxide solutions of mass fraction, 5 parts of propylene glycol diglycidyl ethers and 15 parts is fine Dimension is placed in blender, is stirred and is placed in crosslinking Treatment at 45 DEG C for 24 hours, standing is cooled to room temperature, must stand gel and by Mass ratio 1:10, it will stand in soak to 1% aniline solution of mass fraction for 24 hours, then molten in 1% potassium peroxydisulfate of mass fraction It is impregnated in liquid for 24 hours, collects to obtain cross-linking modified hydrogel and vacuum freeze drying, you can be prepared into a kind of high conductivity compound water congealing Glue material.
Example 1,2,3 prepared by the present invention is tested for the property, specific test result is as follows shown in table table 1：
1 performance test table of table
As seen from the above table, the hydrogel material that prepared by the present invention has excellent mechanical property and electric conductivity.

Claims (4)

1. a kind of preparation method of high conductivity compound hydrogel material, it is characterised in that specific targets step is：
（1）Count in parts by weight, respectively weigh 45~50 parts of absolute ethyl alcohols, 25~30 parts of ethyl orthosilicates, 45~50 parts go from Sub- water and 3~5 parts of hydrochloric acid are stirred, heating water bath, standing is cooled to room temperature to obtain hydrolyzate, in mass ratio 1:8, by boric acid Tributyl solution is added dropwise in hydrolyzate, is stirred and is stood, and modified gel liquid is obtained；
（2）In mass ratio 1:5, carbon nanotube is added in modified gel liquid, grinding distribution, obtains dispersion liquid, in parts by weight Meter weighs 45~50 parts of 0.5% hydrochloric acid solutions of mass fraction, 10~15 parts of cyclodextrin, 10~15 parts of dispersion liquids, 10~15 respectively Part rice bran-fiber and 6~8 parts of carbon nanotubes are placed in blender, are stirred to obtain mixed liquor；
（3）In mass ratio 1:8,20% glutaraldehyde solution of mass fraction is added dropwise in mixed liquor, after being added dropwise to complete, adjusts pH To 7.5, be stirred and stand and be cooled to room temperature filtering and collect filter cake, washing it is dry modified covered fiber；
（4）It counts in parts by weight, weighs 45~50 parts of sodium carboxymethylcelluloses, 3~5 parts of 1% sodium hydroxides of mass fraction respectively Solution, 3~5 parts of propylene glycol diglycidyl ethers and 10~15 parts of modified covered fibers are placed in blender, are stirred and are crosslinked Processing, standing are cooled to room temperature, and must stand gel and in mass ratio 1:10, it will stand in soak to aniline solution, then It is impregnated in potassium persulfate solution, collects to obtain cross-linking modified hydrogel and vacuum freeze drying, you can be prepared into a kind of high conductivity Compound hydrogel material.
2. a kind of preparation method of high conductivity compound hydrogel material according to claim 1, it is characterised in that：Step （1）The butyl borate solution drop rate is 2~3mL/min.
3. a kind of preparation method of high conductivity compound hydrogel material according to claim 1, it is characterised in that：Step （3）The glutaraldehyde solution time for adding is 10~15min.
4. a kind of preparation method of high conductivity compound hydrogel material according to claim 1, it is characterised in that：Step （3）The adjusting pH is using 0.5mol/L sodium hydroxide solutions.
CN201810412212.9A 2018-05-03 2018-05-03 A kind of preparation method of high conductivity compound hydrogel material Withdrawn CN108586793A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114605669A (en) * 2022-03-24 2022-06-10 苏州乐泰医疗科技有限公司 Preparation method of conductive hydrogel

Citations (6)

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