Conductive adhesive with detection parameter convergence and preparation method and application thereof

Abstract

The invention belongs to the technical field of electromagnetic detection, and particularly relates to a conductive adhesive with detection parameter convergence and a preparation method and application thereof. The conductive adhesive provided by the invention comprises a gel component and a function initiation component, the gel component comprises acrylic acid, potassium chloride, potassium hydroxide and glycerol; the functional initiation component is composed of a photoinitiator, a cross-linking agent and a thickening agent; the weight part ratio of the gel component to the function initiating component is (13-17): 1. The conductive adhesive provided by the invention has detection parameter convergence and direct-current offset voltage not greater than 50mv.

Description

Technical Field

[0001] The present invention belongs to the technical field of electromagnetic detection, and in particular relates to a conductive adhesive with detection parameter convergence, a preparation method and an application thereof. Background Art

[0002] Electromagnetic field detection technology is a new technology that has recently emerged both domestically and internationally. When using electromagnetic field biodetection technology, it is crucial to ensure convergence across multiple tests on healthy subjects. This means that the measured values ​​remain stable and the error does not exceed a specified range. For example, a healthy blood pressure monitor's diastolic blood pressure readings are typically between 60-90 and 100-150, respectively. If a patient's blood pressure readings exceed the healthy range, it can be determined to be due to a pathological condition within the organism, thus achieving clinical diagnosis.

[0003] Traditional biomonitoring products, such as thermometers, blood pressure monitors, and ECG monitors, use biosensors (e.g., bandages and ECG electrodes) to detect parameters such as temperature and blood pressure in biological tissue. However, these products lack accuracy and efficiency. Electromagnetic field detection technology can non-invasively, digitally, rapidly, and cost-effectively measure the electrical conductivity of biological tissue, thereby enabling disease detection or discovery. Traditional biomonitoring products (such as conventional ECG electrodes) fail to meet the requirements of electromagnetic field biodetection. This is because the measured values ​​of conventional ECG electrodes exhibit irregular distribution across individuals. Since the measured data from healthy subjects are also scattered, not within a single confidence interval and not normally distributed, it is difficult to distinguish between healthy subjects and patients in clinical practice. Therefore, the development of conductive gels suitable for electromagnetic field detection is of great significance.

[0004] Patent publication number CN107400464A, entitled "A Medical Polyacrylate Conductive Adhesive and Its Preparation Method," discloses a conductive adhesive comprising polyacrylic acid oligomers, sodium polyacrylate, aqueous polyacrylic acid monomers, surfactants, polyglycerol, polyacrylamide, a thickener, and a crosslinker. The patent addresses the technical problem of improving the electrical performance of medical conductive adhesives. However, the adhesive has not demonstrated satisfactory performance for electromagnetic testing.

[0005] In summary, it is necessary to propose new methods and strategies to address the shortcomings of existing technologies. Summary of the Invention

[0006] The purpose of the present invention is to provide a conductive adhesive with convergent detection parameters and its preparation method and application, which partially solves or alleviates the above-mentioned deficiencies in the prior art. The present invention specifically adopts the following technical solutions: A conductive adhesive with detection parameter convergence, the conductive adhesive comprising a gel component and a functional initiating component; the gel component comprising acrylic acid, potassium chloride, potassium hydroxide, and glycerin; the functional initiating component comprising a photoinitiator, a crosslinking agent, and a thickener; the weight ratio of the gel component to the functional initiating component being 13-17:1; The photoinitiator is 2-hydroxy-2-methylphenyl acetone; the crosslinking agent is tripropylene glycol diacrylate; and the tackifier is polyisobutylene. The photoinitiator contains a carbonyl group (C=O) and a hydroxyl group (-OH); the crosslinker contains an acryloyl group (C=C-COO-); and the thickener contains a carbon-carbon single bond and a small amount of carbon-carbon double bond. The conductive adhesive specifically includes the following materials in parts by weight: 10-20 parts of acrylic acid, 1-10 parts of potassium chloride, 15-20 parts of potassium hydroxide, 40-50 parts of glycerol, 0.1-0.5 parts of 2-hydroxy-2-methylphenyl acetone, 0.5-1 parts of tripropylene glycol diacrylate, 3-6 parts of polyisobutylene and 15-30 parts of distilled water.

[0007] Furthermore, the total weight ratio of acrylic acid, potassium chloride and potassium hydroxide to glycerol in the gel component is close to 1:1.

[0008] The “close to 1:1” mentioned in the present invention means that the total weight of acrylic acid, potassium chloride and potassium hydroxide in the gel component, calculated based on the weight of glycerol, differs by less than 20% compared with that of glycerol.

[0009] Preferably, the weight ratio of the total weight of the acrylic acid, potassium chloride and potassium hydroxide to the weight of the glycerol is 0.8-1.2:1.

[0010] Furthermore, the total weight of the photoinitiator and the crosslinking agent in the functional initiating component is less than the weight of the thickener.

[0011] Preferably, the weight ratio of the total weight of the photoinitiator and the cross-linking agent to the weight of the thickener is 1:4-5.

[0012] As a preferred embodiment, the conductive adhesive specifically includes the following materials in parts by weight: 15-20 parts of acrylic acid, 3-10 parts of potassium chloride, 15-20 parts of potassium hydroxide, 40-45 parts of glycerol, 0.1-0.3 parts of 2-hydroxy-2-methylphenyl acetone, 0.7-1 parts of tripropylene glycol diacrylate, 4-6 parts of polyisobutylene and 15-20 parts of distilled water.

[0013] As a more preferred embodiment, the conductive adhesive specifically includes the following materials in parts by weight: 15 parts of acrylic acid, 3 parts of potassium chloride, 19 parts of potassium hydroxide, 43 parts of glycerol, 0.3 parts of 2-hydroxy-2-methylphenylacetone, 0.7 parts of tripropylene glycol diacrylate, 4.5 parts of polyisobutylene and 16 parts of distilled water.

[0014] As another more preferred embodiment, the conductive adhesive specifically comprises the following materials in parts by weight: 20 parts of acrylic acid, 10 parts of potassium chloride, 20 parts of potassium hydroxide, 43 parts of glycerol, 0.3 parts of 2-hydroxy-2-methylphenyl acetone, 0.7 parts of tripropylene glycol diacrylate, 4.5 parts of polyisobutylene and 16 parts of distilled water. An electrode sheet for electromagnetic detection, comprising the above-mentioned conductive glue with detection parameter convergence.

[0015] Furthermore, the electrode sheet also includes a backing and a pressure-sensitive adhesive.

[0016] Those skilled in the art will appreciate that the backing and pressure-sensitive adhesive are conventionally available products in the art, and their function is to assemble into electrode sheets.

[0017] Application of the conductive adhesive with detection parameter convergence in the preparation of biosensors for electromagnetic detection.

[0018] The present invention also provides a method for preparing the conductive adhesive having the above-mentioned detection parameter convergence, comprising the following steps: S01: Dissolve potassium hydroxide in part of the distilled water of the formula components, stir until completely dissolved, to obtain a potassium hydroxide solution, and cool for later use; dissolve potassium chloride in part of the distilled water of the formula components, stir until completely dissolved, to obtain a potassium chloride solution for later use; S02: Pour acrylic acid and the remaining distilled water of the formula components into a container and stir until completely dissolved to obtain an acrylic acid solution; S03: adding the cooled potassium hydroxide solution to the acrylic acid solution and stirring until the mixture is completely uniform to obtain a first mixed solution; S04: adding a photoinitiator and a cross-linking agent to the first mixed solution in sequence, stirring until the mixture is uniformly mixed, and then slowly adding a thickener while stirring to obtain a second mixed solution; S05: adding potassium chloride solution and glycerin to the second mixed solution in sequence, stirring until uniform, to obtain a conductive adhesive solution; S06: UV-curing the conductive adhesive solution to obtain the conductive adhesive.

[0019] Beneficial technical effects: The present invention provides a conductive adhesive for electromagnetic detection, wherein the conductive adhesive has detection parameter convergence and a DC offset voltage of no more than 50 mV. The conductive adhesive comprises a gel component and a functional initiating component, and the present invention screens and verifies the composition and ratio of the gel component and the functional initiating component, respectively. Experimental results show that, when used for electroencephalogram (EEG) detection, the preferred conductive adhesive of the present invention exhibits a generally normal distribution of detection data from 161 healthy subjects, with the data generally falling within a confidence interval and exhibiting convergence. This demonstrates that the preferred conductive adhesive of the present invention can meet the requirements of electromagnetic detection and has the potential to be prepared as an electromagnetic detection biosensor. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following is a brief introduction to the drawings required for the embodiments or the description of the prior art. In all drawings, similar elements or parts are generally identified by similar reference numerals. In the drawings, the various elements or parts are not necessarily drawn according to the actual scale. Obviously, the drawings described below are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without inventive work.

[0021] Figure 1 This is a result diagram showing that the disturbance coefficient obeys a normal distribution in one embodiment; Figure 2 This is a graph showing the normal distribution of disturbance coefficients of healthy subjects in one embodiment. DETAILED DESCRIPTION

[0022] To make the purpose, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0023] As used herein, "and / or" includes any and all combinations of one or more of the associated listed items.

[0024] Herein, "plurality" means two or more than two, ie, it includes two, three, four, five, etc.

[0025] As used in this specification, the term "about" typically means + / - 5% of the stated value, more typically + / - 4% of the stated value, more typically + / - 3% of the stated value, more typically + / - 2% of the stated value, even more typically + / - 1% of the stated value, and even more typically + / - 0.5% of the stated value.

[0026] In this specification, certain embodiments may be disclosed in a format that is within a range. It should be understood that this description of "within a range" is merely for convenience and brevity and should not be interpreted as a rigid limitation on the disclosed range. Therefore, the description of a range should be considered to have specifically disclosed all possible subranges and individual numerical values ​​within this range. For example, the description of a range of 1-6 should be considered to have specifically disclosed subranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as individual numbers within this range, such as 1, 2, 3, 4, 5, and 6. Regardless of the breadth of the range, the above rules apply.

[0027] Definition of noun: "Test parameter convergence" as used herein refers to the stability of test results when the conductive adhesive of the present invention, which exhibits test parameter convergence, is used for electromagnetic testing, with errors within a specified range. Specifically, when N tests are performed on healthy subjects, each of the N test values ​​obtained falls within a confidence interval and follows a normal distribution with a standard deviation less than or equal to a specified standard value.

[0028] Example 1 The invention provides a conductive adhesive with detection parameter convergence and a preparation method thereof.

[0029] The conductive adhesive comprises a gel component and a functional initiating component; the gel component comprises acrylic acid, potassium chloride, potassium hydroxide and glycerin; the functional initiating component comprises a photoinitiator, a crosslinking agent and a thickener; The photoinitiator is 2-hydroxy-2-methylphenyl acetone (photoinitiator 1173); the crosslinking agent is tripropylene glycol diacrylate; and the tackifier is polyisobutylene. The conductive adhesive specifically includes the following components in parts by weight: 15 parts of acrylic acid, 3 parts of potassium chloride, 19 parts of potassium hydroxide, 43 parts of glycerol, 0.3 parts of 2-hydroxy-2-methylphenylacetone, 0.7 parts of tripropylene glycol diacrylate, 4.5 parts of polyisobutylene, and 16 parts of distilled water.

[0030] Based on the conductive adhesive components described above, this embodiment further provides a method for preparing a conductive adhesive with detection parameter convergence, which includes the following steps.

[0031] S01: Dissolve potassium hydroxide in distilled water (1 / 3 of the formula components), stir until completely dissolved, to obtain a potassium hydroxide solution, and cool for later use; dissolve potassium chloride in distilled water (1 / 3 of the formula components), stir until completely dissolved, to obtain a potassium chloride solution for later use.

[0032] S02: Pour acrylic acid and the remaining 1 / 3 of distilled water into a container and stir until completely dissolved to obtain an acrylic acid solution.

[0033] S03: Adding cooled potassium hydroxide solution to the acrylic acid solution and stirring until the mixture is completely uniform to obtain a first mixed solution.

[0034] S04: adding a photoinitiator and a cross-linking agent to the first mixed solution in sequence, stirring until the mixture is uniform, and then slowly adding a thickener while stirring to obtain a second mixed solution.

[0035] S05: adding potassium chloride solution and glycerin to the second mixed solution in sequence, stirring until uniform, to obtain a conductive adhesive solution.

[0036] S06: UV-curing the conductive adhesive solution to obtain a conductive adhesive.

[0037] In some embodiments, potassium hydroxide and potassium chloride may be dissolved in multiple portions of distilled water. The stepwise and batchwise dissolution methods help to better control the dispersion and dissolution of the raw materials and avoid precipitation in subsequent steps.

[0038] Example 2 The present invention provides another conductive adhesive with detection parameter convergence and a preparation method thereof.

[0039] The conductive adhesive comprises a gel component and a functional initiating component; the gel component comprises acrylic acid, potassium chloride, potassium hydroxide and glycerin; the functional initiating component comprises a photoinitiator, a crosslinking agent and a thickener; The photoinitiator is 2-hydroxy-2-methylphenyl acetone (photoinitiator 1173); the crosslinking agent is tripropylene glycol diacrylate; and the tackifier is polyisobutylene. The conductive adhesive specifically includes the following components in parts by weight: 20 parts of acrylic acid, 10 parts of potassium chloride, 20 parts of potassium hydroxide, 43 parts of glycerol, 0.3 parts of 2-hydroxy-2-methylphenylacetone, 0.7 parts of tripropylene glycol diacrylate, 4.5 parts of polyisobutylene, and 16 parts of distilled water.

[0040] Based on the conductive adhesive components described above, this embodiment further provides a method for preparing a conductive adhesive with detection parameter convergence, which includes the following steps.

[0041] S01: Dissolve potassium hydroxide in distilled water (1 / 3 of the formula components), stir until completely dissolved, to obtain a potassium hydroxide solution, and cool for later use; dissolve potassium chloride in distilled water (1 / 3 of the formula components), stir until completely dissolved, to obtain a potassium chloride solution for later use.

[0042] S02: Pour acrylic acid and the remaining 1 / 3 of distilled water into a container and stir until completely dissolved to obtain an acrylic acid solution.

[0043] S03: Adding cooled potassium hydroxide solution to the acrylic acid solution and stirring until the mixture is completely uniform to obtain a first mixed solution.

[0044] S04: adding a photoinitiator and a cross-linking agent to the first mixed solution in sequence, stirring until the mixture is uniform, and then slowly adding a thickener while stirring to obtain a second mixed solution.

[0045] S05: adding potassium chloride solution and glycerin to the second mixed solution in sequence, stirring until uniform, to obtain a conductive adhesive solution.

[0046] S06: UV-curing the conductive adhesive solution to obtain a conductive adhesive.

[0047] Example 3 Based on Example 1, the present invention provides verification of the convergence of detection parameters when using conductive glue for electromagnetic biosensor detection.

[0048] This embodiment is used in conjunction with a noninvasive ambulatory monitor for cerebral edema, which includes test leads, an electrode sheet, and a display screen. The conductive adhesive prepared in Example 1 is combined with a backing and a pressure-sensitive adhesive to form the electrode sheet. When further incorporated with an electrode chip, a small biosensor can be formed.

[0049] After connecting the electrode sheet prepared by the conductive glue of Example 1 to the non-invasive brain edema dynamic monitor through a test line, the electrode sheet was attached to the skin of the brain, and the impedance value was measured. The measured impedance value was analyzed and processed to obtain the perturbation coefficient value. The experiment included 161 healthy subjects, and each healthy subject was tested more than or equal to 3 times to obtain the perturbation coefficient value of the healthy person and record it. The obtained perturbation coefficient value was then statistically described and tested for normality to obtain the perturbation coefficient confidence interval and data convergence effect diagram.

[0050] like Figure 1As shown in the figure, the normality test showed that the mean perturbation coefficients for 161 healthy subjects followed a normal distribution (P = 0.33 > 0.05), essentially showing a normal distribution. The mean perturbation coefficient was 142.33 (13.22), and the 95% confidence interval for the mean was (139.45, 142.93). The 95% range of the perturbation coefficient was (120.83, 163.71), demonstrating that the conductive adhesive prepared in Example 1 exhibited convergence. The data from the 161 healthy subjects were essentially normally distributed, and the data were generally within a single confidence interval. This is shown in Table 1.

[0051] Table 1 Descriptive statistics of disturbance coefficients Figure 2 The perturbation coefficient results of a healthy subject tested for 10 consecutive days are shown in the figure. The conductive adhesive of Example 1 was used for 10 consecutive days of testing. The curve of the perturbation coefficient is stable, indicating that the fluctuation of the perturbation coefficient is small and the test results are stable.

[0052] Example 4 Key material screening and verification are performed on the conductive adhesive with detection parameter convergence provided by the present invention.

[0053] The conductive adhesive with detection parameter convergence includes a gel component and a functional initiating component; the gel component includes acrylic acid, potassium chloride, potassium hydroxide, and glycerin; the functional initiating component includes a photoinitiator, a crosslinker, and a thickener. The conductive adhesive with detection parameter convergence also includes distilled water.

[0054] Table 2 Material and ratio screening verification Note: The photoinitiator in the above table refers to 2-hydroxy-2-methylphenyl acetone; the crosslinker refers to tripropylene glycol diacrylate; and the tackifier refers to polyisobutylene.

[0055] The above results show that: (1) In the comparative examples of Groups 2 and 6, which lack thickener and have excessive thickener, the DC offset voltage is greater than 50mV, but the DC offset voltage result of Group 2 with excessive thickener is worse. (2) Groups 3 and 4, which lack potassium chloride and potassium hydroxide, both have an impact on the DC offset voltage. In comparison, the impact of the lack of potassium chloride is greater. (3) Group 5, which lacks photoinitiator, has a greater impact on the DC offset voltage result. (4) Group 7, which adjusts the ratio of photoinitiator, crosslinker and thickener, has a greater impact on the DC offset voltage when the amount of photoinitiator and crosslinker is increased. (5) The DC offset voltage of the formulations of Groups 1 and 8 is less than 50mV. It can be expected that they have good test result / test parameter convergence when used for electromagnetic testing.

[0056] It should be noted that, in this document, the terms "comprises," "includes," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a process, method, article, or apparatus comprising a series of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus. In the absence of further limitations, an element defined by the phrase "comprising a ..." does not exclude the presence of other identical elements in the process, method, article, or apparatus comprising the element.

[0057] The embodiments of the present invention are described above in conjunction with the accompanying drawings, but the present invention is not limited to the above-mentioned specific implementation methods. The above-mentioned specific implementation methods are merely illustrative and not restrictive. Under the guidance of the present invention, ordinary technicians in this field can also make many forms without departing from the scope of protection of the present invention and the claims, all of which are protected by the present invention.

Claims

1. A conductive adhesive with detection parameter convergence, characterized in that: The conductive adhesive comprises a gel component and a functional initiating component; the gel component comprises acrylic acid, potassium chloride, potassium hydroxide and glycerin; the functional initiating component comprises a photoinitiator, a crosslinking agent and a thickener; the weight ratio of the gel component to the functional initiating component is 13-17:1; The photoinitiator is 2-hydroxy-2-methylphenyl acetone; the crosslinking agent is tripropylene glycol diacrylate; and the tackifier is polyisobutylene; The conductive adhesive specifically includes the following materials in parts by weight: 10-20 parts of acrylic acid, 1-10 parts of potassium chloride, 15-20 parts of potassium hydroxide, 40-50 parts of glycerol, 0.1-0.5 parts of 2-hydroxy-2-methylphenyl acetone, 0.5-1 parts of tripropylene glycol diacrylate, 3-6 parts of polyisobutylene and 15-30 parts of distilled water.

2. The conductive adhesive with detection parameter convergence according to claim 1, characterized in that: The total weight ratio of acrylic acid, potassium chloride and potassium hydroxide to glycerol in the gel component is close to 1:

1.

3. The conductive adhesive with detection parameter convergence according to claim 2, characterized in that: The weight ratio of the total weight of the acrylic acid, potassium chloride and potassium hydroxide to the weight of the glycerol is 0.8-1.2:

1.

4. The conductive adhesive with detection parameter convergence according to claim 1, wherein: The total weight portion of the photoinitiator and the crosslinking agent in the functional initiating component is less than the weight portion of the thickener.

5. The conductive adhesive with detection parameter convergence according to claim 4, characterized in that: The weight ratio of the total weight of the photoinitiator and the crosslinking agent to the weight of the thickener is 1:4-5.

6. The conductive adhesive with detection parameter convergence according to claim 1, wherein: The conductive adhesive specifically includes the following materials in parts by weight: 15-20 parts of acrylic acid, 3-10 parts of potassium chloride, 15-20 parts of potassium hydroxide, 40-45 parts of glycerol, 0.1-0.3 parts of 2-hydroxy-2-methylphenyl acetone, 0.7-1 parts of tripropylene glycol diacrylate, 4-6 parts of polyisobutylene and 15-20 parts of distilled water.

7. An electrode sheet for electromagnetic detection, characterized in that: The electrode sheet comprises the conductive glue with detection parameter convergence according to any one of claims 1 to 6.

8. The electrode sheet according to claim 7, wherein: The electrode sheet further comprises a backing and a pressure-sensitive adhesive.

9. Use of the conductive adhesive with detection parameter convergence according to any one of claims 1 to 6 in the preparation of a biosensor for electromagnetic detection.

10. The method for preparing the conductive adhesive with detection parameter convergence according to any one of claims 1 to 6, characterized in that: The following steps are involved: S01: Dissolve potassium hydroxide in part of the distilled water of the formula components, stir until completely dissolved, to obtain a potassium hydroxide solution, and cool for later use; dissolve potassium chloride in part of the distilled water of the formula components, stir until completely dissolved, to obtain a potassium chloride solution for later use; S02: Pour acrylic acid and the remaining distilled water of the formula components into a container and stir until completely dissolved to obtain an acrylic acid solution; S03: adding the cooled potassium hydroxide solution to the acrylic acid solution and stirring until the mixture is completely uniform to obtain a first mixed solution; S04: adding a photoinitiator and a cross-linking agent to the first mixed solution in sequence, stirring until the mixture is uniformly mixed, and then slowly adding a thickener while stirring to obtain a second mixed solution; S05: adding potassium chloride solution and glycerin to the second mixed solution in sequence, stirring until uniform, to obtain a conductive adhesive solution; S06: UV-curing the conductive adhesive solution to obtain the conductive adhesive with detection parameter convergence.

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