CN111978893B - Acrylate adhesive, preparation method thereof and application thereof in label paper - Google Patents
Acrylate adhesive, preparation method thereof and application thereof in label paper Download PDFInfo
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- CN111978893B CN111978893B CN202010866130.9A CN202010866130A CN111978893B CN 111978893 B CN111978893 B CN 111978893B CN 202010866130 A CN202010866130 A CN 202010866130A CN 111978893 B CN111978893 B CN 111978893B
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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
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
- C09J133/12—Homopolymers or copolymers of methyl methacrylate
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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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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J133/06—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
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
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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
- C09J135/00—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 a carboxyl radical, and containing at least another carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Adhesives based on derivatives of such polymers
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/21—Paper; Textile fabrics
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
- G09F3/02—Forms or constructions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/334—Applications of adhesives in processes or use of adhesives in the form of films or foils as a label
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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
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/20—Presence of organic materials
- C09J2400/28—Presence of paper
- C09J2400/283—Presence of paper in the substrate
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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
- C09J2433/00—Presence of (meth)acrylic polymer
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
- G09F3/02—Forms or constructions
- G09F2003/023—Adhesive
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Abstract
The application belongs to the field of polymer adhesives, and relates to an acrylate adhesive, a preparation method thereof and application thereof in label paper. The acrylate adhesive is prepared by polymerization reaction of preparation raw materials containing the following components at 80-85 ℃: 100 parts of acrylate soft monomer, 2-5 parts of acrylate hard monomer, 10-20 parts of functional monomer, 4-8 parts of modified composite nano particles, 6-8 parts of emulsifier, 0.5-0.7 part of initiator and 100-150 parts of organic solvent, and 30-40 parts of talcum powder can also be included. The preparation of the modified composite nano-particles comprises the following steps: adding the nano-cellulose and the nano-montmorillonite into an ethanol water solution according to the weight ratio of 1 (2-5), adding a silane coupling agent after ultrasonic treatment, adjusting the pH to weak acidity after ultrasonic treatment, stirring, cooling, centrifuging, and freeze-drying to obtain the nano-montmorillonite/nano-montmorillonite composite material. The acrylate adhesive can be used for the back adhesive of a label, and the physical properties of initial adhesion, 180-degree peel strength and permanent adhesion of the acrylate adhesive in the label are improved on the premise that a large amount of talcum powder exists and the production cost of the acrylate adhesive is reduced.
Description
Technical Field
The application relates to the field of high-molecular adhesives, in particular to an acrylate adhesive, a preparation method thereof and application thereof in label paper.
Background
At present, industries with large label usage amount comprise logistics industry, daily chemical industry, electronic and electric industry, medicine industry and the like. With the rapid development of these industries, in recent years, the label industry has been increasing at a high rate, and the annual rate of increase can reach more than 20%. The label mainly comprises base paper such as release paper, an adhesive and surface paper, wherein the quality of the adhesive has an important influence on the service performance of the label.
Acrylate adhesives are one type of adhesive commonly used in labels. However, the label using the acrylate adhesive as the adhesive is easy to have phenomena of edge lifting, wrinkling, falling off and the like during the use process, which is related to the poor physical properties of the acrylate adhesive, such as initial adhesion, peeling strength, holding viscosity and the like. How to continuously improve the above physical properties of the acrylate adhesive is the key to the development of acrylate adhesives.
Disclosure of Invention
In order to improve physical properties such as initial tack, peel strength, permanent tack and the like of the acrylate adhesive, the application provides the acrylate adhesive, a preparation method thereof and application thereof in label paper.
In a first aspect, the present application provides an acrylate adhesive, which adopts the following technical scheme:
an acrylate adhesive is prepared by the polymerization reaction of raw materials comprising the following components: 100 parts of acrylate soft monomer, 2-5 parts of acrylate hard monomer, 10-20 parts of functional monomer, 4-8 parts of modified composite nano-particles, 6-8 parts of emulsifier, 0.5-0.7 part of initiator and 100-150 parts of organic solvent, wherein the preparation method of the modified composite nano-particles comprises the following steps:
mixing nano-cellulose and nano-montmorillonite according to the weight ratio of 1 (2-5) to obtain mixed nano-particles; adding the mixed nano particles into an ethanol aqueous solution according to the addition amount of 30-50g/L, carrying out ultrasonic treatment to obtain a suspension, then adding a silane coupling agent accounting for 2-5% of the volume of the suspension, and continuing the ultrasonic treatment to obtain a dispersed suspension; adjusting the pH of the dispersion suspension to be weakly acidic, stirring at 45-55 ℃, cooling, centrifuging, washing a centrifugal product, and freeze-drying to obtain the modified composite nano-particles.
By adopting the technical scheme, the nano-cellulose and the nano-montmorillonite in a certain ratio are selected as the composite nano-particles, and then the composite nano-particles are modified by a silane coupling agent, ultrasonic treatment and freeze drying to obtain the modified composite nano-particles. Then, the modified composite nano-particles are added into the preparation raw materials of the acrylate adhesive, and meanwhile, the mixture ratio of other raw materials of the acrylate adhesive is properly adjusted. The test results show that the physical properties of initial adhesion, peeling strength and holding adhesion of the acrylate adhesive can be remarkably improved by the treatment means, and the physical properties are related to that the modified composite nano particles enhance the cohesive force of an acrylate adhesive film.
Preferably, the raw materials for preparing the acrylate adhesive also comprise 30-40 parts of talcum powder.
The talcum powder is one kind of stuffing capable of lowering the production cost of acrylate adhesive greatly, and may be used in common acrylate adhesive and label to result in serious negative effect on the initial adhesion, peeling strength, holding adhesion and other physical performance of acrylate adhesive. However, for the present application, the test results show that even if a large amount of talc is added to the raw materials for preparing the acrylate adhesive, the above physical properties of the finally obtained acrylate adhesive are not greatly reduced, and only slightly reduced, however, the production cost of the acrylate is greatly reduced, which has important practical significance in market competition.
Preferably, the acrylate soft monomer is one or more of 2-ethyl hexyl acrylate, butyl acrylate and isooctyl acrylate.
Preferably, the acrylic hard monomer is one or more of methyl acrylate and methyl methacrylate.
Preferably, the functional monomer is one or more of acrylic acid, methacrylic acid, itaconic acid and hydroxyethyl acrylate.
Preferably, the emulsifier is one or more of sodium stearate and sodium dodecyl sulfate.
Preferably, the initiator is azobisisobutyronitrile.
In a second aspect, the present application provides a method for preparing an acrylate adhesive, which adopts the following technical scheme:
the preparation method of the acrylate adhesive comprises the following steps:
taking 70-80% of the total weight of the organic solvent, adding other preparation raw materials of the acrylate adhesive except the initiator and the organic solvent, and uniformly stirring to obtain a mixed solution A;
b, adding the initiator into the residual organic solvent, and uniformly stirring to obtain an initiator solution B;
and c, heating the mixed solution A to 80-85 ℃ under the condition of stirring, then dropwise adding an initiator solution B for reaction, preserving heat for 1-1.5h after dropwise adding is finished, cooling to below 50 ℃ after heat preservation is finished, filtering and discharging to obtain the acrylate adhesive.
For the purposes of this application, the preparation process likewise has a significant influence on the final physical properties of the acrylate adhesives, in particular the parameters relating to temperature, time, etc. during the preparation. By adopting the technical scheme, the preparation parameters of the acrylate adhesive are reasonably limited, and the physical properties of the finally obtained acrylate adhesive, such as initial adhesion, peeling strength, lasting adhesion and the like, can be further improved.
In a third aspect, the present application provides the use of an acrylate adhesive: the back glue is used for the label paper.
In summary, the present application at least includes the following beneficial technical effects:
1. the method adopts a silane coupling agent, ultrasonic treatment and freeze drying composite treatment means to carry out modification treatment on composite nano particles consisting of nano cellulose and nano montmorillonite to obtain modified composite nano particles, and the modified composite nano particles are applied to the preparation of an acrylate adhesive and used in label paper, so that the physical properties of initial adhesion, peel strength and permanent adhesion of the acrylate adhesive are improved. The preparation of the modified composite nano-particles provides a new idea for improving the physical properties of the acrylate adhesive;
2. on the premise of adopting the modified composite nano-particles, a large amount of talcum powder is added, and test results show that the physical properties of initial viscosity, peel strength and permanent viscosity of the acrylate adhesive are only slightly reduced, but the production cost of the acrylate adhesive is greatly reduced, which has important practical significance for improving market competitiveness.
Detailed Description
The information on the provenance, the type, etc. of part of the raw materials used in the following examples and comparative examples is as follows:
the nano-cellulose is purchased from new materials science and technology (Shanghai) Co., Ltd, and the model is 201;
the nano montmorillonite is purchased from Guangzhou hundred million peaking technology, Inc., the type is TY-710C, and the particle size is 50 nm.
Example 1
An acrylate adhesive is prepared from the following raw materials: 100 parts of acrylate soft monomer, 2 parts of acrylate hard monomer, 20 parts of functional monomer, 4 parts of modified composite nano particles, 8 parts of emulsifier, 0.5 part of initiator and 150 parts of organic solvent; wherein, the acrylate soft monomer is acrylic acid-2-ethyl diester and isooctyl acrylate according to the part by weight of 1:1, the acrylic acid hard monomer is methyl acrylate and methyl methacrylate according to the part by weight of 1:1, the functional monomer is acrylic acid and methacrylic acid according to the part by weight of 1:1, the emulsifier is sodium stearate, and the initiator is azobisisobutyronitrile; the organic solvent is absolute ethyl alcohol; the preparation method of the modified composite nano-particles comprises the following steps: preparing absolute ethyl alcohol and deionized water into an ethyl alcohol aqueous solution according to the volume ratio of 3: 1; mixing nano-cellulose and nano-montmorillonite in a weight ratio of 1:2 to obtain mixed nano-particles; adding the mixed nano particles into an ethanol aqueous solution according to the addition amount of 30g/L, carrying out ultrasonic treatment for 20min under the power of 120W to obtain a suspension, then adding a silane coupling agent KH570 accounting for 5% of the volume of the suspension, and carrying out ultrasonic treatment for 20min under the power of 120W to obtain a dispersed suspension; adjusting the pH of the dispersion suspension to be weakly acidic by using citric acid, stirring for 2 hours at 45 ℃, cooling, centrifuging, washing a centrifugal product by using deionized water, and freeze-drying to obtain modified composite nanoparticles;
the preparation method of the acrylate adhesive comprises the following steps:
taking 70% of the total weight of the organic solvent, adding other preparation raw materials of the acrylate adhesive except the initiator and the organic solvent, and uniformly stirring to obtain a mixed solution A;
b, adding the initiator into the residual organic solvent, and uniformly stirring to obtain an initiator solution B;
and c, heating the mixed solution A to 80 ℃ under the condition of stirring, then dropwise adding an initiator solution B for reaction, keeping the temperature for 1h after dropwise adding is finished, cooling to 45 ℃ after the temperature is kept, filtering and discharging to obtain the acrylate adhesive.
Example 2
An acrylate adhesive is prepared from the following raw materials: 100 parts of acrylate soft monomer, 3.5 parts of acrylate hard monomer, 15 parts of functional monomer, 6 parts of modified composite nano-particles, 7 parts of emulsifier, 0.6 part of initiator and 125 parts of organic solvent; wherein the acrylate soft monomer is butyl acrylate, the acrylic acid hard monomer is methyl methacrylate, the functional monomer is itaconic acid, the emulsifier is sodium dodecyl sulfate, and the initiator is azobisisobutyronitrile; the organic solvent is absolute ethyl alcohol;
the preparation method of the modified composite nano-particles comprises the following steps: preparing absolute ethyl alcohol and deionized water into an ethyl alcohol aqueous solution according to the volume ratio of 3: 1; mixing nano-cellulose and nano-montmorillonite according to the weight ratio of 1:3.5 to obtain mixed nano-particles; adding the mixed nano particles into an ethanol aqueous solution according to the adding amount of 40g/L, carrying out ultrasonic treatment for 20min under the power of 120W to obtain a suspension, then adding a silane coupling agent KH570 accounting for 3% of the volume of the suspension, and carrying out ultrasonic treatment for 20min under the power of 120W to obtain a dispersed suspension; adjusting the pH of the dispersion suspension to be weakly acidic by using citric acid, stirring for 2h at 50 ℃, cooling, centrifuging, washing a centrifuged product by using deionized water, and freeze-drying to obtain the modified composite nano-particles.
The preparation method of the acrylate adhesive comprises the following steps:
taking 75% of the total weight of the organic solvent, adding other preparation raw materials of the acrylate adhesive except the initiator and the organic solvent, and uniformly stirring to obtain a mixed solution A;
b, adding the initiator into the residual organic solvent, and uniformly stirring to obtain an initiator solution B;
and c, heating the mixed solution A to 82 ℃ under the condition of stirring, then dropwise adding an initiator solution B for reaction, keeping the temperature for 1.2h after dropwise adding is finished, cooling to 45 ℃ after the temperature is kept, filtering and discharging to obtain the acrylate adhesive.
Example 3
An acrylate adhesive is prepared from the following raw materials: 100 parts of acrylate soft monomer, 5 parts of acrylate hard monomer, 10 parts of functional monomer, 8 parts of modified composite nano-particles, 6 parts of emulsifier, 0.7 part of initiator and 100 parts of organic solvent; wherein the acrylate soft monomer is acrylic acid-2-ethyl diester, the acrylic acid hard monomer is methyl acrylate, the functional monomer is hydroxyethyl acrylate, the emulsifier is sodium dodecyl sulfate, and the initiator is azobisisobutyronitrile; the organic solvent is absolute ethyl alcohol;
the preparation method of the modified composite nano-particles comprises the following steps: preparing absolute ethyl alcohol and deionized water into an ethyl alcohol aqueous solution according to the volume ratio of 3: 1; mixing nano-cellulose and nano-montmorillonite according to the weight ratio of 1:5 to obtain mixed nano-particles; adding the mixed nano particles into an ethanol aqueous solution according to the addition amount of 50g/L, carrying out ultrasonic treatment for 20min under the power of 120W to obtain a suspension, then adding a silane coupling agent KH570 accounting for 2% of the volume of the suspension, and carrying out ultrasonic treatment for 20min under the power of 120W to obtain a dispersed suspension; and adjusting the pH of the dispersion suspension to be weakly acidic by using citric acid, stirring for 2h at 55 ℃, cooling, centrifuging, washing the centrifuged product by using deionized water, and freeze-drying to obtain the modified composite nano-particles.
The preparation method of the acrylate adhesive comprises the following steps:
taking 80% of the total weight of the organic solvent, adding other preparation raw materials of the acrylate adhesive except the initiator and the organic solvent, and uniformly stirring to obtain a mixed solution A;
b, adding the initiator into the residual organic solvent, and uniformly stirring to obtain an initiator solution B;
and c, heating the mixed solution A to 85 ℃ under the condition of stirring, then dropwise adding an initiator solution B for reaction, keeping the temperature for 1.5h after dropwise adding is finished, cooling to 45 ℃ after the temperature is kept, filtering and discharging to obtain the acrylate adhesive.
Example 4
An acrylate adhesive, differing from example 2 in that: the raw materials for preparing the acrylate adhesive also comprise 30 parts of talcum powder.
Example 5
An acrylate adhesive, differing from example 2 in that: the raw materials for preparing the acrylate adhesive also comprise 35 parts of talcum powder.
Example 6
An acrylate adhesive, differing from example 2 in that: the raw materials for preparing the acrylate adhesive also comprise 40 parts of talcum powder.
Comparative example 1
An acrylate adhesive, differing from example 2 in that: the raw materials for preparing the acrylate adhesive do not comprise the modified composite nano particles.
Comparative example 2
An acrylate adhesive, differing from example 2 in that: in the preparation raw materials of the acrylate adhesive, the mixed nano-particles with equal weight parts are directly adopted to replace the modified composite nano-particles.
Comparative example 3
An acrylate adhesive, differing from example 2 in that: in the preparation process of the modified composite nano-particles, only one nano-cellulose is contained in the mixed nano-particles.
Comparative example 4
An acrylate adhesive, differing from example 2 in that: in the preparation process of the modified composite nano-particles, only one kind of nano-montmorillonite is contained in the mixed nano-particles.
Comparative example 5
An acrylate adhesive, differing from example 2 in that: in the preparation process of the modified composite nano-particles, after a centrifugal product is washed by deionized water, freeze drying is not adopted, but room temperature drying is adopted.
Comparative example 6
Commercially available acrylate adhesives are used for similar labels.
Physical Property test of acrylate Adhesives
Initial tack, peel strength and tack are important physical property indicators for acrylate adhesives for reactive labels. The acrylate adhesives of examples 1-6 and comparative examples 1-6 were tested herein for initial tack, 180 peel strength, and tack following labeling adhesives.
In the initial tack test, the measurement was carried out in accordance with the "circular initial tack measurement" in FINAT FTM 9-2005. The specific operation is as follows: a sample of the acrylate adhesive was applied to release paper with a 50 μm wire rod at a coating weight of 20g/m2Drying at 105 ℃ for 3min, then pasting the adhesive surface of the release paper coated with the acrylate adhesive sample on the white cardboard, cutting into 250mm multiplied by 25mm paper strips, and placing the paper strips for 4h at the temperature of 23 ℃ and the humidity of 50% RH; before testing, removing the release paper, enabling the adhesive surface to face outwards, holding two ends of the adhesive tape to form a ring, clamping the 10mm of the tail end of the ring into an upper clamp of a peeling strength tester PT-6801B chest expander, and enabling the ring of the adhesive tape to vertically face downwards; a100 mm × 25mm glass plate is clamped into a lower fixture, an annular adhesive tape is contacted with the glass plate at a speed of 300mm/min, when the contact is completed (the contact surface is 25mm × 25mm), the glass plate is immediately separated at a speed of 300mm/min in a reverse direction, the maximum force value when the separation is completed is recorded, and the average value of four times is taken as an annular initial adhesion value to be represented as the initial adhesion of an acrylate adhesive sample.
The 180 DEG peel strength was performed according to the regulations in GB/T2792-1998. The specific operation is as follows: a sample of an acrylate adhesive was uniformly coated on a 2.5cm wide PET film in an amount of 20g/m2Then, the PET film was attached to a test board, rolled back and forth three times with a 2 kg-weight manual rolling roller, placed for 10min, one end of the PET film was clamped in a tensile force peeling test device, the PET film was peeled off from the surface of the test board at 180 degrees at a test speed of 300mm/min, and the test speed was recordedReadings were recorded and four tests averaged to give a 180 ° peel strength value.
Retention was performed as specified in GB 4851-1998. The specific operation is as follows: coating an acrylate adhesive sample on a 7.0cm multiplied by 2.5cm PET film by a 50-micron wire rod, attaching the PET film on a test board, rolling the PET film three times by a manual rolling roller with the weight of 2kg, vertically hanging the PET film on a test rack, hanging a 1kg weight at the lower end of the PET film, and recording the time for completely separating the PET film as the representation of the adhesion of the acrylate adhesive sample.
The results of measurement of initial tack, peel strength and tack holding property are shown in Table 1.
TABLE 1 results of physical Properties measurements of acrylate adhesive samples
As can be seen from Table 1, the initial tack, 180 ℃ peel strength and tack strength of the acrylate adhesives prepared in examples 1-3 of the present application are greatly improved as compared to the commercially available acrylate adhesive for the same type of label in comparative example 6. The improvement in the performance of the acrylate adhesives produced herein is primarily due to the addition of the modified nanocomposite particles to the raw materials used in the preparation of the acrylate adhesives, as is more clearly seen in the combined comparison of example 2 and comparative example 1. The reason why the modified nanocomposite particles improve the physical properties of the acrylate adhesive is that they enhance the cohesive force of the adhesive film of the acrylate adhesive.
Combining example 2 and comparative example 2, it can be seen that the physical properties of the acrylate adhesive can not be improved but rather can be seriously affected by simply adding the mixed nanoparticles to the raw materials for preparing the acrylate adhesive. This shows that, for the present application, the composite treatment means of silane coupling agent treatment, ultrasonic treatment, and freeze drying treatment on the mixed nanoparticles has important significance for the physical properties of the acrylate adhesive, wherein, in combination with comparative example 5, the significance of freeze drying for the modification of the mixed nanoparticles can be further seen. The reason why the above-mentioned composite treatment means for the mixed nanoparticles can improve the physical properties of the acrylate adhesive is that it improves the dispersibility of the mixed nanoparticles in the acrylate adhesive.
It can be seen from the combination of example 2 and comparative examples 3-4 that the physical properties of the acrylate adhesive cannot be improved well even when the nano-cellulose or the nano-montmorillonite is simply selected as the nano-particles and added to the raw materials for preparing the acrylate adhesive after modification. This illustrates that for the purposes of this application, there is a synergistic effect between nanocellulose and nanomontmorillonite, which may also be related to the ability to improve the dispersibility of each other in polyacrylate adhesives when mixed.
The talcum powder is one kind of stuffing capable of lowering the production cost of acrylate adhesive greatly, and may be used in common acrylate adhesive and label to result in serious negative effect on the physical performance of acrylate adhesive, such as peeling strength, holding viscosity, etc. even if small amount of talcum powder is added into acrylate adhesive, great care is required. However, in the present application, it can be seen from examples 2 and 4 to 6 that even when a large amount of talc is added to the raw materials for producing the acrylic adhesive, the physical properties such as peel strength, tack strength, and lifting of the finally obtained acrylic adhesive are not greatly reduced, but only slightly reduced. The application has the advantages because of the addition of the modified composite nano particles and the adjustment of the proportion of the raw materials for preparing the acrylate adhesive. The acrylate adhesive prepared by the method can keep the physical properties at a higher level on the premise of greatly reducing the production cost, and has important practical significance in market competition.
Use of acrylate adhesives in labels
An operation to be applied here was to apply the acrylic adhesive prepared in examples 1 to 6 as a back adhesive to a release paper at a thickness of 50 μm, dry the release paper coated with the acrylic adhesive at 102 ℃ for 3min, attach a white cardboard to the side of the release paper coated with the acrylic adhesive, and transfer the acrylic adhesive to the white cardboard to form a label paper.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made in accordance with the present application should be covered by the protection scope of the present application.
Claims (9)
1. The acrylate adhesive is characterized by being prepared by carrying out polymerization reaction on raw materials comprising the following components: 100 parts of acrylate soft monomer, 2-5 parts of acrylate hard monomer, 10-20 parts of functional monomer, 4-8 parts of modified composite nano particles, 6-8 parts of emulsifier, 0.5-0.7 part of initiator and 100-150 parts of organic solvent, wherein,
the preparation method of the modified composite nano-particles comprises the following steps:
mixing nano-cellulose and nano-montmorillonite according to the weight ratio of 1 (2-5) to obtain mixed nano-particles; adding the mixed nano particles into an ethanol aqueous solution according to the addition amount of 30-50g/L, carrying out ultrasonic treatment to obtain a suspension, then adding a silane coupling agent accounting for 2-5% of the volume of the suspension, and continuing the ultrasonic treatment to obtain a dispersed suspension; adjusting the pH of the dispersion suspension to be weakly acidic, stirring at 45-55 ℃, cooling, centrifuging, washing a centrifugal product, and freeze-drying to obtain the modified composite nano-particles.
2. The acrylate adhesive of claim 1, wherein: the raw materials for preparing the acrylate adhesive also comprise 30-40 parts of talcum powder.
3. The acrylate adhesive according to claim 1 or 2, wherein: the acrylate soft monomer is one or more of acrylic acid-2-ethyl diester, butyl acrylate and isooctyl acrylate.
4. The acrylate adhesive according to claim 1 or 2, wherein: the acrylic acid hard monomer is one or more of methyl acrylate and methyl methacrylate.
5. The acrylate adhesive according to claim 1 or 2, wherein: the functional monomer is one or more of acrylic acid, methacrylic acid, itaconic acid and hydroxyethyl acrylate.
6. The acrylate adhesive according to claim 1 or 2, wherein: the emulsifier is one or more of sodium stearate and sodium dodecyl sulfate.
7. The acrylate adhesive according to claim 1 or 2, wherein: the initiator is azobisisobutyronitrile.
8. A method for preparing the acrylate adhesive of any one of claims 1 to 7, comprising the steps of:
taking 70-80% of the total weight of the organic solvent, adding other preparation raw materials of the acrylate adhesive except the initiator and the organic solvent, and uniformly stirring to obtain a mixed solution A;
b, adding the initiator into the residual organic solvent, and uniformly stirring to obtain an initiator solution B;
and c, heating the mixed solution A to 80-85 ℃ under the condition of stirring, then dropwise adding an initiator solution B for reaction, preserving heat for 1-1.5h after dropwise adding is finished, cooling after heat preservation is finished, filtering and discharging to obtain the acrylate adhesive.
9. Use of an acrylate adhesive as claimed in any of claims 1 to 7 wherein: the back glue is used for the label paper.
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| CN113737571A (en) * | 2021-08-12 | 2021-12-03 | 佛山南海力豪包装有限公司 | Preparation method of sustainable high-barrier paper base material with enhanced moisture and oxygen resistance |
| CN116120639A (en) * | 2023-02-03 | 2023-05-16 | 桂林桂广申巴粉体材料有限责任公司 | Carrier-free talcum powder granule and preparation method thereof |
| CN118146738B (en) * | 2024-04-04 | 2024-08-30 | 苏州市奥贝新材料科技有限公司 | Preparation method of PVC electrical adhesive tape |
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