CN108034018B - Water-based sealing adhesive emulsion and preparation method thereof - Google Patents
Water-based sealing adhesive emulsion and preparation method thereof Download PDFInfo
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- CN108034018B CN108034018B CN201810048742.XA CN201810048742A CN108034018B CN 108034018 B CN108034018 B CN 108034018B CN 201810048742 A CN201810048742 A CN 201810048742A CN 108034018 B CN108034018 B CN 108034018B
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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
-
- 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
-
- 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
- C08F218/00—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 an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F218/02—Esters of monocarboxylic acids
- C08F218/04—Vinyl esters
- C08F218/08—Vinyl acetate
-
- 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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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
-
- 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
- C08F220/20—Esters of polyhydric alcohols or phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
Abstract
The invention provides a water-based sealing adhesive emulsion and a preparation method thereof, belonging to the technical field of adhesives. The water-based sealing adhesive emulsion comprises the following components in parts by weight: 15-20 parts of polyvinyl alcohol, 2-3 parts of sodium bicarbonate, 15-20 parts of emulsifier, 3-4 parts of initiator, 300-500 parts of butyl acrylate, 100-300 parts of vinyl acetate, 10-20 parts of 2-hydroxyethyl acrylate, 1-2 parts of acrylic acid, 1-2 parts of n-dodecyl mercaptan, 0.5-1 part of sodium bisulfite, 0.5-1 part of defoaming agent, 2-3 parts of preservative and 450-500 parts of deionized water. The water-based sealing adhesive emulsion provided by the invention is used for preparing water-based sealing adhesive, and can be effectively used for edge sealing or lap joint of BOPP/paper, polished/paper, PET/paper, paper/paper, printing ink/paper and UV (ultraviolet) polished/paper.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to an emulsion used in an aqueous sealing adhesive and a preparation method thereof.
Background
The sealing glue is an adhesive widely used in the packaging industry and is used for sealing edges of paper boxes, hand bags and the like. The sealing compound mainly comprises an oil sealing compound and a water sealing compound. The oily sealing glue generally takes toluene and the like as a solvent, takes SBS, terpene resin, rosin and the like as main raw materials, and has great harm to the environment and the health of human bodies. The water-based sealing adhesive is an environment-friendly adhesive taking water as a dispersion medium, is non-toxic and pollution-free, and gradually replaces oil-based sealing adhesive. After a plurality of water-based sealing adhesives in the market are used, the prepared packages are easy to degum in a high-temperature or low-temperature environment, and loss is caused to enterprises, because the bonding strength, the high-temperature resistance and the low-temperature resistance of the water-based sealing adhesives are poor.
Disclosure of Invention
The water-based sealing adhesive prepared by the emulsion has good heat resistance and good frost resistance, and can be effectively used for edge sealing or joint lapping of BOPP/paper, polished/paper, PET/paper, paper/paper, printing ink/paper and UV (ultraviolet) glazing/paper.
In order to achieve the aim, the invention provides a water-based sealing adhesive emulsion, which comprises the following components in parts by weight:
in the technical scheme, butyl acrylate is selected as a soft monomer, vinyl acetate is selected as a hard monomer, and the butyl acrylate and the vinyl acetate can generate better cohesive strength after copolymerization, so that the water resistance, the adhesive force and the transparency are improved. Acrylic acid-2-hydroxyethyl ester and acrylic acid are selected as crosslinking monomers to participate in copolymerization to generate a crosslinking network structure, so that the bonding strength, the high temperature resistance, the low temperature resistance and the stability are improved.
Preferably, the polyvinyl alcohol is a mixture of one or more of PVA1788, PVA0588, PVA1792 and PVA1799 in any proportion.
Preferably, the emulsifier is a mixture of one or more than two of alkyl sulfate, polyoxyethylene ether sulfosuccinate or fatty alcohol-polyoxyethylene ether in any proportion.
Preferably, the initiator is one of potassium persulfate, sodium persulfate or ammonium persulfate.
Preferably, the defoamer is polydimethylsiloxane.
Preferably, the preservative is sodium benzoate.
The invention also provides a preparation method of the water-based sealing adhesive emulsion, which comprises the following steps:
1) dissolving 0.4-0.6 part of initiator in 5-10 parts of water to obtain a primary initiator; dissolving 2.5-3.1 parts of initiator in 40-50 parts of water to obtain a drop initiator; dissolving 0.1-0.3 part of initiator in 5-10 parts of water to obtain a post-initiator; dissolving 0.5-1 part of sodium bisulfite in 10-20 parts of water to obtain a reducing agent;
uniformly mixing and stirring 300-500 parts of butyl acrylate, 100-300 parts of vinyl acetate, 10-20 parts of 2-hydroxyethyl acrylate, 1-2 parts of acrylic acid and 1-2 parts of n-dodecyl mercaptan to obtain a mixed monomer;
2) adding the residual water and 15-20 parts of polyvinyl alcohol into a reaction kettle, starting stirring, heating to 92 ℃, and stirring to disperse the polyvinyl alcohol until the polyvinyl alcohol is completely dissolved;
3) cooling, keeping the temperature between 75 and 80 ℃, sequentially adding 2 to 3 parts of sodium bicarbonate, 15 to 20 parts of emulsifier and primary initiator, and then dropwise adding the mixed monomer and the initiator at a constant speed for 6 hours; then dropwise adding the post initiator at a constant speed for 0.5 hour;
4) heating, keeping the temperature between 80 and 85 ℃, stirring at medium speed, and keeping the temperature for 1 hour;
5) then cooling, when the temperature is reduced to 75 ℃, slowly adding a sodium bisulfite solution in 15 minutes at a constant speed, then cooling to 40 ℃, and sequentially adding 0.5-1 part of defoaming agent and 2-3 parts of preservative;
6) and after uniformly mixing, discharging and filtering to obtain the water-based sealing adhesive emulsion.
Compared with the prior art, the invention has the advantages and positive effects that:
1. the water-based sealing adhesive emulsion provided by the invention is prepared by polymerizing water serving as a dispersion medium and vinyl acetate and butyl acrylate serving as main monomers. It has alkali thickening property, and high initial viscosity; polyvinyl alcohol is used as protective glue, and the high-humidity adhesive and the compatibility stability are achieved; contains special crosslinking monomers of acrylic acid-2-hydroxyethyl ester and acrylic acid, is easy to form composite crosslinking with a bonding interface, and endows stronger adhesive force, flexibility and permanent adhesion; low glass transition temperature and good freezing resistance.
2. The water-based sealing adhesive emulsion provided by the invention is used for preparing water-based sealing adhesive, has high bonding strength, good heat resistance and good frost resistance, meets the technical requirement of HJ 2541-containing 2016 environmental mark products and the standard requirement of GB 18583-containing 2008 harmful substance limit in indoor decoration and finishing material adhesives, and can be widely used for edge sealing or opening lapping of BOPP/paper, polished/paper, PET/paper, paper/paper, ink/paper and UV polished/paper.
Detailed Description
The following description will be made in conjunction with specific embodiments.
Example 1
1) Weighing raw materials:
2) the preparation process comprises the following steps:
dissolving 0.5kg of initiator in 5kg of water to obtain a primary initiator; dissolving 2.5kg of initiator in 45kg of water to obtain a drop of initiator; dissolving 0.2kg of initiator in 5kg of water to obtain a post initiator; 0.5kg of sodium bisulfite was dissolved in 10kg of water to obtain a reducing agent.
310kg of butyl acrylate, 240kg of vinyl acetate, 15kg of 2-hydroxyethyl acrylate, 1kg of acrylic acid and 1.2kg of n-dodecyl mercaptan are mixed and stirred uniformly to obtain a mixed monomer.
Adding 420kg of water and 17.5kg of polyvinyl alcohol into a reaction kettle, starting stirring, heating to 92 ℃, and stirring to disperse the polyvinyl alcohol until the polyvinyl alcohol is completely dissolved.
And (3) cooling, keeping the temperature between 75 and 80 ℃, sequentially adding 2.2kg of sodium bicarbonate, 18kg of emulsifier and an initial initiator, then dropwise adding the mixed monomer and the dropwise initiator at a constant speed for 6 hours, and then dropwise adding the post-initiator at a constant speed for 0.5 hour.
And (3) heating, keeping the temperature between 80 and 85 ℃, stirring at a medium speed, and keeping the temperature for 1 hour.
And then cooling, slowly adding a sodium bisulfite solution at a constant speed for 15 minutes when the temperature is reduced to 75 ℃, then cooling to 40 ℃, and sequentially adding 0.8kg of defoaming agent and 2kg of preservative.
And (3) after uniformly mixing, discharging and filtering to obtain the water-based sealing adhesive emulsion with the Tg of-25 ℃.
Example 2
1) Weighing raw materials:
2) the preparation process comprises the following steps:
dissolving 0.5kg of initiator in 5kg of water to obtain a primary initiator; dissolving 2.5kg of initiator in 45kg of water to obtain a drop of initiator; dissolving 0.2kg of initiator in 5kg of water to obtain a post initiator; 0.5kg of sodium bisulfite was dissolved in 10kg of water to obtain a reducing agent.
400kg of butyl acrylate, 150kg of vinyl acetate, 15kg of 2-hydroxyethyl acrylate, 1kg of acrylic acid and 1.2kg of n-dodecyl mercaptan are mixed and stirred uniformly to obtain a mixed monomer.
Adding 420kg of water and 17.5kg of polyvinyl alcohol into a reaction kettle, starting stirring, heating to 92 ℃, and stirring to disperse the polyvinyl alcohol until the polyvinyl alcohol is completely dissolved.
And (3) cooling, keeping the temperature between 75 and 80 ℃, sequentially adding 2.2kg of sodium bicarbonate, 18kg of emulsifier and an initial initiator, then dropwise adding the mixed monomer and the dropwise initiator at a constant speed for 6 hours, and then dropwise adding the post-initiator at a constant speed for 0.5 hour.
And (3) heating, keeping the temperature between 80 and 85 ℃, stirring at a medium speed, and keeping the temperature for 1 hour.
And then cooling, slowly adding a sodium bisulfite solution at a constant speed for 15 minutes when the temperature is reduced to 75 ℃, then cooling to 40 ℃, and sequentially adding 0.8kg of defoaming agent and 2kg of preservative.
After being mixed evenly, the mixture is discharged and filtered, and the water-based sealing adhesive emulsion with the Tg of-35 ℃ is obtained.
Performance testing
The physical and chemical performance indexes of the aqueous sealing adhesive emulsions prepared in examples 1 to 2 were measured according to the standards of "adhesive for food packaging materials and containers" in GB/T33320-2016 (environmental marking for articles) "technical requirements and adhesive" in HJ 2541-2016 (environmental marking for articles) ", and" limits of harmful substances in indoor decoration materials and adhesives "in GB 18583-2008 (2008), and the results are shown in Table 1.
TABLE 1 results of physical and chemical properties index measurements
| Index (I) | Example 1 | Example 2 |
| Appearance of the product | Milky uniform liquid | Milky uniform liquid |
| pH value | 4.5 | 5.0 |
| Non-volatile matter content | 53.50％ | 53.66％ |
| Viscosity (25 ℃ C.) | 4500mPa·s | 5500mPa·s |
| Free formaldehyde | 0.9g/kg | 0.85g/kg |
To evaluate the properties of the aqueous sealant emulsions obtained in the above two examples, the following experiments were carried out: 700g of the aqueous sealing glue emulsion obtained in the two embodiments are respectively put into two containers, then 150g of anchoring emulsion T-139 of Shanghai Guangsheng chemical company, Inc., 150g of tertiary carbon emulsion T-1316 of Shanghai Guanggu chemical company, 2.5g of AMP-95 multifunctional auxiliary agent, 2g of 2875 wetting agent, 3g of silicon dioxide, 60g of NS-120 rosin emulsion, 5g of dipropylene glycol monomethyl ether, 0.5g of 8034A defoaming agent, 1.5g of preservative and 0.2g of thickener are respectively added, and after mixing, the mixture is uniformly stirred to obtain two aqueous sealing glue finished products.
Two samples of the finished water-based sealing glue are prepared according to the GB/T33320-2016 food packaging material and container adhesive standard, and are detected, and the detection results are shown in Table 2.
TABLE 2 bond Strength test results
| Index (I) | Standard requirements | EXAMPLE 1 finished sample | EXAMPLE 2 finished sample |
| Peel strength | Substrate destruction | Substrate destruction | Substrate destruction |
The test data in Table 2 show that the water-based sealing compound prepared by compounding the emulsion has high bonding strength.
Two samples of the finished product of the water-based sealing compound were tested using a constant temperature and humidity test chamber, and the test results are shown in table 3.
TABLE 3 test results of heat resistance and Low temperature resistance
The test data in Table 3 show that the water-based sealing adhesive prepared by compounding the emulsion has good heat resistance and frost resistance.
Claims (6)
1. The water-based sealing adhesive emulsion is characterized by comprising the following components in parts by weight:
total amount of 1096.4 kg;
the preparation method of the water-based sealing adhesive emulsion comprises the following steps:
1) dissolving 0.5kg of initiator in 5kg of water to obtain a primary initiator; dissolving 2.5kg of initiator in 45kg of water to obtain a drop of initiator; dissolving 0.2kg of initiator in 5kg of water to obtain a post initiator; dissolving 0.5kg of sodium bisulfite in 10kg of water to obtain a reducing agent;
mixing 400kg of butyl acrylate, 150kg of vinyl acetate, 15kg of 2-hydroxyethyl acrylate, 1kg of acrylic acid and 1.2kg of n-dodecyl mercaptan and uniformly stirring to obtain a mixed monomer;
2) adding 420kg of water and 17.5kg of polyvinyl alcohol into a reaction kettle, starting stirring, heating to 92 ℃, and stirring to disperse the polyvinyl alcohol until the polyvinyl alcohol is completely dissolved;
3) cooling, keeping the temperature between 75 and 80 ℃, sequentially adding 2.2kg of sodium bicarbonate, 18kg of emulsifier and an initial initiator, and then dropwise adding the mixed monomer and the initial initiator at a constant speed for 6 hours; then dropwise adding the post initiator at a constant speed for 0.5 hour;
4) heating, keeping the temperature between 80 and 85 ℃, stirring at medium speed, and keeping the temperature for 1 hour;
5) then cooling, when the temperature is reduced to 75 ℃, slowly adding a sodium bisulfite solution in a uniform speed for 15 minutes, then cooling to 40 ℃, and sequentially adding 0.8kg of defoaming agent and 2kg of preservative;
6) after being mixed evenly, the mixture is discharged and filtered, and the water-based sealing adhesive emulsion with the Tg of-35 ℃ is obtained.
2. The aqueous sealant emulsion of claim 1, wherein the polyvinyl alcohol is a mixture of one or more of PVA1788, PVA0588, PVA1792 and PVA1799 at any ratio.
3. The aqueous sealing adhesive emulsion of claim 1, wherein the emulsifier is one or a mixture of two or more of alkyl sulfate, polyoxyethylene ether sulfosuccinate and fatty alcohol-polyoxyethylene ether in any ratio.
4. The aqueous capstock emulsion of claim 1, wherein the initiator is one of potassium persulfate, sodium persulfate, or ammonium persulfate.
5. The aqueous sealant emulsion of claim 1 wherein the defoamer is polydimethylsiloxane.
6. The aqueous sealant emulsion of claim 1 wherein the preservative is sodium benzoate.
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| CN109181588A (en) * | 2018-09-11 | 2019-01-11 | 广东天元实业集团股份有限公司 | A kind of logistic label glue, preparation method and application |
| CN110964464A (en) * | 2019-10-22 | 2020-04-07 | 山东宇龙高分子科技有限公司 | Preparation method of marble adhesive |
| CN113150722A (en) * | 2021-02-25 | 2021-07-23 | 广东银洋环保新材料有限公司 | Adhesive for PVC tablecloth and preparation method thereof |
| CN114854339A (en) * | 2022-06-17 | 2022-08-05 | 南京百聚科技有限公司 | Water-based sealing adhesive for bonding PET (polyethylene terephthalate) and BOPP (biaxially-oriented polypropylene) base materials and preparation method thereof |
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| CN106479408B (en) * | 2016-09-27 | 2018-09-11 | 威远翰林科技有限公司 | The preparation method of aqueous sealing compound gluing agent emulsion |
| CN106366985A (en) * | 2016-09-27 | 2017-02-01 | 威远翰林科技有限公司 | Water-based sealing compound adhesive emulsion and preparation method thereof |
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| 纸品包装类封口胶使用状况的探讨;重庆科亚合成化工有限公司;《中国包装》;20040430;第82-83页 * |
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