CN111057186B - Photo-curing cross-linking conductive hydrogel and preparation method and application thereof - Google Patents
Photo-curing cross-linking conductive hydrogel and preparation method and application thereof Download PDFInfo
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 77
- 238000004132 cross linking Methods 0.000 title claims abstract description 57
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000178 monomer Substances 0.000 claims abstract description 26
- 239000002562 thickening agent Substances 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 14
- 239000003906 humectant Substances 0.000 claims abstract description 14
- 239000006258 conductive agent Substances 0.000 claims abstract description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 162
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 40
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 36
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 36
- 239000000853 adhesive Substances 0.000 claims description 31
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 24
- IPGANOYOHAODGA-UHFFFAOYSA-N dilithium;dimagnesium;dioxido(oxo)silane Chemical group [Li+].[Li+].[Mg+2].[Mg+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O IPGANOYOHAODGA-UHFFFAOYSA-N 0.000 claims description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
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- 238000000034 method Methods 0.000 claims description 7
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- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 3
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- XFHJDMUEHUHAJW-UHFFFAOYSA-N n-tert-butylprop-2-enamide Chemical compound CC(C)(C)NC(=O)C=C XFHJDMUEHUHAJW-UHFFFAOYSA-N 0.000 claims description 3
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- CCTFAOUOYLVUFG-UHFFFAOYSA-N 2-(1-amino-1-imino-2-methylpropan-2-yl)azo-2-methylpropanimidamide Chemical compound NC(=N)C(C)(C)N=NC(C)(C)C(N)=N CCTFAOUOYLVUFG-UHFFFAOYSA-N 0.000 claims description 2
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/24—Detecting, measuring or recording bioelectric or biomagnetic signals of the body or parts thereof
- A61B5/25—Bioelectric electrodes therefor
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
Abstract
The invention discloses a photo-curing cross-linking conductive hydrogel and a preparation method and application thereof. The photo-curing cross-linking conductive hydrogel is prepared from the following components in parts by mass: 12-40 parts of a monomer, 3-9 parts of a neutralizer, 0.07-0.3 part of a cross-linking agent, 20-65 parts of a humectant, 4-10 parts of a conductive agent, 0.3-5 parts of a thickening agent, 0.2-1.2 parts of a photoinitiator and 20-70 parts of water; wherein the monomer is acrylamide monomer. The invention also discloses a preparation method of the photo-curing crosslinking conductive hydrogel and application of the photo-curing crosslinking conductive hydrogel in preparing an electrocardio-electrode patch. The photo-curing crosslinking conductive hydrogel has the characteristics of strong conductivity, good biocompatibility and the like. The disposable electrocardio-electrode paster prepared by the gel can keep good contact with skin for a long time without drying, has no stimulation to the skin, and obtains stable electrocardiosignal potential, clear waveform and convenient operation.
Description
Technical Field
The invention relates to the technical field of conductive gels, in particular to a photo-curing cross-linking conductive hydrogel and a preparation method and application thereof.
Background
The disposable electrocardio-electrode patch is mainly matched with equipment such as an electrocardiograph, a monitor and the like for use. The main application is receiving human electrocardio information, detecting heart rate and pulse, etc. The main component of the disposable electrocardio-electrode patch is medical biological conductive gel. The gel material is formed by polymerizing one or more high molecular monomers according to a certain proportion. The surface of the gel is instantly adhered to the skin of a human body, and then the gel is combined with special medical equipment to transmit electrocardiosignals of the human body.
The medical biological conductive adhesive needs to have excellent conductivity, and after a human body is contacted, adverse reactions such as stimulation and allergy cannot be generated. At present, a polymerization system is adopted for the conductive adhesive applied to clinic, and the monomers are easy to react incompletely during batch production, so that irritation symptoms such as skin red swelling, pruritus and the like are caused; most of the electrical properties are not ideal, the electrode has much interference and high noise, and the monitoring effect and the accurate judgment of diseases are influenced.
Disclosure of Invention
In order to solve the technical problems encountered by the existing conductive adhesive and overcome the defects of the existing disposable electrocardio-electrode patch product, the invention aims to provide a photocuring crosslinking conductive hydrogel, the invention aims to provide a preparation method of the photocuring crosslinking conductive hydrogel, and the invention aims to provide the application of the photocuring crosslinking conductive hydrogel.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a photo-curing cross-linking conductive hydrogel.
A photo-curing cross-linking conductive hydrogel is prepared from the following components in parts by mass: 12-40 parts of a monomer, 3-9 parts of a neutralizer, 0.07-0.3 part of a cross-linking agent, 20-65 parts of a humectant, 4-10 parts of a conductive agent, 0.3-5 parts of a thickening agent, 0.2-1.2 parts of a photoinitiator and 20-70 parts of water; wherein the monomer is acrylamide monomer.
Preferably, the photo-curing cross-linking conductive hydrogel comprises the following components in parts by mass: 15-30 parts of monomer, 4.5-6 parts of neutralizing agent, 0.15-0.3 part of cross-linking agent, 30-60 parts of humectant, 5-6 parts of conductive agent, 0.5-1 part of thickening agent, 0.5-1 part of photoinitiator and 50-60 parts of water.
Preferably, in the photo-curing cross-linking conductive hydrogel, the acrylamide monomer is at least one selected from acrylamide, methacrylamide, N-dimethylacrylamide, N-diethylacrylamide, N-tert-butylacrylamide, N-methylolacrylamide and N- (2-hydroxyethyl) acrylamide; further preferably, the acrylamide monomer is at least one selected from the group consisting of N, N-dimethylacrylamide, N-t-butylacrylamide, N-methylolacrylamide, and N- (2-hydroxyethyl) acrylamide; still more preferably, the acrylamide monomer is at least one selected from the group consisting of N, N-dimethylacrylamide and N-methylolacrylamide.
Preferably, in the photo-curing cross-linking conductive hydrogel, the neutralizing agent is at least one selected from sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium bicarbonate, triethanolamine, diethanolamine, triethanolamine and triethylamine; further preferably, the neutralizing agent is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, and ammonium bicarbonate; still more preferably, the neutralizing agent is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium carbonate, and potassium carbonate.
Preferably, in the photo-curing cross-linking conductive hydrogel, the conductive agent is at least one selected from sodium chloride, potassium chloride, ammonium chloride, sodium sulfate and potassium sulfate; further preferably, the conductive agent is at least one selected from the group consisting of sodium chloride and potassium chloride.
The preferable neutralizing agent and the conductive agent adopted by the invention are common raw materials, and have wide sources, extremely low cost and convenient use. The selected neutralizing agents or conductive agents may be used in combination or alone.
Preferably, in the photo-curing cross-linking conductive hydrogel, the cross-linking agent is at least one selected from N, N ' -vinyl bisacrylamide, N ' - (1, 2-dihydroxyethylene) bisacrylamide and N, N ' -methylene bisacrylamide; more preferably, the crosslinking agent is at least one selected from the group consisting of N, N '- (1, 2-dihydroxyethylene) bisacrylamide and N, N' -methylenebisacrylamide.
Preferably, in the photo-curing cross-linking conductive hydrogel, the humectant is at least one selected from glycerol, propylene glycol and polyethylene glycol; further preferably, the humectant is at least one selected from glycerol and propylene glycol; most preferably, the humectant is glycerin. The humectant can improve the stability of the system in air, greatly prolong the preservation time of gel exposed in air, and eliminate adverse reactions such as skin irritation and sensitization.
Preferably, in the photo-curing crosslinking conductive hydrogel, the thickening agent is lithium magnesium silicate. Because the lithium magnesium silicate has high specific surface area and excellent water solubility, the dispersion degree of a system can be increased, the reaction uniformity is increased, and the self conductivity and the mechanical property of the gel are improved.
Preferably, in the photo-curable crosslinked conductive hydrogel, the photoinitiator is at least one selected from the group consisting of α -hydroxyketone, 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone, 1-hydroxycyclohexyl phenyl ketone, acylphosphine oxide photoinitiator, and 2, 2' -azo-bis (2-amidinopropane) photoinitiator; further preferably, the photoinitiator is at least one selected from the group consisting of 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone (photoinitiator 2959) and 1-hydroxycyclohexyl phenyl ketone (photoinitiator 184). The products of the preferred light curing agents after light curing decomposition have good biocompatibility and no toxic or side effect on human bodies.
The invention provides a preparation method of the photocuring crosslinking conductive hydrogel.
The preparation method of the photo-curing cross-linking conductive hydrogel comprises the following steps:
1) respectively dissolving a monomer, a cross-linking agent, a neutralizing agent and a thickening agent in water to respectively obtain solutions A, B, C and D;
2) adding the solution C into the solution A, mixing, standing and defoaming to obtain a solution E;
3) adding water into the solution E for dilution, and mixing with a conductive agent to obtain a solution F;
4) mixing the solution B, the solution D, the solution F and a humectant to obtain a solution G;
5) adding a photoinitiator into the solution G under a dark condition, and mixing to obtain a conductive adhesive solution;
6) and curing the conductive adhesive solution under ultraviolet light to obtain the photocuring crosslinking conductive hydrogel.
Preferably, in the preparation method of the photo-curing crosslinking conductive hydrogel, in the step 1), the mass concentration of the monomer of the solution A is 30-60%; more preferably, the mass concentration of the monomer in the solution A is 33% to 50%.
Preferably, in the preparation method of the photo-curing crosslinking conductive hydrogel, in the step 1), the mass concentration of the crosslinking agent in the solution B is 10-20%; more preferably, the mass concentration of the crosslinking agent in the solution B is 13 to 17%.
In the step 1) of the preparation method of the photocuring crosslinking conductive hydrogel, the optimal concentration of the monomer and the crosslinking agent can ensure that solid substances are uniformly dispersed and dissolved, the uniformity of a system is improved, the balance of polymerization rate is ensured, and the polymerization reaction can be smoothly carried out.
Preferably, in the preparation method of the photo-curing crosslinking conductive hydrogel, in the step 1), the mass concentration of the neutralizer of the solution C is 10-40%; more preferably, the mass concentration of the neutralizing agent in the solution C is 17 to 35%.
Preferably, in step 1) of the preparation method of the photo-curing crosslinking conductive hydrogel, the obtained solution C is stood and cooled to room temperature.
Preferably, in the preparation method of the photo-curing crosslinking conductive hydrogel, in the step 1), the mass concentration of the thickener of the solution D is 5-20%; more preferably, the mass concentration of the thickener in the solution D is 9% to 17%. By controlling the concentration of the thickener, the thickener can be dispersed in the aqueous solution more quickly, and the aqueous phase system is beneficial to the uniformity of the subsequent solution mixing.
Preferably, in the step 2) of the preparation method of the photo-curing cross-linking conductive hydrogel, the final pH range of the solution E is 5-9.
Preferably, in the step 2) of the preparation method of the photo-curing cross-linking conductive hydrogel, after the neutralizer solution C is cooled to room temperature, the solution C is slowly added into the solution A, stirring and mixing are carried out, standing is carried out for defoaming, and the final pH value of the solution needs to be controlled to be 5-9. The step can release heat released by the dissolution of the neutralizing agent, has mild conditions when neutralizing with the monomer, does not need additional control, and avoids the advance polymerization of the monomer caused by overhigh temperature. The pH value of the solution after the neutralization reaction is biased to be neutral, so that the stimulation and the damage to the human body are avoided.
In the step 3) of the preparation method of the photo-curing crosslinking conductive hydrogel, the amount of the added water is calculated according to the formula amount, and the water is the rest except the total amount of the water used in the step 1).
Preferably, in the steps 1) to 5) of the preparation method of the photo-curing crosslinked conductive hydrogel, the dissolving or mixing is carried out under uniform stirring in the same direction, and the stirring speed is 300r/min to 500 r/min.
Preferably, in step 5) of the preparation method of the photo-curing cross-linking conductive hydrogel, the conductive gel solution needs to be stored at 4 ℃ in a dark place. This prevents premature polymerization of the monomers under the influence of ultraviolet rays in natural light.
Preferably, in step 6) of the preparation method of the photo-curing cross-linking conductive hydrogel, the wavelength of the ultraviolet light is 250nm to 420 nm.
Preferably, in step 6) of the preparation method of the photo-curing cross-linking conductive hydrogel, the curing time is 5 seconds to 60 seconds; more preferably, the curing time is 5 seconds to 20 seconds.
In the preparation method of the conductive hydrogel, the monomer, the cross-linking agent, the neutralizer and the thickening agent need to be prepared into a solution in advance and then mixed. The method can control the reaction process of the neutralizer in the reaction with the monomer, and avoid the generation of a large amount of gas at the over-speed of the reaction. In the batch industrial production, all component solutions are prepared in advance, so that reactants can be rapidly and uniformly mixed in a short time, and the industrial production requirements can be met.
The invention provides application of the photo-curing cross-linking conductive hydrogel.
The application of the photo-curing cross-linking conductive hydrogel in preparing an electrode patch.
Preferably, in application, the light-cured crosslinked conductive hydrogel, the non-woven fabric and the electrode buckle form an electrode patch.
Preferably, in application, the electrode patch is an electrocardio-electrode patch; further preferably, the electrode patch is a disposable electrocardio-electrode patch.
The invention has the beneficial effects that:
the photo-curing crosslinking conductive hydrogel provided by the invention has the characteristics of strong conductivity, good biocompatibility and the like. The disposable electrocardio-electrode paster prepared by the gel can keep good contact with skin for a long time without drying, has no stimulation to the skin, and obtains stable electrocardiosignal potential, clear waveform and convenient operation.
Specifically, compared with the prior art, the invention has the following advantages:
the invention takes acrylamide homologues as a main body, dissolves a monomer, a neutralizer, a cross-linking agent, a humectant, a conductive agent and a thickening agent in water to prepare an aqueous solution, uniformly disperses a photoinitiator in the solution, prepares a conductive adhesive solution through reasonable proportion, and cures the conductive adhesive solution into a conductive gel product under the illumination of 250-420 nm. The reaction system is clear, the conditions are mild, no waste liquid is discharged in the production process, and the method is simple and environment-friendly. The prepared mixing process is clear and rapid. The conductive gel does not contain acrylic substances, and no monomer is left after mass production.
The conductive gel prepared by the invention has the characteristics of strong conductivity, good biocompatibility and the like. The disposable electrocardio-electrode paster prepared by the gel can keep good contact with skin for a long time without drying, has no stimulation to the skin, and obtains stable electrocardiosignal potential, clear waveform and convenient operation.
Drawings
FIG. 1 is a comparison of ECG monitoring signals of the electrode of the present invention and an inlet electrode.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or apparatus used in the examples and comparative examples were obtained from conventional commercial sources unless otherwise specified. Unless otherwise indicated, the testing or testing methods are conventional in the art.
Example 1
The composition of the photo-curable crosslinked conductive hydrogel of this example is shown in Table 1.
Table 1 example 1 composition of photo-cured crosslinked conductive hydrogel
| Components | Mass portion of |
| N-methylolacrylamide | 20 portions of |
| Anhydrous potassium carbonate | 4 portions of |
| Potassium hydroxide | 0.5 portion |
| N, N' -methylenebisacrylamide | 0.2 part |
| Glycerol | 40 portions of |
| Potassium chloride | 6 portions of |
| Lithium magnesium silicate | 1 part of |
| 1- [4- (2-Hydroxyethoxy) -phenyl]-2-hydroxy-2-methyl-propanone | 0.5 portion |
| Water (W) | 50 portions of |
The preparation method of the photo-curing cross-linking conductive hydrogel comprises the following steps:
s1: weighing 20g N-hydroxymethyl acrylamide, dissolving in 20g of water, and stirring to dissolve completely to obtain a solution A;
s2: weighing 0.2g N, N' -methylene bisacrylamide, dissolving in 1g of water, and stirring until the mixture is completely dissolved to obtain a solution B;
s3: weighing 4g of potassium carbonate and 0.5g of potassium hydroxide, dissolving in 10g of water, stirring until the potassium carbonate and the potassium hydroxide are completely dissolved, and standing the solution to room temperature to obtain a solution C;
s4: weighing 1g of lithium magnesium silicate, dissolving the lithium magnesium silicate in 5g of water, and stirring until the lithium magnesium silicate is completely dissolved to obtain a solution D;
s5: slowly pouring the solution C into the solution A, fully stirring, and defoaming to obtain a solution E;
s6: weighing 14g of water, adding the solution E and stirring uniformly; weighing 6g of potassium chloride, slowly adding the potassium chloride into the solution, and stirring until the potassium chloride is completely dissolved to obtain a solution F;
s7: mixing the solution B, the solution D and the solution F, then fully stirring, weighing 40G of glycerol, adding into the solution, and fully stirring until the solution is uniform to obtain a solution G;
s8: weighing 0.5G of 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone, adding the solution G under the condition of keeping out of the sun, and stirring until the solution G is completely dissolved to obtain a conductive adhesive solution;
s9: and under the ultraviolet illumination condition with the wavelength of 250-420nm, crosslinking for 20 seconds to obtain the conductive adhesive.
Example 2
The composition of the photo-curable crosslinked conductive hydrogel of this example is shown in Table 2.
Table 2 example 2 composition of photo-cured crosslinked conductive hydrogel
| Components | Mass portion of |
| N, N-dimethylacrylamide | 15 portions of |
| Anhydrous sodium carbonate | 6 portions of |
| N, N' -methylenebisacrylamide | 0.3 part |
| Glycerol | 30 portions of |
| Sodium chloride | 5 portions of |
| Lithium magnesium silicate | 1 part of |
| 1-hydroxycyclohexyl phenyl methanones | 0.3 part |
| 1- [4- (2-Hydroxyethoxy) -phenyl]-2-hydroxy-2-methyl-propanone | 0.2 part |
| Water (W) | 60 portions of |
The preparation method of the photo-curing cross-linking conductive hydrogel comprises the following steps:
s1: weighing 15g N, N-dimethylacrylamide, dissolving in 30g of water, and stirring until the solution is completely dissolved to obtain a solution A;
s2: weighing 0.3g N, N' -methylene bisacrylamide, dissolving in 2g of water, and stirring until the mixture is completely dissolved to obtain a solution B;
s3: weighing 6g of anhydrous sodium carbonate, dissolving the anhydrous sodium carbonate in 10g of water, stirring until the anhydrous sodium carbonate is completely dissolved, and standing the solution to room temperature to obtain a solution C;
s4: weighing 1g of lithium magnesium silicate, dissolving the lithium magnesium silicate in 5g of water, and stirring until the lithium magnesium silicate is completely dissolved to obtain a solution D;
s5: slowly pouring the solution C into the solution A, fully stirring, and defoaming to obtain a solution E;
s6: weighing 13g of water, adding the solution E and stirring uniformly; weighing 5g of sodium chloride, slowly adding the sodium chloride into the solution, and stirring until the sodium chloride is completely dissolved to obtain a solution F;
s7: mixing the solution B, the solution D and the solution F, then fully stirring, weighing 30G of glycerol, adding into the solution, and fully stirring until the solution is uniform to obtain a solution G;
s8: weighing 0.3G of 1-hydroxycyclohexyl phenyl ketone and 0.2G of 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone, adding the solution G under the condition of keeping out of the sun, and stirring until the solution G is completely dissolved to obtain a conductive adhesive solution;
s9: and under the ultraviolet illumination condition with the wavelength of 250-420nm, crosslinking for 5 seconds to obtain the conductive adhesive.
Example 3
The composition of the photo-curable crosslinked conductive hydrogel of this example is shown in Table 3.
Table 3 example 3 composition of photo-cured crosslinked conductive hydrogel
The preparation method of the photo-curing cross-linking conductive hydrogel comprises the following steps:
s1: weighing 30g N-hydroxymethyl acrylamide, dissolving in 30g of water, and stirring to dissolve completely to obtain a solution A;
s2: weighing 0.15g N, N' - (1, 2-dihydroxyethylene) bisacrylamide, dissolving in 1g of water, and stirring until the solution is completely dissolved to obtain a solution B;
s3: weighing 4g of sodium hydroxide and 1g of anhydrous sodium carbonate, dissolving in 10g of water, stirring until the sodium hydroxide and the anhydrous sodium carbonate are completely dissolved, and standing the solution to room temperature to obtain a solution C;
s4: weighing 0.5g of lithium magnesium silicate, dissolving the lithium magnesium silicate in 5g of water, and stirring until the lithium magnesium silicate is completely dissolved to obtain a solution D;
s5: slowly pouring the solution C into the solution A, fully stirring, and defoaming to obtain a solution E;
s6: weighing 4g of water, adding the solution E and stirring uniformly; weighing 6g of sodium chloride, slowly adding the sodium chloride into the solution, and stirring until the sodium chloride is completely dissolved to obtain a solution F;
s7: mixing the solution B, the solution D and the solution F, then fully stirring, weighing 60G of glycerol, adding into the solution, and fully stirring until the solution is uniform to obtain a solution G;
s8: weighing 1G of 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone, adding the solution G under the condition of keeping out of the sun, and stirring until the solution G is completely dissolved to obtain a conductive adhesive solution;
s9: and under the ultraviolet illumination condition with the wavelength of 250-420nm, crosslinking for 10 seconds to obtain the conductive adhesive.
Comparative example 1
The composition of the photo-curable crosslinked conductive hydrogel of this example is shown in Table 4.
Table 4 composition of comparative example 1 photo-cured crosslinked conductive hydrogel
The preparation method of the photo-curing cross-linking conductive hydrogel comprises the following steps:
s1: weighing 20g N-hydroxymethyl acrylamide, dissolving in 20g of water, and stirring to dissolve completely to obtain a solution A;
s2: weighing 0.2g N, N' -methylene bisacrylamide, dissolving in 1g of water, and stirring until the mixture is completely dissolved to obtain a solution B;
s3: weighing 4g of potassium carbonate and 0.5g of potassium hydroxide, dissolving in 10g of water, stirring until the potassium carbonate and the potassium hydroxide are completely dissolved, and standing the solution to room temperature to obtain a solution C;
s4: weighing 1g of lithium magnesium silicate, dissolving the lithium magnesium silicate in 5g of water, and stirring until the lithium magnesium silicate is completely dissolved to obtain a solution D;
s5: slowly pouring the solution C into the solution A, fully stirring, and defoaming to obtain a solution E;
s6: weighing 54g of water, adding the solution E and stirring uniformly; weighing 6g of potassium chloride, slowly adding the potassium chloride into the solution, and stirring until the potassium chloride is completely dissolved to obtain a solution F;
s7: mixing the solution B, the solution D and the solution F, and then fully stirring until the solution is uniform to obtain a solution G;
s8: weighing 0.5G of 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone, adding the solution G under the condition of keeping out of the sun, and stirring until the solution G is completely dissolved to obtain a conductive adhesive solution;
s9: and under the ultraviolet illumination condition with the wavelength of 250-420nm, crosslinking for 20 seconds to obtain the conductive adhesive.
Comparative example 2
The composition of the photo-curable crosslinked conductive hydrogel of this example is shown in Table 5.
TABLE 5 composition of photo-cured crosslinked conductive hydrogel of comparative example 2
| Components | Mass portion of |
| N-methylolacrylamide | 20 portions of |
| Anhydrous potassium carbonate | 4 portions of |
| Potassium hydroxide | 0.5 portion |
| N, N' -methylenebisacrylamide | 0.2 part |
| Glycerol | 40 portions of |
| Potassium chloride | 6 portions of |
| 1- [4- (2-Hydroxyethoxy) -phenyl]-2-hydroxy-2-methyl-propanone | 0.5 portion |
| Water (W) | 50 portions of |
The preparation method of the photo-curing cross-linking conductive hydrogel comprises the following steps:
s1: weighing 20g N-hydroxymethyl acrylamide, dissolving in 20g of water, and stirring to dissolve completely to obtain a solution A;
s2: weighing 0.2g N, N' -methylene bisacrylamide, dissolving in 1g of water, and stirring until the mixture is completely dissolved to obtain a solution B;
s3: weighing 4g of potassium carbonate and 0.5g of potassium hydroxide, dissolving in 10g of water, stirring until the potassium carbonate and the potassium hydroxide are completely dissolved, and standing the solution to room temperature to obtain a solution C;
s4: slowly pouring the solution C into the solution A, fully stirring, and defoaming to obtain a solution D;
s5: weighing 14g of water, adding the solution D and stirring uniformly; weighing 6g of potassium chloride, slowly adding the potassium chloride into the solution, and stirring until the potassium chloride is completely dissolved to obtain a solution E;
s6: mixing the solution B and the solution E, fully stirring, weighing 40g of glycerol, adding into the solution, and fully stirring until the solution is uniform to obtain a solution F;
s7: weighing 0.5g of 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone, adding the solution F under the condition of keeping out of the sun, and stirring until the solution F is completely dissolved to obtain a conductive adhesive solution;
s8: and under the ultraviolet illumination condition with the wavelength of 250-420nm, crosslinking for 30 seconds to obtain the conductive adhesive.
Comparative example 3
The composition of the photo-curable crosslinked conductive hydrogel of this example is shown in Table 6.
TABLE 6 COMPARATIVE EXAMPLE 3 composition of photo-cured crosslinked conductive hydrogel
| Components | Mass portion of |
| N-methylolacrylamide | 20 portions of |
| N, N' -methylenebisacrylamide | 0.2 part |
| Glycerol | 40 portions of |
| Potassium chloride | 6 portions of |
| Lithium magnesium silicate | 1 part of |
| 1- [4- (2-Hydroxyethoxy) -phenyl]-2-hydroxy-2-methyl-propanone | 0.5 portion |
| Water (W) | 50 portions of |
The preparation method of the photo-curing cross-linking conductive hydrogel comprises the following steps:
s1: weighing 20g N-hydroxymethyl acrylamide, dissolving in 20g of water, and stirring to dissolve completely to obtain a solution A;
s2: weighing 0.2g N, N' -methylene bisacrylamide, dissolving in 1g of water, and stirring until the mixture is completely dissolved to obtain a solution B;
s3: weighing 1g of lithium magnesium silicate, dissolving the lithium magnesium silicate in 5g of water, and stirring until the lithium magnesium silicate is completely dissolved to obtain a solution C;
s6: weighing 24g of water, adding the solution C and stirring uniformly; weighing 6g of potassium chloride, slowly adding the potassium chloride into the solution, and stirring until the potassium chloride is completely dissolved to obtain a solution D;
s7: mixing the solution A, the solution C and the solution D, then fully stirring, weighing 40g of glycerol, adding into the solution, and fully stirring until the solution is uniform to obtain a solution E;
s8: weighing 0.5g of 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone, adding the solution E under the condition of keeping out of the sun, and stirring until the solution E is completely dissolved to obtain a conductive adhesive solution;
s9: and under the ultraviolet illumination condition with the wavelength of 250-420nm, crosslinking for 30 seconds to obtain the conductive adhesive.
The photo-curing cross-linking conductive hydrogel prepared in the embodiments 1 to 3 and the comparative examples 1 to 3 is subjected to performance detection, and detection items comprise monomer residue condition, alternating current impedance, stability of exposed air, cytotoxicity and stability. Wherein the electrical property test is according to YY/T0196-2005, the cytotoxicity is according to GB/T16886.5, and the stability is observed by exposing the conductive hydrogel in the air. Meanwhile, a certain commercially available photocuring conductive adhesive is subjected to comparative test under the same conditions according to the same method, and the commercially available photocuring conductive adhesive takes an acrylic monomer as a main component. The results are shown in Table 7.
TABLE 7 comparison of conductive adhesive Performance test results
| Item | Monomer residue | AC impedance | Tensile Properties | Stability of | Cytotoxicity |
| Example 1 | Is free of | 90Ω | Is stronger | Is stable for more than one year | Level 0 |
| Example 2 | Is free of | 83Ω | Is stronger | Is stable for more than one year | Level 0 |
| Example 3 | Is free of | 92Ω | Is stronger | Is stable for more than one year | Level 0 |
| Comparative example 1 | Is free of | 75Ω | Is stronger | Dry for three days | Level 0 |
| Comparative example 2 | Is free of | 104Ω | Weak (weak) | Yellowing for one week | Level 0 |
| Comparative example 3 | Is free of | 230Ω | Is stronger | More than one year | Stage 2 |
| Commercially available product | 0.02～0.5wt％ | 140Ω | Weak (weak) | Yellowing in one month | Stage 2 |
As can be seen from the performance test results of table 7: in the absence of the humectant glycerin component of comparative example 1, the resulting photocurable crosslinked conductive hydrogel dried on exposure to air on the third day; in the comparative example 2, the component of magnesium lithium silicate, which is a thickener, is absent, the alternating current impedance is increased, the tensile property is reduced, and the stability is poor; in the absence of the neutralizing agent component of comparative example 3, the reduction in ions resulted in a substantial increase in ac impedance, while the cytotoxicity increased significantly due to the acidic pH. Therefore, the humectant, the thickener and the neutralizer are indispensable effective components required by the performance of the photo-curing crosslinking conductive hydrogel obtained by the invention.
As can be seen from the performance test results of table 7: the commercial conductive adhesive has trace monomer residues, and the photocuring crosslinking conductive hydrogel prepared by the method has no monomer residues; the alternating current impedance of the photocuring crosslinking conductive hydrogel prepared by the invention is about 80-90 omega, and is reduced by more than 50% compared with the commercially available electrode conductive adhesive; the conductive adhesive prepared by the invention has long-term stability when exposed in the air, and the commercially available electrode conductive adhesive becomes yellow after being exposed in the air for one month; the cytotoxicity of the photo-curing cross-linking conductive hydrogel prepared by the invention is 0 grade, and the commercial electrode conductive adhesive reaches 2 grade, which shows that the conductive adhesive obtained by the invention has more excellent biocompatibility.
The conductive hydrogel prepared in the embodiment 1, the non-woven fabric and the electrode buckle form a disposable electrocardio electrode, and the disposable electrocardio electrode and the imported electrode patch product can monitor electrocardio signals of the same patient at the same time and the same instrument. And comparing a section of waveform in the real-time monitoring period. FIG. 1 is a comparison graph of ECG monitoring signals of the electrode made in the present invention and the inlet electrode. In fig. 1, channels 1, 3 and 5 are electrode patches prepared by the present invention, and channels 2, 4 and 6 are inlet electrode patch products. The comparison shows that the electrode patch obtained by the invention has clear signals, stable waveform, capability of recording fine electrocardio fluctuation and more excellent performance compared with the imported electrode patch product.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A photocurable crosslinked conductive hydrogel characterized by: the adhesive is prepared from the following components in parts by mass: 12-40 parts of a monomer, 3-9 parts of a neutralizer, 0.07-0.3 part of a cross-linking agent, 20-65 parts of a humectant, 4-10 parts of a conductive agent, 0.3-5 parts of a thickening agent, 0.2-1.2 parts of a photoinitiator and 20-70 parts of water; the monomer is an acrylamide monomer; the acrylamide monomer is selected from at least one of acrylamide, methacrylamide, N-dimethylacrylamide, N-diethylacrylamide, N-tert-butylacrylamide, N-methylolacrylamide and N- (2-hydroxyethyl) acrylamide; the thickener is lithium magnesium silicate.
2. A photocurable crosslinked conductive hydrogel in accordance with claim 1, characterized in that: the neutralizing agent is at least one selected from sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium bicarbonate, triethanolamine, diethanolamine and triethylamine.
3. A photocurable crosslinked conductive hydrogel in accordance with claim 1, characterized in that: the conductive agent is at least one selected from sodium chloride, potassium chloride, ammonium chloride, sodium sulfate and potassium sulfate.
4. A photocurable crosslinked conductive hydrogel in accordance with claim 1, characterized in that: the cross-linking agent is at least one selected from N, N ' -vinyl bisacrylamide, N ' - (1, 2-dihydroxyethylene) bisacrylamide and N, N ' -methylene bisacrylamide.
5. A photocurable crosslinked conductive hydrogel in accordance with claim 1, characterized in that: the humectant is at least one selected from glycerol, propylene glycol and polyethylene glycol.
6. A photocurable crosslinked conductive hydrogel in accordance with claim 1, characterized in that: the photoinitiator is at least one selected from alpha-hydroxyketone, 1- [4- (2-hydroxyethoxy) -phenyl ] -2-hydroxy-2-methyl acetone, 1-hydroxycyclohexyl phenyl ketone, acylphosphine oxide photoinitiator and 2, 2' -azo-bis (2-amidinopropane) photoinitiator.
7. A method for preparing the photo-curing crosslinking conductive hydrogel according to any one of claims 1 to 6, which comprises the following steps: the method comprises the following steps:
1) respectively dissolving a monomer, a cross-linking agent, a neutralizing agent and a thickening agent in water to respectively obtain solutions A, B, C and D;
2) adding the solution C into the solution A, mixing, standing and defoaming to obtain a solution E;
3) adding water into the solution E for dilution, and mixing with a conductive agent to obtain a solution F;
4) mixing the solution B, the solution D, the solution F and a humectant to obtain a solution G;
5) adding a photoinitiator into the solution G under a dark condition, and mixing to obtain a conductive adhesive solution;
6) and curing the conductive adhesive solution under ultraviolet light to obtain the photocuring crosslinking conductive hydrogel.
8. Use of the photo-curable cross-linked conductive hydrogel of any one of claims 1 to 6 in the preparation of an electrode patch.
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