CN109959783B - Sample injection adhesive tape and preparation method thereof - Google Patents
Sample injection adhesive tape and preparation method thereof Download PDFInfo
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- CN109959783B CN109959783B CN201910256949.0A CN201910256949A CN109959783B CN 109959783 B CN109959783 B CN 109959783B CN 201910256949 A CN201910256949 A CN 201910256949A CN 109959783 B CN109959783 B CN 109959783B
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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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
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- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
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- G01N33/531—Production of immunochemical test materials
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
- G01N33/531—Production of immunochemical test materials
- G01N33/532—Production of labelled immunochemicals
- G01N33/533—Production of labelled immunochemicals with fluorescent label
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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Abstract
The invention relates to a sample injection adhesive tape and a preparation method thereof, wherein the sample injection adhesive tape comprises a base material layer, an adhesive layer, a non-woven fabric layer and a buffer solution layer which are sequentially attached, the adhesive layer is a special acrylate polymer capable of resisting acid and alkali solution, and the buffer solution layer comprises at least one of phosphate, carbonate, borate, organic acid and Tris buffer solution. The preparation method of the sample injection adhesive tape comprises the following steps: and coating the adhesive layer on the substrate layer, drying, attaching the non-woven fabric layer, dipping and coating the buffer solution on the non-woven fabric layer by using a coating machine, and drying at 80-100 ℃ for 5-10 min to obtain the required sample injection adhesive tape. Compared with the prior art, the invention has the advantages that: the sampling device has a stable and reliable sampling effect, reduces the processing procedures of a client, and is convenient for realizing automatic production.
Description
Technical Field
The invention relates to the technical field of immunochromatography, in particular to a sample injection adhesive tape and a preparation method thereof.
Background
In Vitro Diagnostics (IVD) refers to products and services that obtain clinical diagnostic information by detecting samples (blood, body fluids, tissues, etc.) of the human body, outside the human body. The in vitro diagnosis product is widely applied to each clinical stage and runs through the whole process of disease treatment such as primary diagnosis, treatment scheme selection, effectiveness evaluation, confirmed diagnosis and cure and the like. Currently, around 80% of clinical diagnostic information comes from in vitro diagnosis, called "doctor's eye".
The in vitro diagnosis is classified into various types, such as biochemical diagnosis, immunodiagnosis, molecular diagnosis, bedside diagnosis, blood detection, cell detection, microbial detection, urine detection, blood coagulation diagnosis, and flow cytometry, according to the detection principle or detection method. At present, biochemical, immune and molecular diagnostic reagents are three main types of diagnostic reagents in China.
The test paper based on the immunochromatographic technology comprises a sample injection pad/a conjugate release pad/a chromatographic membrane/an absorption pad/a bottom plate, for example, the invention patent of fluorescence immunochromatographic test paper strip and reagent card with the patent application number of CN201810491770.9 (with the publication number of CN108918865A) discloses a fluorescence immunochromatographic test paper strip which comprises a bottom plate, wherein a sample pad, a fluorescence pad, a nitrocellulose membrane and a sample absorption pad are sequentially arranged on the bottom plate along the length direction of the bottom plate; the sample pad is partially overlapped with the fluorescent pad, the fluorescent pad is partially overlapped with the nitrocellulose membrane, one side edge of the fluorescent pad is positioned below the sample pad, and the other opposite side edge of the fluorescent pad is positioned above one side edge of the nitrocellulose membrane; the nitrocellulose membrane is partially overlapped with the sample absorbing pad, and the other opposite side edge of the nitrocellulose membrane is positioned below the sample absorbing pad; the nitrocellulose membrane is provided with a detection line and a quality control line, and the detection line is close to the fluorescent pad; the sample pad is treated by the sample pad treatment solution, and the sample pad treatment solution contains 0.1-0.5% of bromocresol green ethanol solution with the concentration of 10%, so that the detection sensitivity is high, and the detection efficiency and the accuracy are high.
The sample injection part except the chromatographic membrane in the test paper containing the fluorescence immunochromatographic test strip is generally prepared by adopting the traditional process, plays a role in transmitting liquid in the whole test process and avoids influencing the liquid. Most of the traditional processes are bottom plate adhesive film or double-sided adhesive tape and then all parts processed by biological reagent are bonded together step by step, or all parts are processed by biological reagent after being bonded, so that the parts are bonded piece by piece, the processes are complicated and the processing cost is high.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a sample introduction adhesive tape which has stable and reliable sample introduction effect, simple processing procedure and convenient realization of automatic production aiming at the current situation of the prior art.
The second technical problem to be solved by the invention is to provide a preparation method of the sample injection adhesive tape.
The technical scheme adopted by the invention for solving the first technical problem is as follows: a sample injection adhesive tape is characterized in that: including substrate layer, glue film, non-woven fabrics layer and the buffer solution layer of laminating in proper order, the glue film is but acid and alkali resistance's special acrylic ester polymer, the buffer solution layer includes at least one in phosphate, carbonate, borate, organic acid, the Tris buffer solution.
Preferably, the buffer solution further comprises a surfactant.
The technical scheme adopted by the invention for solving the second technical problem is as follows: the preparation method of the sample injection adhesive tape is characterized by comprising the following steps of: and coating the adhesive layer on the substrate layer, drying, attaching the non-woven fabric layer, dipping and coating the buffer solution on the non-woven fabric layer by using a coating machine, and drying at 80-100 ℃ for 5-10 min to obtain the required sample injection adhesive tape.
Preferably, the adhesive layer is prepared from the following raw materials in parts by mass:
acrylate Polymer 100 parts by weight
0.01 to 0.5 part by mass of a crosslinking agent.
Further, the preparation method of the adhesive layer comprises the following steps:
(1) mixing 60-80 parts of isooctyl acrylate, 10-30 parts of butyl acrylate, 0.5-3 parts of acrylic acid, 0.5-2 parts of hydroxyethyl acrylate, 0.5-5 parts of long-chain acrylate monomer and 0.05-1.0 part of molecular weight regulator with 50-100 parts of ethyl acetate, stirring for 1hr under the protection of nitrogen, heating to 70 ℃, gradually adding 0.01-0.5 part of initiator to react for 4hr, and then adding 50-80 parts of ethyl acetate to dilute and cool to obtain the required acrylate polymer;
(2) and (2) mixing the acrylate polymer obtained in the step (1) with a cross-linking agent according to a mass part ratio to obtain the required adhesive layer.
And further, the weight average molecular weight of the acrylate polymer in the step (1) is 60-100W, the solid content is 35-45%, and the viscosity is 6000-10000 cps.
Still further, in the above-mentioned patent document,
the long-chain acrylate monomer is at least one of lauryl acrylate and octadecyl acrylate and is used for increasing the water resistance and the alcohol resistance;
the molecular weight is adjusted to be at least one of dodecyl mercaptan and methyl styrene linear dimer, and the solvent does not contain benzene, so that the reaction is easy to be too fast, the molecular weight distribution is too wide, and the reaction rhythm can be controlled by the molecular weight regulator;
the initiator is at least one of dimethyl azodiisobutyrate, azodiisobutyronitrile, azodiisoheptonitrile, cumene hydroperoxide and tert-butyl hydroperoxide;
the cross-linking agent is at least one of an epoxy cross-linking agent and a metal chelate.
Preferably, the non-woven fabric layer is composed of the following raw materials in percentage by mass:
60 to 80 percent of viscose
15-35% of polyester fiber
5-10% of sea-island fiber.
Further, in the present invention, it is preferable that,
the viscose is at least one of viscose cotton type short fiber, viscose wool type short fiber, strong viscose fiber, rich strong fiber, high-crimp high-wet modulus viscose fiber and modified viscose fiber; the viscose fiber is subjected to physical and chemical reactions for many times in the manufacturing process to crack cellulose macromolecular groups, so that the macromolecules of the viscose fiber are shortened, the molecular gaps are large, the arrangement is loose and disordered, the polarity of hydroxyl (-OH) in the molecules is good, and a large amount of hydroxyl (-OH) contained in the viscose fiber can adsorb a large amount of water molecules or other molecules, so that the viscose fiber provides good moisture absorption;
the polyester fiber is at least one of polyethylene terephthalate fiber, polybutylene terephthalate fiber, polytrimethylene terephthalate fiber, poly-1, 4-cyclohexanedimethylester terephthalate fiber, poly-2, 6-naphthalenedicarboxylate fiber and modified polyester fiber; because the rigidity of macromolecular chains of the polyester fibers is higher, the elastic modulus of the polyester fibers is high, the fibers are not easy to deform, and the processed fabric has higher strength and elastic recovery capability and good chemical resistance;
the sea-island fiber is a water-soluble modified polyester/polyamide composite fiber; the sea-island fiber fabric not only has the characteristics of non-ironing property, good size stability, small shrinkage rate and the like of synthetic fibers, but also has the advantages of good drapability, moisture absorption, moisture permeability and the like of natural fibers, and the sea-island fiber fabric has large specific surface area and more gaps and can endow the fabric with good filterability.
Further, the preparation method of the non-woven fabric layer comprises the following steps: grabbing the viscose fibers, the polyester fibers and the sea-island fibers according to the mass percentage by using a weighing machine, winding the fibers according to a spunlace process, splitting by an alkali-reducing method, washing by deionized water, and finally drying and rolling to obtain the required non-woven fabric layer.
Further, the gram weight of the cloth layer is 40-80 g/m2The water absorption capacity is 300 to 600g/m2The water absorption rate is 1-3 s/35mm, the tensile strength is 2-5 Kg/15mm, and the ion content is less than 5000 ppm.
Compared with the prior art, the invention has the advantages that: the utility model provides an integrated into one piece's advance kind sticky tape, including the substrate layer, glue film, non-woven fabrics layer and the buffer solution layer of laminating in proper order, this advance kind sticky tape has certain filter effect to test liquid to can provide a stable pH environment, have reliable and stable kind effect, its sample inlet volume and feed liquor time control are in certain extent, can leave the use of inhaling appearance pad in some test paper strip designs, have reduced customer end manufacturing procedure, are convenient for realize automated production.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
(1) mixing 80 parts of isooctyl acrylate, 10 parts of butyl acrylate, 3 parts of acrylic acid, 1.5 parts of hydroxyethyl acrylate, 3 parts of lauryl acrylate and 0.05 part of dodecyl mercaptan by mass with 100 parts of ethyl acetate, stirring for 1hr under the protection of nitrogen, heating to 70 ℃, gradually adding 0.05 part of azobisisobutyronitrile for reaction for 4hr, adding 70 parts of ethyl acetate for dilution and cooling to obtain an acrylate polymer with the weight-average molecular weight of 80W, the solid content of 37% and the viscosity of 8000 cps;
(2) grabbing 80 parts by mass of viscose fibers, 15 parts by mass of polyester fibers and 5 parts by mass of water-soluble modified polyester/polyamide composite fibers by using a weighing machine, carrying out fiber winding according to a spunlace process, splitting by using an alkali reduction method, washing by using deionized water, and finally drying and winding; the gram weight obtained is 70g/m2The spunlace nonwoven fabric has the tensile strength of 3.3Kg/15mm and the ion content of less than 5000 ppm;
(3) taking 100g of the acrylic ester polymer, adding 0.025g E-100C crosslinking agent, uniformly mixing, coating on a PET substrate layer with the thickness of 175 micrometers by using a scraper type coating device, coating the PET substrate layer with the thickness of 30 micrometers, drying, and attaching a non-woven fabric layer;
(4) dipping and coating a Tris-HCl buffer solution (pH8.5) on the non-woven fabric surface of the composite material by a scraper type coating device, and drying at 90 ℃ for 10min to obtain the sample injection adhesive tape finally treated by the buffer solution.
Example 2:
(1) mixing 60 parts of isooctyl acrylate, 30 parts of butyl acrylate, 0.5 part of acrylic acid, 2 parts of hydroxyethyl acrylate, 5 parts of octadecyl acrylate and 1.0 part of methyl styrene linear dimer with 50 parts of ethyl acetate, stirring for 1hr under the protection of nitrogen, heating to 70 ℃, gradually adding 0.12 part of dimethyl azodiisobutyrate for reaction for 4hr, adding 80 parts of ethyl acetate for dilution and cooling to obtain an acrylate polymer with the weight-average molecular weight of 60W, the solid content of 45% and the viscosity of 10000 cps;
(2) grabbing 60 parts by mass of viscose fibers, 35 parts by mass of polyester fibers and 5 parts by mass of water-soluble modified polyester/polyamide composite fibers by using a weighing machine, carrying out fiber winding according to a spunlace process, splitting by using an alkali reduction method, washing by using deionized water, and finally drying and winding; the gram weight of the obtained product is 40g/m2The spun-laced non-woven fabric has the tensile strength of 2.1Kg/15mm and the ion content of less than 5000 ppm;
(3) taking 100g of the acrylate polymer, adding 0.1g of an aluminum acetylacetonate crosslinking agent, uniformly mixing, coating the mixture on a PS (polystyrene) base material layer with the thickness of 500 micrometers by using scraper type coating equipment, coating the PS base material layer with the thickness of 35 micrometers, drying and attaching a non-woven fabric layer;
(4) and dipping and coating a non-woven fabric surface of the composite material with Tris-HCl buffer solution (pH8.5) by a scraper type coating device, and drying at 95 ℃ for 8min to obtain the sample injection adhesive tape treated by the buffer solution finally.
Example 3:
(1) mixing 70 parts of isooctyl acrylate, 20 parts of butyl acrylate, 2 parts of acrylic acid, 0.5 part of hydroxyethyl acrylate, 0.5 part of lauryl acrylate and 0.5 part of dodecyl mercaptan agent with 70 parts of ethyl acetate, stirring under the protection of nitrogen for 1 hour, heating to 70 ℃, gradually adding 0.01 part of azobisisoheptonitrile for reacting for 4 hours, adding 80 parts of ethyl acetate for diluting and cooling to obtain an acrylate polymer with the weight-average molecular weight of 70W, the solid content of 38% and the viscosity of 7000 cps;
(2) grabbing 70 parts by mass of viscose, 20 parts by mass of polyester fiber and 10 parts by mass of water-soluble modified polyester/polyamide composite fiber by using a weighing machine, performing fiber winding according to a spunlace process, splitting by using an alkali reduction method, washing by using deionized water, and finally drying and rolling; the gram weight of the obtained product is 60g/m2The spunlace nonwoven fabric has the tensile strength of 2.3Kg/15mm and the ion content of less than 5000 ppm;
(3) taking 100g of the acrylate polymer, adding 0.04g E-AX crosslinking agent, uniformly mixing, coating the mixture on a PET substrate layer with the thickness of 50 microns by a scraper type coating device, coating the coating with the thickness of 15 microns, drying, and attaching a non-woven fabric layer;
(4) and (3) dipping and coating a sodium dihydrogen phosphate-disodium hydrogen phosphate buffer solution (pH6.5) on the non-woven fabric surface of the composite material by a scraper type coating device, and drying at 100 ℃ for 5min to obtain the sample injection adhesive tape treated by the buffer solution finally.
Example 4:
(1) mixing 75 parts of isooctyl acrylate, 15 parts of butyl acrylate, 1.5 parts of acrylic acid, 1 part of hydroxyethyl acrylate, 2.5 parts of octadecyl acrylate and 0.3 part of dodecyl mercaptan by mass with 100 parts of ethyl acetate, stirring for 1 hour under the protection of nitrogen, heating to 70 ℃, gradually adding 0.2 part of dimethyl azodiisobutyrate to react for 4 hours, adding 80 parts of ethyl acetate to dilute and cool, and obtaining an acrylate polymer with the weight-average molecular weight of 100W, the solid content of 35 percent and the viscosity of 6000 cps;
(2) grabbing 60 parts by mass of viscose fibers, 33 parts by mass of polyester fibers and 7 parts by mass of water-soluble modified polyester/polyamide composite fibers by using a weighing machine, carrying out fiber winding according to a spunlace process, splitting by using an alkali reduction method, washing by using deionized water, and finally drying and winding; the gram weight obtained is 80g/m2The spunlace nonwoven fabric has the tensile strength of 4.5Kg/15mm and the ion content of less than 5000 ppm;
(3) taking 100g of the acrylate polymer, adding 0.3g of an aluminum acetylacetonate crosslinking agent, uniformly mixing, coating the mixture on a PET (polyethylene terephthalate) base material layer with the thickness of 200 micrometers by using scraper type coating equipment, coating the coating with the thickness of 25 micrometers, drying and attaching a non-woven fabric layer;
(4) and (3) dipping and coating a sodium dihydrogen phosphate-disodium hydrogen phosphate buffer solution (pH6.5) on the non-woven fabric surface of the composite material by a scraper type coating device, and drying at 90 ℃ for 7min to obtain the sample injection adhesive tape treated by the buffer solution finally.
Example 5:
(1) mixing 70 parts of isooctyl acrylate, 20 parts of butyl acrylate, 2 parts of acrylic acid, 1.2 parts of hydroxyethyl acrylate, 2 parts of long-chain acrylate monomer and 0.2 part of dodecyl mercaptan by mass with 100 parts of ethyl acetate, stirring for 1hr under the protection of nitrogen, heating to 70 ℃, gradually adding 0.1 part of tert-butyl cumyl peroxide by mass, reacting for 4hr, adding 50 parts of ethyl acetate, diluting and cooling to obtain an acrylate polymer with the weight-average molecular weight of 80W, the solid content of 39% and the viscosity of 8000 cps;
(2) grabbing 70 parts by mass of viscose, 25 parts by mass of polyester fiber and 5 parts by mass of water-soluble modified polyester/polyamide composite fiber by using a weighing machine, performing fiber winding according to a spunlace process, splitting by using an alkali reduction method, washing by using deionized water, and finally drying and rolling; the gram weight obtained is 70g/m2The spun-laced non-woven fabric has the tensile strength of 2.7Kg/15mm and the ion content of less than 5000 ppm;
(3) taking 100g of the acrylate polymer, adding 0.01g E-100C crosslinking agent, uniformly mixing, coating on a PVC base material layer with the thickness of 250 micrometers by using a scraper type coating device, coating the PVC base material layer with the thickness of 25 micrometers, drying, and attaching a non-woven fabric layer;
(4) and (3) dipping and coating boric acid-borax buffer solution (pH7.8) on the non-woven fabric surface of the composite material by a scraper type coating device, and drying at 95 ℃ for 7min to obtain the sample injection adhesive tape treated by the buffer solution finally.
Example 6:
(1) mixing 60 parts of isooctyl acrylate, 10 parts of butyl acrylate, 1.5 parts of acrylic acid, 1 part of hydroxyethyl acrylate, 1 part of lauryl acrylate and 0.1 part of dodecyl mercaptan by mass with 80 parts of ethyl acetate, stirring for 1hr under the protection of nitrogen, heating to 70 ℃, gradually adding 0.5 part of tert-butyl hydroperoxide by mass, reacting for 4hr, adding 50 parts of ethyl acetate, diluting and cooling to obtain an acrylate polymer with the weight-average molecular weight of 90W, the solid content of 36% and the viscosity of 7000 cps;
(2) grabbing 70 parts by mass of viscose, 25 parts by mass of polyester fiber and 7 parts by mass of water-soluble modified polyester/polyamide composite fiber by using a weighing machine, performing fiber winding according to a spunlace process, splitting by using an alkali reduction method, washing by using deionized water, and finally drying and rolling; the gram weight of the obtained product is 60g/m2Spunlace nonwoven fabric with tensile strength of 3.0Kg/15mm and ion content of less than 5000 ppm;
(3) taking 100g of the acrylate polymer, adding 0.5g of copper acetylacetonate crosslinking agent, uniformly mixing, coating the mixture on a PET (polyethylene terephthalate) base material layer with the thickness of 175 micrometers by a scraper type coating device, coating the coating with the thickness of 50 micrometers, drying and attaching a non-woven fabric layer;
(4) and (3) dipping and coating citric acid-sodium citrate buffer solution (pH6.6) on the non-woven fabric surface of the composite material by a scraper type coating device, and drying at 85 ℃ for 9min to obtain the sample injection adhesive tape treated by the buffer solution finally.
Example 7:
(1) mixing 80 parts of isooctyl acrylate, 10 parts of butyl acrylate, 0.5 part of acrylic acid, 2 parts of hydroxyethyl acrylate, 1.5 parts of octadecyl acrylate and 0.7 part of methyl styrene linear dimer with 80 parts of ethyl acetate, stirring under the protection of nitrogen for 1 hour, heating to 70 ℃, gradually adding 0.3 part of dimethyl azodiisobutyrate initiator, reacting for 4 hours, adding 80 parts of ethyl acetate, diluting and cooling to obtain an acrylate polymer with the weight-average molecular weight of 90W, the solid content of 37 percent and the viscosity of 7000 cps;
(2) grabbing 60 parts by mass of viscose, 30 parts by mass of polyester fiber and 10 parts by mass of water-soluble modified polyester/polyamide composite fiber by using a weighing machine, performing fiber winding according to a spunlace process, splitting by using an alkali reduction method, washing by using deionized water, and finally drying and rolling; the gram weight of 50g/m is obtained2The spunlace nonwoven fabric has the tensile strength of 2.7Kg/15mm and the ion content of less than 5000 ppm;
(3) taking 100g of the acrylate polymer, adding 0.05g of an aluminum acetylacetonate crosslinking agent, uniformly mixing, coating the mixture on a PC base material layer with the thickness of 200 micrometers by using scraper type coating equipment, coating the coating with the thickness of 25 micrometers, drying and attaching a non-woven fabric layer;
(4) dipping and coating a Tris-HCl buffer solution (pH8.0) on the non-woven fabric surface of the composite material by a scraper type coating device, and drying for 10min at 90 ℃ to obtain the sample injection adhesive tape finally treated by the buffer solution.
Example 8:
(1) mixing 70 parts of isooctyl acrylate, 20 parts of butyl acrylate, 2 parts of acrylic acid, 1.5 parts of hydroxyethyl acrylate, 2 parts of octadecyl acrylate and 0.3 part of methyl styrene linear dimer with 70 parts of ethyl acetate, stirring for 1 hour under the protection of nitrogen, heating to 70 ℃, gradually adding 0.1 part of dimethyl azodiisobutyrate initiator for reaction for 4 hours, adding 80 parts of ethyl acetate for dilution and cooling to obtain the acrylate polymer with the weight-average molecular weight of 80W, the solid content of 39% and the viscosity of 8000 cps.
(2) Grabbing 65 parts by mass of viscose, 30 parts by mass of polyester fiber and 5 parts by mass of water-soluble modified polyester/polyamide composite fiber by using a weighing machine, carrying out fiber winding according to a spunlace process, splitting by using an alkali reduction method, and removingRinsing with son water, and finally drying and rolling; the gram weight of the obtained product is 60g/m2Spunlace nonwoven fabric with tensile strength of 3.5Kg/15mm and ion content of less than 5000 ppm;
(3) taking 100g of the acrylate polymer, adding 0.25g of an aluminum acetylacetonate crosslinking agent, uniformly mixing, coating the mixture on a PMMA substrate layer with the thickness of 200 microns by scraper type coating equipment, coating the coating with the thickness of 30 microns, and attaching a non-woven fabric layer after drying;
(4) and (3) dipping and coating a PBS buffer solution (pH7.2) on the non-woven fabric surface of the composite material by a scraper type coating device, and drying for 8min at 85 ℃ to obtain the sample injection adhesive tape treated by the buffer solution finally.
Comparative example 1:
(1) mixing 20 parts of isooctyl acrylate, 70 parts of butyl acrylate, 5 parts of acrylic acid and 50 parts of ethyl acetate, stirring for 1hr under the protection of nitrogen, heating to 75 ℃, gradually adding 0.15 part of azobisisobutyronitrile initiator for reaction for 4hr, adding 80 parts of ethyl acetate for dilution and cooling to obtain an acrylate polymer with the weight-average molecular weight of 45W, the solid content of 43% and the viscosity of 12000 cps;
(2) grabbing 65 parts by mass of viscose, 30 parts by mass of polyester fiber and 5 parts by mass of water-soluble modified polyester/polyamide composite fiber by using a weighing machine, performing fiber winding according to a spunlace process, splitting by using an alkali reduction method, washing by using deionized water, and finally drying and rolling; the gram weight of 50g/m is obtained2The tensile strength is 2.4Kg/15 mm; a spunlace nonwoven fabric with an ion content of less than 5000 ppm;
(3) taking 100g of the acrylate polymer and 1.2g of polymethylene phenyl polyisocyanate crosslinking agent, uniformly mixing, coating the mixture on a PET (polyethylene terephthalate) base material layer with the thickness of 175 micrometers by using scraper type coating equipment, wherein the coating thickness is 25 micrometers, and bonding a non-woven fabric layer after drying;
(4) dipping and coating a Tris buffer solution (pH8.5) on the non-woven fabric surface of the composite material by a scraper type coating device, and drying at 85 ℃ for 8min to obtain the sample injection adhesive tape treated by the buffer solution finally.
Comparative example 2:
(1) mixing 80 parts of isooctyl acrylate, 10 parts of butyl acrylate, 3 parts of acrylic acid, 1.5 parts of hydroxyethyl acrylate, 3 parts of lauryl acrylate and 0.05 part of dodecyl mercaptan by mass with 100 parts of ethyl acetate, stirring for 1 hour under the protection of nitrogen, heating to 70 ℃, gradually adding 0.05 part of tert-butyl cumyl peroxide initiator by mass, reacting for 4 hours, adding 70 parts of ethyl acetate, diluting and cooling to obtain an acrylate polymer with the weight-average molecular weight of 80W, the solid content of 37% and the viscosity of 8000 cps;
(2) taking 100 parts by mass of polypropylene, melting, extruding and stretching the polypropylene to form filaments, laying the filaments into a net, fixing the net in a hot rolling mode, and finally slitting and rolling; the gram weight of the obtained product is 60g/m2Spun-bonded non-woven fabric with tensile strength of 2.7Kg/15 mm;
(3) taking 100g of the acrylate polymer, adding 0.025g of an aluminum acetylacetonate crosslinking agent, uniformly mixing, coating the mixture on a PS substrate layer with the thickness of 300 microns by scraper type coating equipment, wherein the coating thickness is 35 microns, and attaching a non-woven fabric layer after drying; and obtaining the final sample injection adhesive tape.
The results of the performance tests of all the above examples and comparative examples are shown in table 1.
Note: in table 1, the test methods for various properties of the adhesive tape are as follows:
(1) adhesive force: coating an acrylic polymer mixed with a curing agent on a 25-micron PET (polyethylene terephthalate) base material in a standard environment, cutting a formed adhesive tape into a sample with the width of 25mm and the length of 150mm, attaching the sample to a polished steel plate, rolling the sample for 3 times back and forth by using a 2kg rubber shaft, placing the sample for 20min, and peeling the sample at 180 degrees at the speed of 300mm/min by using a tensile testing machine;
(2) water absorption capacity: cutting the sample into 6 cm-5 cm specifications, placing the sample under constant temperature and humidity conditions for 24hr to test the weight increased when the sample completely absorbs saturated deionized water after reaching humidity regulation balance;
(3) diffusion speed: cutting the sample into a circle with a diameter of 35mm, placing the circle under the conditions of constant temperature and constant humidity for 24hr, and testing the time required for the sample to be completely wetted by deionized water in a single-hole no-pressure mode after the humidity is adjusted and balanced;
(4) coefficient of variation: combining the HCG standard sample with an NC membrane attached with an antibody into an early pregnancy test strip, testing the HCG standard sample by adopting a chemiluminescence immunoassay method, and calculating a Coefficient of Variation (CV) value aiming at a test value, namely: coefficient of Variation (CV) ═ standard deviation (σ)/mean (μ) × 100%. Since immunochromatography generally has no specific numerical value and a CV value cannot be calculated, a test was performed by a chemiluminescence immunoassay.
As can be seen from table 1:
(1) after the acrylate polymers in examples 1-8 were treated with acid-base buffer solutions, the adhesion performance remained comparable to the initial stage, and no hydrolysis or cohesive failure occurred; in comparative example 1, the polymer generated by the reaction is not resistant to acid and alkali buffer because the acrylic acid content in the monomer is high and long-chain acrylate monomers and molecular weight regulators are not used;
(2) the water absorption capacity and diffusion rate of the sample injection adhesive tape in the examples 1-8 are better than those of the comparative examples 1-2, so that sample injection is facilitated, and the non-woven fabric in the comparative example 1 has different component proportions, low viscose content and reduced water absorption and diffusion performance; in comparative example 2, the polypropylene material used in the hot rolling process had poor water absorption;
(3) through the formula verification of the embodiments 1 to 8, the amounts of the main monomer, the long-chain acrylate monomer, the initiator, the solvent and the hardening agent are adjusted within the following ranges (60 to 80 parts of isooctyl acrylate, 10 to 30 parts of butyl acrylate, 0.5 to 3 parts of acrylic acid, 0.5 to 2 parts of hydroxyethyl acrylate, 0.5 to 5 parts of long-chain acrylate monomer, 0.05 to 1.0 part of molecular weight regulator and 50 to 100 parts of ethyl acetate mixture), so that the results of small adhesive force change and small variation coefficient before and after buffer solution treatment can be obtained, and therefore, the sample injection adhesive tape has a stable and reliable sample injection effect.
TABLE 1 results of the Performance test of all examples and comparative examples
Claims (7)
1. A preparation method of a sample injection adhesive tape is characterized by comprising the following steps: the sample injection adhesive tape comprises a base material layer, an adhesive layer, a non-woven fabric layer and a buffer solution layer which are sequentially attached, wherein the adhesive layer is a special acrylate polymer capable of resisting acid and alkali solution, and the buffer solution layer comprises at least one of phosphate, carbonate, borate, organic acid and Tris buffer solution;
the preparation method of the sample injection adhesive tape comprises the following steps: coating the glue layer on the base material layer, drying, attaching the non-woven fabric layer, dipping and coating the non-woven fabric layer with a buffer solution by using a coating machine, and drying at 80-100 ℃ for 5-10 min to obtain the required sample injection adhesive tape;
the adhesive layer is prepared from the following raw materials in parts by mass:
acrylate Polymer 100 parts by weight
0.01 to 0.5 parts by mass of a crosslinking agent;
the preparation method of the adhesive layer comprises the following steps:
(1) mixing 60-80 parts of isooctyl acrylate, 10-30 parts of butyl acrylate, 0.5-3 parts of acrylic acid, 0.5-2 parts of hydroxyethyl acrylate, 0.5-5 parts of long-chain acrylate monomer and 0.05-1.0 part of molecular weight regulator with 50-100 parts of ethyl acetate, stirring for 1hr under the protection of nitrogen, heating to 70 ℃, gradually adding 0.01-0.5 part of initiator to react for 4hr, and then adding 50-80 parts of ethyl acetate to dilute and cool to obtain the required acrylate polymer;
(2) and (2) mixing the acrylate polymer obtained in the step (1) with a cross-linking agent according to the mass part ratio to obtain the required adhesive layer.
2. The production method according to claim 1, characterized in that: the weight-average molecular weight of the acrylate polymer in the step (1) is 60-100W, the solid content is 35-45%, and the viscosity is 6000-10000 cps.
3. The method of claim 1, wherein:
the long-chain acrylate monomer is at least one of lauryl acrylate and octadecyl acrylate;
the molecular weight is adjusted to be at least one of dodecyl mercaptan and methyl styrene linear dimer;
the initiator is at least one of dimethyl azodiisobutyrate, azodiisobutyronitrile, azodiisoheptonitrile, cumene hydroperoxide and tert-butyl hydroperoxide;
the cross-linking agent is at least one of an epoxy cross-linking agent and a metal chelate.
4. The preparation method of claim 1, wherein the non-woven fabric layer is prepared from the following raw materials in percentage by mass:
60 to 80 percent of viscose
15-35% of polyester fiber
5-10% of sea-island fiber.
5. The method of claim 4, wherein:
the viscose is at least one of viscose cotton type short fiber, viscose wool type short fiber, strong viscose fiber, rich strong fiber, high-crimp high-wet modulus viscose fiber and modified viscose fiber;
the polyester fiber is at least one of polyethylene terephthalate fiber, polybutylene terephthalate fiber, polytrimethylene terephthalate fiber, poly-1, 4-cyclohexanedimethylester terephthalate fiber, poly-2, 6-naphthalenedicarboxylate fiber and modified polyester fiber;
the sea-island fiber is a water-soluble modified polyester/polyamide composite fiber.
6. The method for preparing the nonwoven fabric layer according to any one of claims 4 to 5, wherein the method for preparing the nonwoven fabric layer comprises the following steps: grabbing the viscose fibers, the polyester fibers and the sea-island fibers according to the mass percentage by using a weighing machine, winding the fibers according to a spunlace process, splitting by an alkali-reducing method, washing by deionized water, and finally drying and rolling to obtain the required non-woven fabric layer.
7. The production method according to any one of claims 4 to 5, characterized in that: the gram weight of the non-woven fabric layer is 40-80 g/m2The water absorption capacity is 300 to 600g/m2The water absorption rate is 1-3 s/35mm, the tensile strength is 2-5 Kg/15mm, and the ion content is less than 5000 ppm.
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