CN112521803A - Conductive carbon slurry for mobile blood glucose test piece and preparation method and application thereof - Google Patents

Conductive carbon slurry for mobile blood glucose test piece and preparation method and application thereof Download PDF

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Publication number
CN112521803A
CN112521803A CN202011409065.3A CN202011409065A CN112521803A CN 112521803 A CN112521803 A CN 112521803A CN 202011409065 A CN202011409065 A CN 202011409065A CN 112521803 A CN112521803 A CN 112521803A
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conductive carbon
blood glucose
carbon paste
glucose test
mobile blood
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CN202011409065.3A
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Chinese (zh)
Inventor
高艳飞
黄济超
项云
罗红艳
郭艳平
孙惠芳
陶良毅
潘斌
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Zhongshan Torch Polytechnic
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Zhongshan Torch Polytechnic
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/033Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/102Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • C09D11/104Polyesters

Abstract

The application provides conductive carbon paste for a mobile blood glucose test piece and a preparation method and application thereof, the conductive carbon paste is composed of 18-25 wt% of polyester resin, 8-12 wt% of ketone solvent, 5-8 wt% of ether solvent, 1-3 wt% of silicone assistant and 57-62 wt% of conductive carbon black, gloss oil formed by blending polyester resin, ketone solvent, ether solvent and silicone assistant is compounded with the conductive carbon black, the conductive carbon black mainly plays a conductive role, the polyester resin is used for coating the conductive carbon black, the conductive carbon black is bonded into a film, the ketone solvent and the ether solvent are used for dissolving the polyester resin coated with the conductive carbon black, the silicone assistant is used for promoting the leveling effect of printing the conductive carbon paste ink, the conductive carbon paste has the resistance 5 times lower than that of the conductive carbon paste sold on the market at present, and has good adhesive force, the requirement of low square resistance of a conductive circuit printed on a mobile blood glucose test piece product can be met, has good application prospect.

Description

Conductive carbon slurry for mobile blood glucose test piece and preparation method and application thereof
Technical Field
The invention belongs to the technical field of conductive carbon paste printing ink, and particularly relates to conductive carbon paste for a mobile blood glucose test piece, and a preparation method and application thereof.
Background
In the application of the conductive carbon paste ink in the IVD test piece, the conductive carbon paste cannot contain metal additives due to the characteristics of the IVD test piece. Therefore, the sheet resistance of the conductive carbon paste is mainly 10-20 Ω/sq (25 um). However, for some narrower conductive circuits in the mobile blood glucose test strip, the sheet resistance of the conductive carbon paste in the prior art cannot meet the requirements of some products, and the development of the conductive carbon paste with lower sheet resistance is urgently needed.
Disclosure of Invention
The invention provides conductive carbon paste with low sheet resistance for a mobile blood glucose test piece, aiming at solving the technical problem of high sheet resistance of the conventional conductive carbon paste applied to the mobile blood glucose test piece.
The invention also aims to provide a preparation method of the conductive carbon paste for the mobile blood glucose test piece.
The third purpose of the invention is to provide the application of the conductive carbon paste for the mobile blood sugar test piece.
The conductive carbon slurry for the mobile blood glucose test piece consists of the following components: 18-25 wt% of polyester resin, 8-12 wt% of ketone solvent, 5-8 wt% of ether solvent, 1-3 wt% of silicone additive and 57-62 wt% of conductive carbon black.
The application provides conductive carbon paste for a mobile blood sugar test piece, which consists of 18-25 wt% of polyester resin, 8-12 wt% of ketone solvent, 5-8 wt% of ether solvent, 1-3 wt% of silicone assistant and 57-62 wt% of conductive carbon black, gloss oil formed by blending the polyester resin, the ketone solvent, the ether solvent and the silicone assistant is compounded with the conductive carbon black, the conductive carbon black mainly plays a role of conductivity, the polyester resin is used for coating the conductive carbon black, the conductive carbon black is bonded into a film, the ketone solvent and the ether solvent are used for dissolving the polyester resin coated with the conductive carbon black, the silicone assistant is used for promoting the leveling effect of the printing of the conductive carbon paste ink, the conductive carbon paste has the resistance which is 5 times lower than that of the conductive carbon paste sold on the market at present, and has good adhesive force, and can meet the requirement of low square resistance of a printed conductive circuit on a mobile blood sugar test piece product, has good application prospect.
Preferably, the polyester resin has a glass transition temperature (Tg) of 60 to 100 ℃ and an average molecular weight of 8000 to 20000. The polyester resin (CAS NO.25038-59-9) of the present application, as the main resin in the composition, employs high molecular weight saturated polyester resin, which has the advantages of reduced curing shrinkage of the coating, improved substrate adhesion, and improved surface drying effect of the coating. The moderate molecular weight of the saturated polyester resin is beneficial to dissolving the conductive carbon paste in the conductive carbon paste, and a skeleton supporting effect is formed in the carbon paste. If the molecular weight is too large and larger than 20000, the conductive carbon black is difficult to dissolve and tends to cause a sharp increase in the viscosity of the system. The Tg point of the saturated polyester resin is too high to be adhered to the surface of PET, so that the adhesion is reduced, and if the Tg point is too low, the surface drying effect of the coating is not improved. More preferably, the saturated polyester resin comprises at least one of 226, 240, 280, GK250, GK810 of the eastern ocean spinning Vylon series.
Preferably, the particle size of the conductive carbon black is 10-100 nm, and the oil absorption value is 160-200 ml/100 g. The conductive carbon black is preferably products of Kamot corporation with the models of XC72, XC72R, VXC72 and VXC72R, the particle diameter is preferably 30nm, the oil absorption value is 174-192 ml/100g, and the specific surface area is 254m2The conductive carbon paste has the characteristics of high conductivity and easy dispersion, and is used as a main material in a formula, so that a conductive carbon paste product with low resistance can be obtained.
Preferably, the ketone solvent is one or more of isophorone, methyl isobutyl ketone and cyclohexanone. The ketone solvent plays a role of a diluent, preferably, the ketone solvent is isophorone (CAS NO.78-59-1), has the characteristics of higher boiling point, very low hygroscopicity and small evaporation speed, has strong dissolving capacity, good dispersibility and good leveling property of isophorone, has the balance capacity of formed dispersoid and the existence of polarity and hydrogen bond force, has excellent dissolving capacity of isophorone on polyester resin, and has good solubility when being mixed with ether solvents. Preferably VESTASOL or vestatat, a product of the winning creative goods company.
Preferably, the ether solvent is one or more of ethylene glycol butyl ether, ethylene glycol monomethyl ether and ethylene glycol hexyl ether. The ether solvent is preferably ethylene glycol butyl ether (CAS NO.111-76-2) under the action of a diluent, and can be used for well dissolving polyester resin and conductive carbon black when being compounded with isophorone.
Preferably, the silicone-based auxiliary agent is methylphenyldimethylsilicone. The silicone auxiliary agent plays a role of a leveling agent and a dispersing agent, and can inhibit and break bubbles in the ink construction process, reduce the surface tension of the ink film of the image layer, improve the leveling of the ink and promote the leveling effect of the printing of the conductive ink.
Preferably, the surface resistance of the conductive carbon paste for the mobile blood glucose test piece is 1.4k omega-1.5 k omega. The resistance of the conductive ink pattern tested by the four-probe resistance tester for the conductive carbon paste prepared in the embodiment of the application is 1.4-1.5 kilo-ohm, and is more than 5 times lower than the resistance of the current commercially available conductive carbon paste, so that the requirement of low sheet resistance of the printed conductive circuit on the mobile blood glucose test piece product can be met, and the four-probe resistance tester for the conductive carbon paste has a good application prospect.
A preparation method of conductive carbon paste for a mobile blood glucose test piece comprises the following steps:
(1) uniformly mixing polyester resin, a ketone solvent, an ether solvent and a silicone auxiliary agent, and stirring at a high speed until the mixture is completely dissolved to obtain gloss oil;
(2) adding conductive carbon powder into gloss oil, stirring at a low speed, and uniformly mixing to obtain a mixture;
(3) and grinding the mixture with uniform mixture to obtain the product.
Preferably, in the step (1), the high-speed stirring is carried out at a stirring speed of 3000-10000 r/min for 60-100 min;
in the step (2), the low-speed stirring is carried out at a stirring speed of 300-1000 rpm for 30-80 minutes;
in the step (3), the grinding is to put the mixture into a three-roll grinder to grind for 3-5 times until the fineness is less than or equal to 10 um.
An application of the conductive carbon paste for the mobile blood glucose test piece in the mobile blood glucose test piece. The conductive carbon paste for the mobile blood glucose test piece is mainly applied to printing of conductive circuits on the mobile blood glucose test piece, the resistance of a conductive ink pattern tested by the four-probe resistance tester for the conductive carbon paste prepared in the specific embodiment is 1.4-1.5 kilo-ohm, the resistance is lower than that of the conductive carbon paste sold in the market by more than 5 times, the requirement of low sheet resistance of the conductive circuits printed on the mobile blood glucose test piece product can be met, and the conductive carbon paste has a good application prospect.
Compared with the prior art, the invention has the following advantages:
the application provides conductive carbon paste for a mobile blood sugar test piece, which consists of 18-25 wt% of polyester resin, 8-12 wt% of ketone solvent, 5-8 wt% of ether solvent, 1-3 wt% of silicone assistant and 57-62 wt% of conductive carbon black, gloss oil formed by blending the polyester resin, the ketone solvent, the ether solvent and the silicone assistant is compounded with the conductive carbon black, the conductive carbon black mainly plays a role of conductivity, the polyester resin is used for coating the conductive carbon black, the conductive carbon black is bonded into a film, the ketone solvent and the ether solvent are used for dissolving the polyester resin coated with the conductive carbon black, the silicone assistant is used for promoting the leveling effect of the printing of the conductive carbon paste ink, the conductive carbon paste has the resistance which is 5 times lower than that of the conductive carbon paste sold on the market at present, and has good adhesive force, and can meet the requirement of low square resistance of a printed conductive circuit on a mobile blood sugar test piece product, has good application prospect.
The preparation method of the conductive carbon paste for the mobile blood glucose test piece is simple to process and low in cost, the prepared conductive carbon paste has very low sheet resistance, the requirement of printing the conductive circuit on a mobile blood glucose test piece product on the low sheet resistance can be met, the conductive carbon paste of the embodiment of the application is stored for 2 months and then an oil layer is observed, the conductive carbon paste is free of layering phenomenon, can be completely cured at 80-90 ℃, is low in drying temperature, and can meet the use requirement of the mobile blood glucose test piece.
The application of the conductive carbon paste for the mobile blood glucose test piece is mainly the application of printing a conductive circuit on the mobile blood glucose test piece, the resistance of a conductive ink pattern tested by a four-probe resistance tester for the conductive carbon paste prepared in the embodiment is 1.4-1.5 kilo-ohm, the resistance is 5 times lower than that of the current commercially available conductive carbon paste, the requirement of low sheet resistance of the printed conductive circuit on the mobile blood glucose test piece product can be met, a hundred-grid test is carried out by using a 3M 610 adhesive tape, and the adhesion of the conductive ink on a PET material is tested to be 5B.
Detailed Description
The following describes a specific embodiment of the present invention with reference to specific examples 1 to 4 and comparative examples:
example 1:
a preparation method of conductive carbon paste for a mobile blood glucose test piece comprises the following steps:
weighing the components according to the weight ratio in the table 1, uniformly mixing the polyester resin, the ketone solvent, the ether solvent and the silicone auxiliary agent, stirring at a high speed of 3000 r/min for 100 min until the components are completely dissolved to obtain varnish, adding the conductive carbon powder into the varnish, stirring at a low speed of 1000 r/min for 30min, uniformly mixing to obtain a mixture, uniformly grinding the mixture in a three-roll grinder for 3-5 times until the fineness is less than or equal to 10um, and thus obtaining the conductive silicone oil.
Example 2:
a preparation method of conductive carbon paste for a mobile blood glucose test piece comprises the following steps:
weighing the components according to the weight ratio in the table 1, uniformly mixing the polyester resin, the ketone solvent, the ether solvent and the silicone auxiliary agent, stirring at a high speed of 8000 rpm for 70 minutes until the components are completely dissolved to obtain varnish, adding the conductive carbon powder into the varnish, stirring at a low speed of 800 rpm for 50 minutes, uniformly mixing to obtain a mixture, uniformly grinding the mixture in a three-roll grinder for 3-5 times until the fineness is less than or equal to 10 microns, and thus obtaining the conductive silicone oil.
Example 3:
a preparation method of conductive carbon paste for a mobile blood glucose test piece comprises the following steps:
weighing the components according to the weight ratio in the table 1, uniformly mixing the polyester resin, the ketone solvent, the ether solvent and the silicone auxiliary agent, stirring at a high speed of 10000 r/min for 60 minutes until the components are completely dissolved to obtain varnish, adding the conductive carbon powder into the varnish, stirring at a low speed of 300 r/min for 80 minutes, uniformly mixing to obtain a mixture, uniformly grinding the mixture in a three-roll grinder for 3-5 times until the fineness is less than or equal to 10 microns, and thus obtaining the conductive silicone oil.
Example 4:
a preparation method of conductive carbon paste for a mobile blood glucose test piece comprises the following steps:
weighing the components according to the weight ratio in the table 1, uniformly mixing the polyester resin, the ketone solvent, the ether solvent and the silicone auxiliary agent, stirring at a high speed of 5000 r/min for 90 minutes until the components are completely dissolved to obtain varnish, adding the conductive carbon powder into the varnish, stirring at a low speed of 600 r/min for 60 minutes, uniformly mixing to obtain a mixture, uniformly grinding the mixture in a three-roll grinder for 3-5 times until the fineness is less than or equal to 10 microns, and thus obtaining the conductive silicone oil.
Table 1: example 1-4 weight ratio of conductive carbon paste for Mobile blood glucose test piece
Figure BDA0002819225890000071
Comparative example 1: conductive carbon paste available from Acheson corporation under the model number ED581 ss;
comparative example 2: conductive carbon paste manufactured by LOCTITE EDAG, model 965 SS;
comparative example 3: tengchang company, model FC-451.
The conductive carbon pastes prepared in examples 1 to 4 and commercially available conductive carbon pastes were subjected to performance comparison tests, and the performance test methods and items were as follows:
the conductive carbon paste prepared in the examples 1 to 4 and the conductive carbon paste of the commercial conductive carbon paste comparative examples 1 to 3 were printed with conductive ink patterns onto a PET film by a screen printer, the PET film printed with the conductive patterns was placed in an oven and baked at 80 ℃ for 30min, using a 200-mesh polyester-nylon composite screen as the printing screen. After being taken out and cooled, the resistance of the conductive ink pattern was measured by a four-probe resistance tester, and the adhesion of the conductive ink to the PET material was measured by a hundred grid test using 3M 610 tape, with the test results shown in table 2.
Table 2: results of Performance testing
Figure BDA0002819225890000081
From the experimental test results, the resistance of the conductive ink pattern tested by the four-probe resistance tester for the conductive carbon paste prepared in the embodiment of the application is 1.4 kilo-ohm to 1.5 kilo-ohm, which is 5 times lower than the resistance of the current commercially available conductive carbon paste. A hundred-grid test is carried out on the 3M 610 adhesive tape, and the adhesion force of the conductive ink on the PET material is 5B, which shows that the conductive ink has good adhesion force as the conductive carbon paste sold in the market. Can be completely cured at 80-90 ℃ and has low drying temperature. And the conductive carbon paste of the embodiment of the application is stored for 2 months, and then an oil layer is observed, and no layering phenomenon exists.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (10)

1. The conductive carbon paste for the mobile blood glucose test piece is characterized by comprising the following components: 18-25 wt% of polyester resin, 8-12 wt% of ketone solvent, 5-8 wt% of ether solvent, 1-3 wt% of silicone additive and 57-62 wt% of conductive carbon black.
2. The conductive carbon paste for a mobile blood glucose test strip according to claim 1, wherein: the polyester resin has a glass transition temperature (Tg) of 60-100 ℃ and an average molecular weight of 8000-20000.
3. The conductive carbon paste for a mobile blood glucose test strip according to claim 1, wherein: the conductive carbon black has a particle size of 10 to 100nm and an oil absorption value of 160 to 200ml/100 g.
4. The conductive carbon paste for a mobile blood glucose test strip according to claim 1, wherein: the ketone solvent is one or more of isophorone, methyl isobutyl ketone and cyclohexanone.
5. The conductive carbon paste for a mobile blood glucose test strip according to claim 1, wherein: the ether solvent is one or more of ethylene glycol butyl ether, ethylene glycol monomethyl ether and ethylene glycol hexyl ether.
6. The conductive carbon paste for a mobile blood glucose test strip according to claim 1, wherein: the silicone assistant is methyl phenyl dimethyl silicone.
7. The conductive carbon paste for a mobile blood glucose test strip according to claim 1, wherein: the surface resistance of the conductive carbon paste for the mobile blood glucose test piece is 1.4k omega-1.5 k omega.
8. A preparation method of conductive carbon paste for a mobile blood glucose test piece is characterized by comprising the following steps:
(1) uniformly mixing polyester resin, a ketone solvent, an ether solvent and a silicone auxiliary agent, and stirring at a high speed until the mixture is completely dissolved to obtain gloss oil;
(2) adding conductive carbon powder into gloss oil, stirring at a low speed, and uniformly mixing to obtain a mixture;
(3) and grinding the mixture with uniform mixture to obtain the product.
9. The method for preparing conductive carbon paste for a mobile blood glucose test strip according to claim 8, wherein the method comprises the following steps: in the step (1), the high-speed stirring is carried out at a stirring speed of 3000-10000 rpm for 60-100 minutes;
in the step (2), the low-speed stirring is carried out at a stirring speed of 300-1000 rpm for 30-80 minutes;
in the step (3), the grinding is to put the mixture into a three-roll grinder to grind for 3-5 times until the fineness is less than or equal to 10 um.
10. Use of the conductive carbon paste for a mobile blood glucose test strip according to any one of claims 1 to 8 in a mobile blood glucose test strip.
CN202011409065.3A 2020-12-06 2020-12-06 Conductive carbon slurry for mobile blood glucose test piece and preparation method and application thereof Pending CN112521803A (en)

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CN113773687A (en) * 2021-06-28 2021-12-10 浙江兴顺新材料科技有限公司 Noctilucent powder coating
RU2810995C1 (en) * 2023-04-04 2024-01-09 Общество с ограниченной ответственностью "Компания ЭЛТА" Carbon conductive paste for screen printing

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