CN112164489B - Conductive carbon paste for blood glucose test paper, preparation method thereof and blood glucose test paper - Google Patents
Conductive carbon paste for blood glucose test paper, preparation method thereof and blood glucose test paper Download PDFInfo
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Abstract
The invention relates to conductive carbon paste for blood glucose test paper, a preparation method thereof and the blood glucose test paper, wherein the conductive carbon paste comprises the following components in percentage by mass: 5-35% of graphene, 0.1-15% of conductive carbon black, 0.001-1% of a dispersing agent, 5-50% of an oily resin and 35-80% of a solvent, wherein the oily resin is acrylate resin. According to the invention, the graphene sheet and the carbon black are added into the specific resin, and the dispersing agent is matched for use, so that the electrode obtained after the prepared conductive carbon slurry is solidified has good conductivity and stable electrochemical performance, the surface of the electrode and the enzyme solution also have good wettability, and the adhesion of the dried enzyme film on the electrode is good. The conductive carbon paste is used for preparing the electrode of the blood glucose test paper, the electrode has good and stable conductive performance, the surface of the electrode has the characteristics of easy uniform distribution of biological enzymes such as glucose oxidase or glucose dehydrogenase and the like, good adhesive force and the like, and the problems of poor sensitivity and poor reliability of the existing blood glucose test paper in practical application are solved.
Description
Technical Field
The invention belongs to the technical field of conductive carbon paste for blood glucose test paper, and particularly relates to conductive carbon paste for blood glucose test paper, a preparation method of the conductive carbon paste and the blood glucose test paper.
Background
The electrochemical detection method for measuring blood sugar concentration is a common blood sugar concentration detection method, and reflects the blood sugar concentration by detecting a current signal generated in the reaction process of enzyme and glucose in an electrode reaction area through a blood sugar test paper. The current signal output value of the blood glucose test paper is in direct proportion to the reaction area of the electrode reaction area, and the distribution area of the enzyme in the electrode reaction area directly determines the effective reaction area of the electrode reaction area. The wettability of the electrode surface has a crucial influence on the distribution of the enzyme in the electrode reaction region, thereby influencing the reliability and sensitivity of the blood glucose detection result. In addition, the conductivity and performance stability of the electrodes can also affect the reliability and sensitivity of blood glucose detection.
At present, most of blood glucose test paper electrodes made of conductive carbon paste have the defects of poor wettability between the surface of the electrode and enzyme, poor conductivity, unstable performance and the like, and cause the problems of low sensitivity and poor reliability of blood glucose detection. For this reason, some technical means have been adopted to improve the performance of the conductive carbon paste.
For example, the Chinese patent CN104569093A discloses a carbon paste for an electrochemical detection test strip and a preparation method thereof, and an electrochemical detection test strip and a preparation method thereof, wherein the raw material formula of the carbon paste comprises 10.8-38.3% of graphite, 1.8-17.0% of conductive carbon black, 4.5-7.5% of polyester resin, 0.2-5.0% of surfactant and 45.0-69.8% of solvent. The thin film electrode prepared by the carbon paste has good wettability with enzyme, but the conductivity and performance stability of the thin film electrode are not related, and the test sensitivity of the prepared electrochemical test strip is not obviously improved.
The flexible film adopts a raw material formula of slurry which comprises 60-88.45 parts of polyurethane resin, 0.5-10 parts of graphene or graphene compound, 1-15 parts of carbon conductive filler, 2-10 parts of dispersant, 0.5 part of auxiliary agent and solvent. The slurry improves the conductive network structure in the polymer matrix and has excellent conductive performance, however, the slurry is developed aiming at the heating material, and is not suitable for conductive carbon slurry of blood glucose test paper in terms of the formula and the selected resin.
In a word, most of the current blood glucose test paper electrodes made of conductive carbon paste have the defects of poor wettability between the electrode surface and enzyme, poor conductivity, unstable performance and the like, and the sensitivity and reliability of blood glucose detection are seriously influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an improved conductive carbon paste for blood glucose test paper and a preparation method thereof.
The invention also provides a blood glucose test paper.
In order to achieve the purpose, the invention adopts the technical scheme that:
the conductive carbon paste for the blood glucose test paper comprises the following raw materials in percentage by mass:
the oleoresin is acrylate resin.
Further, the raw material formula of the conductive carbon paste comprises the following components in percentage by mass:
according to some embodiments of the invention, the conductive carbon black has a particle size of 14 to 300 nm.
According to some embodiments of the invention, the graphene is a 1-8 layer graphene sheet.
According to some embodiments of the invention, the acrylic resin is an oleoacrylic resin having a solids content of 65-100%. Preferably, the acrylic resin is oily acrylic resin with the solid content of 70-100%. Such as NDG6113 from Nentada Chemicals, Canada, NDG6728, and CFT2371 from Weifang Fule New materials, Inc.
According to some embodiments of the invention, the dispersant is one or more of lysine, polyacrylamide, polyvinylpyrrolidone.
According to some embodiments of the invention, the solvent is one or more of N-methylpyrrolidone, diethylene glycol ethyl ether acetate, and ethylene glycol butyl ether.
The invention adopts another technical proposal: a preparation method of the conductive carbon paste for the blood glucose test paper comprises the following steps:
(1) mixing graphene, conductive carbon black, a dispersant and a solvent according to a formula, and then grinding;
(2) adding oleoresin into the slurry obtained in the step (1), stirring, and then grinding until the particle size is below 10 microns;
(3) and (3) defoaming the slurry obtained in the step (2) to prepare the conductive carbon slurry.
According to some embodiments of the invention, in the step (1), zirconia beads with a particle size of 0.3-0.5mm are used for grinding for 30-50 min. The graphene, the conductive carbon black and the dispersing agent are ground, so that the dispersibility and the conductivity can be effectively improved.
According to some embodiments of the present invention, in the step (3), the defoaming is performed until the bubble volume ratio is 0.1% or less.
According to some embodiment aspects of the invention, the defoaming is performed under a vacuum degree of 0.1 ± 0.05MPa, and the defoaming time is 30-60 seconds.
The particle size and the bubble residue of the slurry are controlled, and the stability of the conductive carbon slurry can be effectively improved. Too large a particle size affects the conductivity of the slurry, and too many bubbles affect the uniformity of film formation.
According to yet another technical scheme, the blood glucose test paper comprises a base material and an electrode layer formed on the base material, wherein the electrode layer is formed by coating the conductive carbon paste on the base material and curing the conductive carbon paste.
Further, the base material is PET, PVC, PP or PC.
Further, the curing is carried out at 100-140 ℃ for baking.
Further, the coating is performed by printing.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the invention, the graphene sheet and the carbon black are added into the specific resin, and the dispersing agent is matched for use, so that the electrode obtained after the prepared conductive carbon slurry is solidified has good conductivity and stable electrochemical performance, the surface of the electrode and the enzyme solution also have good wettability, and the adhesion of the dried enzyme film on the electrode is good.
The preparation method of the conductive carbon paste has low requirement on equipment, simple process and easy operation and industrial production.
The conductive carbon paste is used for preparing the electrode of the blood glucose test paper, the electrode has good and stable conductive performance, the surface of the electrode has the characteristics of easy uniform distribution of biological enzymes such as glucose oxidase or glucose dehydrogenase and the like, good adhesive force and the like, and the problems of poor sensitivity and poor reliability of the existing blood glucose test paper in practical application are solved.
Drawings
FIG. 1 is a graph showing the relationship between the response current and the blood glucose concentration of blood glucose test strips prepared using the conductive carbon pastes of examples 1 to 3 and comparative examples 1 to 3.
Detailed Description
The technical solutions of the present invention are described in detail below with reference to specific examples so that those skilled in the art can better understand and implement the technical solutions of the present invention, but the present invention is not limited to the scope of the examples.
Example 1
The conductive carbon paste for blood glucose test paper provided by the embodiment comprises the following raw materials: 9 wt% of graphene, 0.5 wt% of conductive carbon black, 10.5 wt% of oily acrylic resin, 0.01 wt% of polyacrylamide, 0.09 wt% of polyvinylpyrrolidone, 19.9 wt% of N-methylpyrrolidone and 60 wt% of diethylene glycol ethyl ether acetate.
The oily acrylic resin is available from Canada and can reach the chemical level, and the model is NDG 6113.
The thin-layer graphene with 1-8 layers of graphene is self-made, and the multilayer graphene is obtained by mechanically/chemically stripping graphite.
The conductive carbon black has a particle size of 30-40nm, and is under the brand name TIMCAL and the model number SUPER P LI.
The conductive carbon paste is prepared by the following method:
(1) mixing graphene, conductive carbon black, polyvinylpyrrolidone, N-methyl pyrrolidone and diethylene glycol ethyl ether acetate, adding into a sand mill, and grinding, wherein the diameter of zirconia beads used for grinding is 0.3-0.5mm, the rotating speed is controlled to be 2200 rpm, and the grinding time is 45 minutes;
(2) adding the oily acrylic resin and the slurry obtained in the step (1) into a stirrer for stirring, wherein the rotating speed is controlled to be 1000 revolutions per minute, and the stirring is carried out for 30 minutes;
(3) and (3) grinding the slurry obtained in the step (2) in a three-roll grinder for 3-5 times, wherein the roll gap is controlled to be 10 mu m, and the grinding is carried out until the particle size of the slurry is below 10 mu m.
(4) And (4) adding the slurry obtained in the step (3) into a defoaming stirrer to perform defoaming and stirring treatment, wherein the time is controlled to be 60 seconds, the vacuum degree is controlled to be 0.1MPa, the rotating speed is controlled to be 2000 r/min, and defoaming is performed until the foam volume ratio is less than 0.1%. After the process is finished, the conductive carbon paste for the blood glucose test paper is obtained.
Example 2
The raw material formulation of the conductive carbon paste for blood glucose test paper provided in this example is shown in table 1, and the preparation method is the same as that of example 1. Among them, the oleo acrylic resin was purchased from the canadian dunkoku model NDG 6728.
The dispersant is polyvinylpyrrolidone.
The solvent is diethylene glycol ethyl ether acetate.
Example 3
The raw material formulation of the conductive carbon paste for blood glucose test paper provided in this example is shown in table 1, and the preparation method is the same as that of example 1. Wherein the oily acrylic resin is purchased from Weifang Fule New Material Co., Ltd, and the model is CFT 2371.
The dispersant is polyacrylamide.
The solvent is ethylene glycol butyl ether.
Comparative example 1
The raw material formulation of the conductive carbon paste provided in this comparative example is shown in table 1, and the rest is the same as that of example 1. Wherein the resin is oil polyurethane resin, and is purchased from Dongguan treasure Jing chemical Co., Ltd, model MR-917.
Comparative example 2
The raw material formulation of the conductive carbon paste provided in this comparative example is shown in table 1, and the rest is the same as that of example 1. The resin is polyester resin of SK company, model ES 550.
Comparative example 3
The conductive carbon paste provided by the comparative example was a brand of conductive carbon paste purchased.
Table 1 shows the raw material formulations (in mass percent) of the conductive carbon pastes of examples 1 to 3 and comparative examples 1 to 3
Performance test of conductive carbon pastes of examples 1 to 3 and comparative examples 1 to 3
1) Preparation of a detection sample: the conductive carbon pastes of examples 1 to 3 and comparative examples 1 to 3 were respectively printed on a PET substrate by screen printing and baked at 120 c for 3 minutes to form an electrode thin film layer on the substrate.
2) And measuring the resistivity of the electrode film layer by using a four-probe method, and re-measuring the resistivity after the electrode film layer is placed at normal temperature for half a year.
3) Dropping the enzyme slurry on an electrode thin film layer of a sample, testing the contact angle of the enzyme slurry on the surface of the electrode by using a contact angle measuring instrument, and taking an average value after 10 times of testing, wherein the small contact angle shows that the electrode thin film layer has better wettability to the enzyme slurry, thereby being beneficial to the uniform distribution of the enzyme slurry on the electrode thin film layer; the enzyme membrane was rubbed 10 times to determine the adhesion to the electrode by observing whether the dried enzyme membrane was separated from the electrode.
The enzyme slurry is self-prepared 1 ‰ glucose oxidase aqueous solution, and the glucose oxidase is purchased from Aladdin, model G109029.
4) The prepared electrode samples are respectively applied to blood glucose test strips, response current and blood glucose concentration curves of the blood glucose test strips are tested by an electrochemical workstation, and the sensitivity of the blood glucose test strips is calculated by referring to the graph shown in figure 1.
The results of the blood glucose test paper samples prepared by using the conductive carbon pastes of examples 1 to 3 and comparative examples 1 to 3 are shown in Table 2 after the test by the method.
Table 2 shows the results of the performance test of the conductive carbon pastes of examples 1 to 3 and comparative examples 1 to 3
As can be seen from table 2:
(1) the resistivity of examples 1-3 was as low as 0.01 Ω · cm, and the resistivity of examples 1-3 was lower than that of comparative examples 1-3, indicating that the conductive properties of examples 1-3 were superior. After half a year of standing at room temperature, the resistivity of examples 1-3 changed very little; the resistivity of comparative examples 1 to 3 changed by more than 20% after being left at room temperature for half a year. This indicates that examples 1-3 have stable and excellent conductivity, and can effectively ensure the reliability of the test result of the blood glucose test paper.
(2) The contact angles of examples 1 to 3 and comparative example 2 were small, and the contact angles of comparative example 1 and comparative example 3 were large, indicating that the electrodes prepared in examples 1 to 3 and comparative example 2 had good surface wettability and that the enzyme slurry was easily uniformly distributed thereon.
(3) In examples 1 to 3, the enzyme membrane was not peeled off after kneading the enzyme membrane 10 times, and in comparative examples 1 to 3, the enzyme membrane was peeled off to various degrees after kneading the enzyme membrane 10 times. This indicates that the enzyme membrane has good adhesion to the electrodes prepared in examples 1-3.
(4) The sensitivity of the blood glucose test strips prepared in examples 1-3 was 0.314-0.346. mu.A/mmol/L.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Claims (9)
1. The conductive carbon paste for the blood glucose test paper is characterized by comprising the following raw materials in percentage by mass:
8-10% of graphene;
0.5-5% of conductive carbon black;
0.005-0.5% of a dispersant;
10-30% of an oily resin;
55-80% of a solvent;
the oleoresin is acrylic resin.
2. The conductive carbon paste for blood glucose test strips according to claim 1, wherein: the particle size of the conductive carbon black is 14-300 nm.
3. The conductive carbon paste for blood glucose test strips according to claim 1, wherein: the graphene is a graphene sheet with 1-8 layers.
4. The conductive carbon paste for blood glucose test strips according to claim 1, wherein: the acrylic resin is oily acrylic resin with the solid content of 65-100%.
5. The conductive carbon paste for blood glucose test strips according to claim 1, wherein: the solvent is one or a combination of N-methyl pyrrolidone, diethylene glycol ethyl ether acetate and ethylene glycol butyl ether.
6. A preparation method of the conductive carbon paste for the blood glucose test paper as set forth in any one of claims 1 to 5, characterized in that the preparation method comprises the following steps:
(1) mixing graphene, conductive carbon black, a dispersant and a solvent according to a formula, and then grinding;
(2) adding oleoresin into the slurry obtained in the step (1), stirring, and then grinding until the particle size is below 10 microns;
(3) and (3) defoaming the slurry obtained in the step (2) to prepare the conductive carbon slurry.
7. The method for preparing the conductive carbon paste for blood glucose test strips according to claim 6, wherein the method comprises the following steps: in the step (1), zirconia beads with the particle size of 0.3-0.5mm are used for grinding, and the grinding time is 30-50 min; in the step (3), the defoaming is carried out until the volume ratio of bubbles is less than or equal to 0.1%.
8. A blood glucose test strip comprises a substrate and an electrode layer formed on the substrate, and is characterized in that: the electrode layer is formed by coating the conductive carbon paste of any one of claims 1 to 5 on the substrate and curing.
9. The blood glucose test strip of claim 8, wherein: the base material is PET, PVC, PP or PC.
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| CN202010919535.4A CN112164489B (en) | 2020-09-04 | 2020-09-04 | Conductive carbon paste for blood glucose test paper, preparation method thereof and blood glucose test paper |
| PCT/CN2020/131017 WO2022048040A1 (en) | 2020-09-04 | 2020-11-24 | Electrically conductive carbon paste for blood glucose test paper, preparation method therefor, and blood glucose test paper |
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| CN109817385A (en) * | 2018-12-28 | 2019-05-28 | 常州碳森石墨烯科技有限公司 | A kind of preparation method that environment-friendly type graphene conductive carbon is starched and its application on flexible heating film |
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| TWI532793B (en) * | 2014-04-15 | 2016-05-11 | 安炬科技股份有限公司 | Graphene masterbatch |
| CN104449010A (en) * | 2014-12-26 | 2015-03-25 | 苏州格瑞丰纳米科技有限公司 | Polymer/graphene anti-static coating, preparation method and application thereof |
| CN104569093B (en) * | 2015-01-23 | 2017-09-12 | 三诺生物传感股份有限公司 | A kind of electrochemical detection test strip is starched and preparation method thereof and a kind of electrochemical detection test strip and preparation method thereof with carbon |
| CN106243836A (en) * | 2016-08-15 | 2016-12-21 | 青岛德通纳米技术有限公司 | A kind of graphene conductive carbon slurry and preparation method thereof |
| CN106433319B (en) * | 2016-10-14 | 2020-05-26 | 中国科学院山西煤炭化学研究所 | Water-based environment-friendly conductive carbon paste based on graphene-carbon black composite filler and preparation method thereof |
| CN108039225A (en) * | 2017-12-13 | 2018-05-15 | 常州烯材碳材料科技有限公司 | Environment-friendly type low resistance graphene carbon fiber conductive carbon paste and preparation method thereof |
| US11134874B2 (en) * | 2018-04-06 | 2021-10-05 | Zense-Life Inc. | Enhanced carbon-enzyme membrane for a working electrode of a continuous biological sensor |
| CN110310762A (en) * | 2018-08-22 | 2019-10-08 | 苏州怡拓生物传感技术有限公司 | Modified graphene conductive carbon paste |
| CN109637697A (en) * | 2018-12-24 | 2019-04-16 | 广东省稀有金属研究所 | A kind of graphene conductive slurry and preparation method thereof |
| CN111073396A (en) * | 2020-01-19 | 2020-04-28 | 浙江纳美新材料股份有限公司 | Graphene-based water-based conductive ink and preparation method thereof |
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