CN109401690B - Water-based epoxy modified acrylate medical pressure-sensitive adhesive and preparation method thereof - Google Patents
Water-based epoxy modified acrylate medical pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09J133/24—Homopolymers or copolymers of amides or imides
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- 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09J133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
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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
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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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
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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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
- C08F220/1818—C13or longer chain (meth)acrylate, e.g. stearyl (meth)acrylate
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Abstract
The invention discloses a water-based epoxy modified acrylate medical pressure-sensitive adhesive and a preparation method thereof. The raw materials of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive comprise A, B two components in percentage by weight, wherein the component A comprises: 30-35% of soft monomer, 3-6% of functional monomer, 2-4% of crosslinking monomer, 60% of deionized water, and 0.2-0.5%, 0.4-1% and 0.4-0.8% of initiator, anionic emulsifier and nonionic emulsifier respectively based on the total mass of the soft monomer, the functional monomer and the crosslinking monomer; the component B is multifunctional epoxy resin and accounts for 0.5-3% of the total weight of the component A. The pressure-sensitive adhesive has the stripping force of 500-600g and low VOC, and the adhesive tape product has no fog residue after being stripped from the adhered surface, has no anaphylactic reaction when being adhered to skin, and can be used for fine protection in the medical process.
Description
Technical Field
The invention relates to the field of pressure-sensitive adhesives, in particular to a water-based epoxy modified acrylate medical pressure-sensitive adhesive and a preparation method thereof.
Background
The pressure-sensitive adhesive is a pressure-sensitive adhesive, is commonly called as adhesive sticker, is very convenient to bond, can be bonded by only slightly applying pressure or slightly pressing with fingers, and does not need large pressure, heating or solvent action in the process. Therefore, the adhesive has the largest use amount and the widest application range by the unique performance and characteristics, and products of the adhesive are distributed in various fields of packaging, automobiles, transportation, communication, electrical appliances, building materials, machinery, aviation, light industry, sanitation and the like. Compared with solvent-based pressure-sensitive adhesives, the water-based pressure-sensitive adhesive has the advantages of low VOC, environmental protection and simple production process, and is easy to polymerize into pressure-sensitive adhesives with higher molecular weight and stronger cohesive strength. Therefore, solvent-based pressure-sensitive adhesives are being gradually replaced in high-grade pressure-sensitive adhesive products.
The polyacrylate pressure-sensitive adhesive is the main product with the fastest development in pressure-sensitive adhesives due to the reasons of simple formula, wide bonding range, good weather resistance, strong light resistance, excellent oil resistance, good water resistance, good wettability, no phenomena of phase separation, migration and the like, convenient operation, low price and the like, and the product is widely applied to medical adhesive tapes. However, pressure-sensitive adhesives based on short-chain acrylate monomers have certain limitations on skin adhesion and insufficient cohesive strength in the molecule.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a water-based epoxy modified acrylate medical pressure-sensitive adhesive and a preparation method thereof.
The raw materials of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive comprise A, B two components in percentage by weight;
the component A comprises: 30-35% of soft monomer, 3-6% of functional monomer, 2-4% of crosslinking monomer, 60% of deionized water, and 0.2-0.5%, 0.4-1% and 0.4-0.8% of initiator, anionic emulsifier and nonionic emulsifier respectively based on the total weight of the soft monomer, the functional monomer and the crosslinking monomer;
the component B is multifunctional epoxy resin and accounts for 0.5-3% of the total weight of the component A.
Wherein the soft monomer is at least one of isodecyl methacrylate, isodecyl acrylate, stearic acid acrylate, butyl acrylate and isooctyl acrylate.
In addition, the functional monomer is itaconic acid.
In addition, the crosslinking monomer is at least one of N, N-methylene bisacrylamide, N-hydroxymethyl acrylamide and urea-formaldehyde ethyl methacrylate.
Further, the initiator is 2, 2-azobis (2-amidinopropane) dihydrochloride.
In addition, the anionic emulsifier is sodium lauryl sulfate.
In addition, the nonionic emulsifier is polyoxyethylene ether sorbitol hexastearate.
In addition, the multifunctional epoxy resin is one of 4, 5-epoxycyclohexane-1, 2-dicarboxylic acid diglycidyl ester, waterborne epoxy resin 6006-W-68A and waterborne epoxy resin 5003-W-55A.
The invention also provides a preferable waterborne epoxy modified acrylate medical pressure-sensitive adhesive, wherein the component A comprises the following raw materials in percentage by weight:
soft monomer: 20% of butyl acrylate and 12% of stearic acid acrylate;
functional monomer: 5% of itaconic acid;
crosslinking monomer: 3% of N, N-methylene bisacrylamide;
initiator: 2, 2-azobis (2-amidinopropane) dihydrochloride at 0.3% by weight based on the total weight of the soft monomers, functional monomers and crosslinking monomers;
anionic emulsifiers: sodium dodecyl sulfate accounting for 0.7 percent of the total weight of the soft monomer, the functional monomer and the crosslinking monomer;
non-ionic emulsifier: polyoxyethylene ether sorbitol hexastearate accounting for 0.6 percent of the total weight of the soft monomer, the functional monomer and the crosslinking monomer;
the raw material of the component B is waterborne epoxy resin 6006-W-68A accounting for 1.8% of the total weight of the component A.
The invention also provides a preparation method of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive, which comprises the following steps:
(1) weighing a soft monomer, a functional monomer, a crosslinking monomer, deionized water, an initiator, an anionic emulsifier, a nonionic emulsifier and multifunctional epoxy resin, uniformly stirring the anionic emulsifier, the nonionic emulsifier and 50-70% of deionized water, slowly dripping a mixture of the soft monomer, the functional monomer and the crosslinking monomer, and stirring at a high speed of 400r/min multiplied by 30min to prepare a pre-emulsion;
(2) uniformly stirring an initiator and 10-20% of deionized water to obtain an initiator aqueous solution;
(3) mixing the initiator aqueous solution with the concentration of 40-60% in the step (2) and the pre-emulsion with the concentration of 40-60% in the step (1) at 79-82 ℃, and reacting for 30-60min to obtain seed emulsion;
(4) uniformly mixing the residual initiator aqueous solution in the step (2), the residual pre-emulsion in the step (1) and the residual deionized water, dripping into the seed emulsion for 1.5-2.5h, preserving heat for 2h after dripping is finished, cooling and discharging to obtain a component A;
(5) and adding the raw material of the component B into the component A, and uniformly mixing to obtain the waterborne epoxy modified acrylate medical pressure-sensitive adhesive.
The invention solves the problems of low glass transition temperature and soft adhesive layer of the adhesive by the design of the main monomer formula, can fill rough surfaces such as lines of skin and the like, and improves the adhesive property of the skin and products. On the other hand, polyfunctional epoxy resin is introduced to react with carboxyl functional groups in itaconic acid on a molecular structure to form a dense network structure, so that insufficient cohesive strength caused by excessive softness of the adhesive is avoided. Therefore, the product not only has better initial adhesion, holding adhesion and adhesion retention, but also has the peel strength controlled at 500-600g, and the adhesive product has no mist residue after being peeled from the adhered surface and has no allergic reaction when being adhered to skin. The pressure-sensitive adhesive product can also be coated on PE, PU films and non-woven fabric substrates, and has wide applicability.
Detailed Description
The present invention will be further explained with reference to the following detailed description, which should be understood that the preferred embodiments described herein are only for the purpose of illustrating and explaining the present invention and are not to be construed as limiting the present invention.
The raw materials of the invention are all commercially available products. As an example, some materials in the present invention are of the following brand: the waterborne epoxy resin 6006-W-68A and the waterborne epoxy resin 5003-W-55A are respectively prepared from pickaxe charm chemical Co., Ltd, EPIKOTE-6006-W-68A and EPIKOTE-5003-W-55A; the 4, 5-epoxycyclohexane-1, 2-dicarboxylic acid diglycidyl ester adopts TDE-85 of Shandong Baihong New technology Co.
Example 1
(1) 15g of isooctyl acrylate, 15g of isodecyl methacrylate, 6g of itaconic acid, 4g of N-methylolacrylamide, 60g of deionized water, 0.2g of 2, 2-azobis (2-amidinopropane) dihydrochloride, 0.4g of sodium lauryl sulfate, 0.4g of polyoxyethylene ether sorbitol hexastearate and 0.5g of 4, 5-epoxycyclohexane-1, 2-dicarboxylic acid diglycidyl ester were weighed out.
Uniformly stirring 0.4g of sodium dodecyl sulfate, 0.4g of polyoxyethylene ether sorbitol hexastearate and 30g (50%) of deionized water, slowly dripping a mixture of 15g of isooctyl acrylate, 15g of isodecyl methacrylate, 6g of itaconic acid and 4g of N-hydroxymethyl acrylamide, and stirring at a high speed of 400r/min multiplied by 30min to prepare a pre-emulsion;
(2) 0.2g of 2, 2-azobis (2-amidinopropane) dihydrochloride and 6g (10%) of deionized water are stirred uniformly to obtain an initiator aqueous solution;
(3) mixing 2.48g (40%) of initiator aqueous solution in the step (2) with 28.32g (40%) of pre-emulsion in the step (1) at 79 ℃ for 30min to prepare seed emulsion;
(4) uniformly mixing the residual 3.72g of initiator aqueous solution in the step (2), the residual 42.48g of pre-emulsion in the step (1) and the residual 24g of deionized water, dripping into seed emulsion for 1.5h, preserving heat for 2h after finishing dripping, cooling and discharging to obtain a component A;
(5) and adding 0.5g of 4, 5-epoxycyclohexane-1, 2-dicarboxylic acid diglycidyl ester of the component B into the component A, and uniformly mixing to obtain the waterborne epoxy modified acrylate medical pressure-sensitive adhesive.
Example 2
(1) 20g of butyl acrylate, 15g of isodecyl acrylate, 3g of itaconic acid, 2g of urea-formaldehyde ethyl methacrylate, 60g of deionized water, 0.5g of 2, 2-azobis (2-amidinopropane) dihydrochloride, 1g of sodium lauryl sulfate, 0.8g of polyoxyethylene ether sorbitol hexastearate and 3g of 4, 5-epoxycyclohexane-1, 2-dicarboxylic acid diglycidyl ester were weighed out.
Uniformly stirring 1g of sodium dodecyl sulfate, 0.8g of polyoxyethylene ether sorbitol hexastearate and 42g (70%) of deionized water, slowly dripping a mixture of 20g of butyl acrylate, 15g of isodecyl acrylate, 3g of itaconic acid and 2g of urea-formaldehyde ethyl methacrylate, and stirring at a high speed of 400r/min multiplied by 30min to obtain a pre-emulsion;
(2) 0.5g of 2, 2-azobis (2-amidinopropane) dihydrochloride and 12g (20%) of deionized water are stirred uniformly to obtain an initiator aqueous solution;
(3) mixing 7.5g (60%) of initiator aqueous solution obtained in the step (2) with 50.28g (60%) of pre-emulsion obtained in the step (1) at 82 ℃ for 60min to obtain seed emulsion;
(4) uniformly mixing the 5g of initiator aqueous solution remained in the step (2), the 33.52g of pre-emulsion remained in the step (1) and the 6g of deionized water remained in the step (1), dripping into the seed emulsion for 2.5h, preserving heat for 2h after dripping is finished, cooling and discharging to obtain a component A;
(5) and 3g of 4, 5-epoxycyclohexane-1, 2-dicarboxylic acid diglycidyl ester of the component B is added into the component A and uniformly mixed to prepare the waterborne epoxy modified acrylate medical pressure-sensitive adhesive.
Example 3
(1) 20g of butyl acrylate, 12g of stearic acid acrylate, 5g of itaconic acid, 3g N, N-methylenebisacrylamide, 60g of deionized water, 0.3g of 2, 2-azobis (2-amidinopropane) dihydrochloride, 0.7g of sodium dodecyl sulfate, 0.6g of polyoxyethylene ether sorbitol hexastearate, and 1.8g of waterborne epoxy resin 6006-W-68A were weighed.
Uniformly stirring 0.7g of sodium dodecyl sulfate, 0.6g of polyoxyethylene ether sorbitol hexastearate and 36g (60%) of deionized water, slowly dripping a mixture of 20g of butyl acrylate, 12g of stearic acid acrylate, 5g of itaconic acid and 3g N, N-methylene bisacrylamide, and stirring at a high speed of 400r/min multiplied by 30min to prepare a pre-emulsion;
(2) 0.3g of 2, 2-azobis (2-amidinopropane) dihydrochloride and 9g (15%) of deionized water are stirred uniformly to obtain an initiator aqueous solution;
(3) mixing 4.65g (50%) of initiator aqueous solution obtained in the step (2) with 38.65g (50%) of pre-emulsion obtained in the step (1) at 80 ℃ for 45min to obtain seed emulsion;
(4) uniformly mixing the residual 4.65g of initiator aqueous solution in the step (2), the residual 38.65g of pre-emulsion in the step (1) and the residual 15g of deionized water, dripping into seed emulsion for 2 hours, preserving heat for 2 hours after dripping is finished, cooling and discharging to obtain a component A;
(5) and adding 1.8g of waterborne epoxy resin 6006-W-68A as the component B into the component A, and uniformly mixing to obtain the waterborne epoxy modified acrylate medical pressure-sensitive adhesive.
Example 4
(1) 35g of stearic acid acrylate, 3g of itaconic acid, 1g N, N-methylenebisacrylamide, 1g N-hydroxymethylacrylamide, 60g of deionized water, 0.2g of 2, 2-azobis (2-amidinopropane) dihydrochloride, 0.4g of sodium lauryl sulfate, 0.4g of polyoxyethylene ether sorbitol hexastearate and 0.5g of waterborne epoxy resin 5003-W-55A were weighed.
Uniformly stirring 0.4g of sodium dodecyl sulfate, 0.4g of polyoxyethylene ether sorbitol hexastearate and 30g (50%) of deionized water, slowly dripping a mixture of 35g of stearic acid acrylate, 3g of itaconic acid, 1g N, N-methylene bisacrylamide and 1g N-hydroxymethyl acrylamide, and stirring at a high speed of 400r/min multiplied by 30min to prepare a pre-emulsion;
(2) 0.2g of 2, 2-azobis (2-amidinopropane) dihydrochloride and 6g (10%) of deionized water are stirred uniformly to obtain an initiator aqueous solution;
(3) mixing 2.48g (40%) of initiator aqueous solution in the step (2) with 28.32g (40%) of pre-emulsion in the step (1) at 79 ℃ for 30min to prepare seed emulsion;
(4) uniformly mixing the residual 3.72g of initiator aqueous solution in the step (2), the residual 42.48g of pre-emulsion in the step (1) and the residual 24g of deionized water, dripping into seed emulsion for 1.5h, preserving heat for 2h after finishing dripping, cooling and discharging to obtain a component A;
(5) adding 0.5g of waterborne epoxy resin 5003-W-55A as the component B into the component A, and uniformly mixing to obtain the waterborne epoxy modified acrylate medical pressure-sensitive adhesive.
Example 5
(1) 10g of butyl acrylate, 20g of isooctyl acrylate, 6g of itaconic acid, 2g N, N-methylenebisacrylamide, 2g of urea-formaldehyde ethyl methacrylate, 60g of deionized water, 0.5g of 2, 2-azobis (2-amidinopropane) dihydrochloride, 1g of sodium lauryl sulfate, 0.8g of polyoxyethylene ether sorbitol hexastearate and 3g of waterborne epoxy resin 5003-W-55A were weighed.
Uniformly stirring 1g of sodium dodecyl sulfate, 0.8g of polyoxyethylene ether sorbitol hexastearate and 42g (70%) of deionized water, slowly dripping a mixture of 10g of butyl acrylate, 20g of isooctyl acrylate, 6g of itaconic acid, 2g N, N-methylene bisacrylamide and 2g of urea-formaldehyde ethyl methacrylate, and stirring at a high speed of 400r/min multiplied by 30min to prepare a pre-emulsion;
(2) 0.5g of 2, 2-azobis (2-amidinopropane) dihydrochloride and 12g (20%) of deionized water are stirred uniformly to obtain an initiator aqueous solution;
(3) mixing 7.5g (60%) of initiator aqueous solution obtained in the step (2) with 50.28g (60%) of pre-emulsion obtained in the step (1) at 82 ℃ for 60min to obtain seed emulsion;
(4) uniformly mixing the 5g of initiator aqueous solution remained in the step (2), the 33.52g of pre-emulsion remained in the step (1) and the 6g of deionized water remained in the step (1), dripping into the seed emulsion for 2.5h, preserving heat for 2h after dripping is finished, cooling and discharging to obtain a component A;
(5) and adding 3g of waterborne epoxy resin 5003-W-55A serving as the component B into the component A, and uniformly mixing to obtain the waterborne epoxy modified acrylate medical pressure-sensitive adhesive.
And (3) performance testing:
the 180 DEG peel strength test method for pressure-sensitive adhesive tapes was in accordance with GB/T2792-1998.
Initial adhesion test of pressure-sensitive adhesive was measured according to GB/T4582-2002.
The pressure-sensitive adhesive tack test was carried out in accordance with GB/T4851-1998.
The adhesion retention ratio was (R '/R) × 100% (where R is the 180 ° peel force of the tape and R' is the 180 ° peel force of the tape after repeated application and removal 10 times.
The performance tests are shown in Table 1
TABLE 1
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
180 degree peel force (steel plate) (g/25 mm) | 600 | 510 | 550 | 583 | 515 |
Initial adhesion (#) | 10 | 9 | 11 | 10 | 9 |
Holding power (h) | >120 | >120 | >120 | >120 | >120 |
Adhesion retention (%) | 88 | 79 | 95 | 85 | 73 |
As can be seen from examples 1-5, the peel strength of the product is 500-600g, and the initial adhesion, initial adhesion and adhesion retention are better measured. The special internal crosslinking monomer N, N-methylene-bisacrylamide and the multifunctional epoxy resin EPIKOTE-6006-W-68A adopted in the embodiment 3 enable the pressure-sensitive adhesive to have strong cohesive strength and large adhesive force, have high adhesive retention rate and are convenient to reuse.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The preparation method of the water-based epoxy modified acrylate medical pressure-sensitive adhesive is characterized in that the raw material of the pressure-sensitive adhesive comprises A, B two components in percentage by weight;
the component A comprises: 30-35% of soft monomer, 3-6% of functional monomer, 2-4% of crosslinking monomer, 60% of deionized water, and 0.2-0.5%, 0.4-1% and 0.4-0.8% of initiator, anionic emulsifier and nonionic emulsifier respectively based on the total weight of the soft monomer, the functional monomer and the crosslinking monomer;
the component B is multifunctional epoxy resin and accounts for 0.5 to 3 percent of the total weight of the component A;
the preparation method of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive comprises the following steps:
(1) weighing a soft monomer, a functional monomer, a crosslinking monomer, deionized water, an initiator, an anionic emulsifier, a nonionic emulsifier and multifunctional epoxy resin, uniformly stirring the anionic emulsifier, the nonionic emulsifier and 50-70% of deionized water, slowly dripping a mixture of the soft monomer, the functional monomer and the crosslinking monomer, and stirring at a high speed of 400r/min multiplied by 30min to prepare a pre-emulsion;
(2) uniformly stirring an initiator and 10-20% of deionized water to obtain an initiator aqueous solution;
(3) mixing the initiator aqueous solution with the concentration of 40-60% in the step (2) and the pre-emulsion with the concentration of 40-60% in the step (1) at 79-82 ℃, and reacting for 30-60min to obtain seed emulsion;
(4) uniformly mixing the residual initiator aqueous solution in the step (2), the residual pre-emulsion in the step (1) and the residual deionized water, dripping into the seed emulsion for 1.5-2.5h, preserving heat for 2h after dripping is finished, cooling and discharging to obtain a component A;
(5) adding the raw material of the component B into the component A, and uniformly mixing to prepare the waterborne epoxy modified acrylate medical pressure-sensitive adhesive;
the soft monomer is at least one of isodecyl methacrylate, isodecyl acrylate, stearic acid acrylate, butyl acrylate and isooctyl acrylate;
the functional monomer is itaconic acid;
the crosslinking monomer is at least one of N, N-methylene bisacrylamide, N-hydroxymethyl acrylamide and urea-formaldehyde ethyl methacrylate.
2. The preparation method of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive according to claim 1, wherein the initiator is 2, 2-azobis (2-amidinopropane) dihydrochloride.
3. The preparation method of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive according to claim 1, wherein the anionic emulsifier is sodium dodecyl sulfate.
4. The preparation method of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive according to claim 1, wherein the non-ionic emulsifier is polyoxyethylene ether sorbitol hexastearate.
5. The preparation method of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive according to claim 1, wherein the multifunctional epoxy resin is one of 4, 5-epoxycyclohexane-1, 2-dicarboxylic acid diglycidyl ester, waterborne epoxy resin 6006-W-68A and waterborne epoxy resin 5003-W-55A.
6. The preparation method of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive according to claim 1, wherein the raw materials of the component A comprise, by weight:
soft monomer: 20% of butyl acrylate and 12% of stearic acid acrylate;
functional monomer: 5% of itaconic acid;
crosslinking monomer: 3% of N, N-methylene bisacrylamide;
initiator: 2, 2-azobis (2-amidinopropane) dihydrochloride at 0.3% by weight based on the total weight of the soft monomers, functional monomers and crosslinking monomers;
anionic emulsifiers: sodium dodecyl sulfate accounting for 0.7 percent of the total weight of the soft monomer, the functional monomer and the crosslinking monomer;
non-ionic emulsifier: polyoxyethylene ether sorbitol hexastearate accounting for 0.6 percent of the total weight of the soft monomer, the functional monomer and the crosslinking monomer;
the raw material of the component B is waterborne epoxy resin 6006-W-68A accounting for 1.8% of the total weight of the component A.
7. The waterborne epoxy modified acrylate medical pressure-sensitive adhesive prepared by the preparation method of the waterborne epoxy modified acrylate medical pressure-sensitive adhesive according to any one of claims 1 to 6.
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CN111471145B (en) * | 2020-04-23 | 2023-02-03 | 巨石集团有限公司 | Emulsion type epoxy modified acrylate pressure-sensitive adhesive and preparation method and application thereof |
CN112915250A (en) * | 2021-01-29 | 2021-06-08 | 振德医疗用品股份有限公司 | Low-viscosity isolation acrylic pressure-sensitive adhesive for wound surface and preparation method thereof |
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