CN112812710A - Preparation method of environment-friendly modified EVA (ethylene-vinyl acetate) adhesive, adhesive and packaging product - Google Patents
Preparation method of environment-friendly modified EVA (ethylene-vinyl acetate) adhesive, adhesive and packaging product Download PDFInfo
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- CN112812710A CN112812710A CN202110080013.4A CN202110080013A CN112812710A CN 112812710 A CN112812710 A CN 112812710A CN 202110080013 A CN202110080013 A CN 202110080013A CN 112812710 A CN112812710 A CN 112812710A
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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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/26—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers modified by chemical after-treatment
- C09J123/36—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers modified by chemical after-treatment by reaction with compounds containing nitrogen, e.g. by nitration
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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
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
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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
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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Abstract
The invention relates to a preparation method of an environment-friendly modified EVA adhesive, the adhesive and a packaging product, wherein the method comprises the following steps: s1, adding isocyanate and EVA emulsion into a solvent, heating to a first temperature, and reacting to obtain a material A; s2, continuously heating the material A to a second temperature which is at least 30 ℃ higher than the first temperature, keeping the temperature, adding titanium acetylacetonate at the second temperature, reacting, and cooling to obtain the environment-friendly modified EVA adhesive. According to the invention, the EVA emulsion is modified to replace solid EVA hot melt adhesive, and isocyanate and titanium acetylacetonate are introduced to modify EVA, so that the content of EVA plastics in the packaging bag is greatly reduced on the premise of not reducing the bonding strength of the EVA adhesive, the environmental protection property of the packaging bag is improved, and the attractiveness and market competitiveness of high-grade luxury packaging bags are improved to a great extent.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a preparation method of an environment-friendly modified EVA adhesive, an adhesive and a packaging system.
Background
In the field of luxury goods, in order to improve the aesthetic property and market competitiveness of products, upscale paper bags are mainly used to replace plastic bags as upscale luxury packaging bags, and upscale paper packaging bags are mainly composed of paper bags and nylon handles, and hot melt adhesives are generally used as adhesives to bond the handles and the packaging bags together in the connection of the upscale paper bags and the upscale paper bags. However, the hot melt adhesive leaves a large amount of plastic components in the packaging bag, which results in that the environmental protection performance of the packaging bag is not over-critical and the environment is polluted greatly.
Patent document CN111909508A discloses a copolyamide hot-melt resin and a preparation method thereof, wherein the copolyamide hot-melt resin comprises the following components in parts by weight: caprolactam: 80-120 parts of a solvent; nylon 66 salt: 80-100 parts of a solvent; and (3) modifying EVA: 10-20 parts; the modified ethylene-vinyl acetate copolymer is EVA resin with amide groups. The resin is obtained through chemical copolymerization modification, the melting point can be effectively reduced, large-dose addition is not needed, and the obtained copolymer resin also has an amide group on a branched chain, so that the hot-melt adhesive bonding with a nylon material has a better effect.
The patent document with publication number CN111647374A discloses a modified EVA hot melt adhesive and a preparation method thereof, wherein the modified EVA hot melt adhesive is prepared from the following raw materials in parts by weight: 25-30 parts of EVA resin, 5-10 parts of POP resin, 5-10 parts of APAO resin, 35-45 parts of tackifying resin, 15-20 parts of lubricant and 0.3-1 part of antioxidant; the tackifying resin is styrene modified carbon-five petroleum resin and rosin pentaerythritol ester; the lubricant is one or more of polyethylene wax, Fischer-Tropsch wax and microcrystalline wax.
The two modified hot melt resins improve the characteristics of the EVA resin by introducing a new branched side group into an EVA molecular chain. Modified EVA can have better compatibility with nylon molecules because molecular structure is similar, and modified EVA can fully disperse between nylon molecules, obtains the resin through chemical copolymerization modification, can effectively reduce the melting point, does not need the large-dose to add to the copolymer resin who obtains also has the acylamino on the branch chain, makes like this and nylon materials's hot melt bonding have better effect. The high and low temperature resistance and the binding power to cartons of the existing EVA adhesive are greatly improved by introducing the polyolefin plastomer POP and the amorphous alpha olefin copolymer APAO.
The two modification modes improve the performance of the EVA adhesive to a certain extent, but the problem of low environmental protection caused by overhigh solid content of resin of the hot melt adhesive is not solved, and the essential problem is not solved.
Disclosure of Invention
In order to solve the problem, the EVA emulsion is modified to replace solid EVA hot melt adhesive, and isocyanate and titanium acetylacetonate are introduced to modify EVA, so that the content of EVA plastics in the packaging bag is greatly reduced on the premise of not reducing the bonding strength of the EVA adhesive, the environmental protection property of the packaging bag is improved, and the attractiveness and market competitiveness of high-grade luxury packaging bags are greatly improved.
The EVA emulsion has high fluidity, particularly when the mass proportion of vinyl acetate in the ethylene-vinyl acetate copolymer is 20-45%, toluene is used as a solvent, the mass concentration of the toluene in the emulsion is 2-10%, and after the EVA emulsion reacts with isocyanate, the obtained colloid has low viscosity and high fluidity and is difficult to apply to the bonding of a packaging product. In general, in order to enhance the viscosity of the product, auxiliaries such as fillers, polyols or acids are introduced into the reaction system, however, after the auxiliaries participate in the reaction, the solid content of the resin in the colloid is often further increased.
In the invention, isocyanate and EVA emulsion are reacted at a first temperature, preferably 30-40 ℃, for 10-30min, the reaction temperature is low, the time is short, the isocyanate and the EVA emulsion are primarily combined, and the formed material A is liquid with high fluidity. After heating to a second temperature, which is at least 30 c, preferably 60-80 c, above the first temperature, the reaction time is 30-90min, for example 65 c, 70 c or 75 c, the reaction time is 40, 50,60,70, or 80 min. At higher temperatures and under the action of titanium acetylacetonate, the material A is gradually converted into a white viscous liquid which has low flowability and is convenient for packaging applications, in particular for gluing luxury packaging bags. After drying, the shearing strength of the adhesive layer formed by the environment-friendly modified EVA adhesive is more than or equal to 160N, so that the use requirement of the packaging bag is met.
The other key point of the invention is the optimization of the mixture ratio of the raw materials, preferably, the mass ratio of the isocyanate, the EVA emulsion and the titanium acetylacetonate is (300- & gt 700): (50-300): (1-15), more preferably (400- & 600): (100-200): (3-12), for example 420:150:6, or 450:180: 9. The EVA emulsion is a high-molecular emulsion which is prepared by using vinyl acetate and ethylene monomers as basic raw materials and copolymerizing the vinyl acetate and other auxiliary materials by an emulsion polymerization method, and mainly comprises ethylene-vinyl acetate copolymer and toluene, wherein the purity of the ethylene-vinyl acetate copolymer is greater than or equal to 99 wt%, the mass proportion of the vinyl acetate in the ethylene-vinyl acetate copolymer is 20-45%, and the mass concentration of the toluene in the emulsion is 2-10%.
The invention also provides a preparation method of the environment-friendly modified EVA adhesive, and the prepared environment-friendly modified EVA adhesive; and packaging products, such as packaging bags, packaging boxes, gift boxes, packaging boxes and the like, obtained by adopting the environment-friendly modified EVA adhesive for bonding.
The specific scheme is as follows:
a preparation method of an environment-friendly modified EVA adhesive comprises the following steps:
s1, adding isocyanate and EVA emulsion into a solvent, heating to a first temperature, and reacting to obtain a material A;
s2, continuously heating the material A to a second temperature which is at least 30 ℃ higher than the first temperature, keeping the temperature, adding titanium acetylacetonate at the second temperature, reacting, and cooling to obtain the environment-friendly modified EVA adhesive.
Further, the EVA emulsion is a solution containing ethylene-vinyl acetate copolymer, and the mass proportion of vinyl acetate in the ethylene-vinyl acetate copolymer is 20-45%.
Further, the mass ratio of the isocyanate, the EVA emulsion and the titanium acetylacetonate is (50-300): (300-700): (1-15);
optionally, the solvent is toluene or xylene, isocyanate: the mass ratio of the solvent is (5-30): (1-15).
Further, the first temperature is 30-40 ℃, and the reaction time is 10-30 min.
Further, the second temperature is 60-80 ℃, and the reaction time is 30-90 min.
Further, the titanium acetylacetonate is a uniform solution formed by dispersing the titanium acetylacetonate in toluene or xylene, heating to 150-180 ℃ and stirring for 10-30min to fully dissolve the titanium acetylacetonate.
The invention also protects the environment-friendly modified EVA adhesive prepared by applying the preparation method of the environment-friendly modified EVA adhesive.
Furthermore, the environment-friendly modified EVA adhesive is white viscous liquid, and the shear strength of an adhesive layer formed after drying is more than or equal to 160N.
The invention also protects a packaging product which is bonded by adopting the environment-friendly modified EVA adhesive.
Has the advantages that:
according to the preparation method of the environment-friendly modified EVA adhesive, isocyanate and titanium acetylacetonate are added into the EVA emulsion in a certain proportion, the polymerization degree is controlled by combining a process, the adhesive with higher shear strength is obtained, and the adhesive can be used for bonding a handle and a bag body in a high-grade luxury packaging bag, so that the content of plastic resin in the high-grade luxury packaging bag is reduced, the higher connection strength is ensured, the environmental friendliness of the high-grade luxury packaging bag is improved, and the core competitiveness of the product is greatly improved.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available. In the following examples, "%" means weight percent, unless otherwise specified.
The EVA emulsion used in the examples was purchased from Aquyu adhesive products Co., Ltd, manufactured under the trade name H3313FJ, in which the ethylene-vinyl acetate copolymer had a mass concentration of 94%.
Example 1
The preparation method of the environment-friendly modified EVA adhesive comprises the following steps:
s1, adding 0.2g of dimethylbenzene into a reaction kettle, heating to 30 ℃ under the stirring condition, and then adding 1g of isocyanate and 5g of EVA emulsion, and reacting for 15 min;
s2, adding 0.2g of xylene and 0.05g of titanium acetylacetonate into a reaction kettle, fully heating to 150 ℃, and stirring for 10min to fully dissolve the titanium acetylacetonate;
s3, continuously heating the reaction liquid obtained in the step S1 to 70 ℃, stopping heating, adding the titanium acetylacetonate solution obtained in the step S2 at the temperature, and fully stirring for reaction for 30 min;
and S4, cooling the reaction solution to room temperature after the reaction is finished, and obtaining the environment-friendly modified EVA adhesive. The main performance indexes are as follows:
appearance: milky viscous liquid
And (3) storage period: more than or equal to 3 months
The shear strength test is carried out by using a 10cm by 2mm aluminum plate, the prepared EVA adhesive is coated on the aluminum plate, the dried EVA adhesive is dried for 12 hours, and then the tensile test is carried out by using a 5KN universal testing machine, wherein the main performance indexes are as follows:
coating thickness: 0.7mm
Gluing area: 1.5cm by 10cm
Shear strength: 183N
Compared with the conventional solid EVA hot melt adhesive, the EVA adhesive prepared by the invention is liquid glue, has better spreadability on the surface of the packaging bag, reduces the coating thickness and simultaneously improves the coating area, thereby obtaining more excellent coating effect.
Therefore, the EVA adhesive prepared by the invention is adopted to paste the packaging material, so that the use amount of glue is greatly reduced, and the aim of reducing the content of EVA plastic resin in the packaging bag is fulfilled; meanwhile, the same adhesive force is required to be achieved, and the coating amount only accounts for 20-40% of the mass of the solid EVA hot melt adhesive, so that the adhesive strength formed after the prepared EVA adhesive is cured is higher under the condition of the same dosage.
Example 2
A modified EVA adhesive was prepared according to the method of example 1, except that the heating temperature in S1 was changed to 35 ℃, and the main performance indices were as follows:
appearance: milky viscous liquid
And (3) storage period: more than or equal to 3 months
The shear strength test is carried out by using a 10cm by 2mm aluminum plate, the prepared EVA adhesive is coated on the aluminum plate, the dried EVA adhesive is dried for 12 hours, and then the tensile test is carried out by using a 5KN universal testing machine, wherein the main performance indexes are as follows:
coating thickness: 0.7mm
Gluing area: 1.5cm by 10cm
Shear strength: 191N
Example 3
A modified EVA adhesive was prepared as in example 1, except that the amount of titanium acetylacetonate added in S2 was changed to 0.1g, and the main performance criteria were as follows:
appearance: milky viscous liquid
And (3) storage period: more than or equal to 3 months
The shear strength test is carried out by using a 10cm by 2mm aluminum plate, the prepared EVA adhesive is coated on the aluminum plate, the dried EVA adhesive is dried for 12 hours, and then the tensile test is carried out by using a 5KN universal testing machine, wherein the main performance indexes are as follows:
coating thickness: 0.7mm
Gluing area: 1.5cm by 10cm
Shear strength: 212N
Example 4
A modified EVA adhesive was prepared as in example 1, except that the amount of isocyanate added in S1 was changed to 0.8g, and the main performance criteria were as follows:
appearance: milky viscous liquid
And (3) storage period: more than or equal to 3 months
The shear strength test is carried out by using a 10cm by 2mm aluminum plate, the prepared EVA adhesive is coated on the aluminum plate, the dried EVA adhesive is dried for 12 hours, and then the tensile test is carried out by using a 5KN universal testing machine, wherein the main performance indexes are as follows:
coating thickness: 0.7mm
Gluing area: 1.5cm by 10cm
Shear strength: 165N
Example 5
A modified EVA adhesive was prepared as in example 1, except that the amount of EVA emulsion in S1 was changed to 6g, and the main performance criteria were as follows:
appearance: milky viscous liquid
And (3) storage period: more than or equal to 3 months
The shear strength test is carried out by using a 10cm by 2mm aluminum plate, the prepared EVA adhesive is coated on the aluminum plate, the dried EVA adhesive is dried for 12 hours, and then the tensile test is carried out by using a 5KN universal testing machine, wherein the main performance indexes are as follows:
coating thickness: 0.7mm
Gluing area: 1.5cm by 10cm
Shear strength: 187N
Example 6
A modified EVA adhesive was prepared as in example 1, except that the heating temperature in S1 was changed to 40 deg.C, and the amount of isocyanate added was changed to 1.2g, with the following main performance criteria:
appearance: milky viscous liquid
And (3) storage period: more than or equal to 3 months
The shear strength test is carried out by using a 10cm by 2mm aluminum plate, the prepared EVA adhesive is coated on the aluminum plate, the dried EVA adhesive is dried for 12 hours, and then the tensile test is carried out by using a 5KN universal testing machine, wherein the main performance indexes are as follows:
coating thickness: 0.7mm
Gluing area: 1.5cm by 10cm
Shear strength: 221N
Comparative example 1
Comparative EVA adhesive 1 was prepared by the following steps:
s1, adding 0.2g of dimethylbenzene into a reaction kettle, heating to 30 ℃ under the stirring condition, and then adding 1g of isocyanate and 5g of EVA emulsion, and reacting for 15 min;
s2, continuing to heat the reaction solution obtained in the step S1 to 70 ℃, stopping heating, and fully stirring and reacting at the temperature for 30 min;
and S3, cooling the reaction solution to room temperature after the reaction is finished, and obtaining the comparative EVA adhesive 1. The main performance indexes are as follows:
appearance: milky white liquid with fluidity
The shear strength test is carried out by using a 10cm by 2mm aluminum plate, the prepared product is coated on the aluminum plate, dried for 12 hours and then subjected to a tensile test by using a 5KN universal testing machine, and the main performance indexes are as follows:
coating thickness: 0.7mm
Gluing area: 1.5cm by 10cm
Shear strength: 125N
Comparative example 2
A comparative EVA adhesive 2 was prepared with the following steps:
s1, adding 0.2g of dimethylbenzene into a reaction kettle, heating to 30 ℃ under the stirring condition, and then adding 1g of isocyanate and 5g of EVA emulsion, and reacting for 15 min;
s2, continuously heating the reaction liquid obtained in the step S1 to 70 ℃, stopping heating, adding a silane coupling agent KH-550 at the temperature, and fully stirring for reaction for 30 min;
and S3, cooling the reaction solution to room temperature after the reaction is finished, and obtaining the comparative EVA adhesive 2. The main performance indexes are as follows:
appearance: milky white liquid with fluidity
The shear strength test is carried out by using a 10cm by 2mm aluminum plate, the prepared product is coated on the aluminum plate, dried for 12 hours and then subjected to a tensile test by using a 5KN universal testing machine, and the main performance indexes are as follows:
coating thickness: 0.7mm
Gluing area: 1.5cm by 10cm
Shear strength: 121N
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (9)
1. A preparation method of an environment-friendly modified EVA adhesive is characterized by comprising the following steps: the method comprises the following steps:
s1, adding isocyanate and EVA emulsion into a solvent, heating to a first temperature, and reacting to obtain a material A;
s2, continuously heating the material A to a second temperature which is at least 30 ℃ higher than the first temperature, keeping the temperature, adding titanium acetylacetonate at the second temperature, reacting, and cooling to obtain the environment-friendly modified EVA adhesive.
2. The preparation method of the environment-friendly modified EVA adhesive according to claim 1, wherein the preparation method comprises the following steps: the EVA emulsion is a solution containing an ethylene-vinyl acetate copolymer, and the mass proportion of vinyl acetate in the ethylene-vinyl acetate copolymer is 20-45%.
3. The preparation method of the environment-friendly modified EVA adhesive according to claim 2, wherein the preparation method comprises the following steps: the mass ratio of the isocyanate, the EVA emulsion and the titanium acetylacetonate is (50-300): (300-700): (1-15);
optionally, the solvent is toluene or xylene, isocyanate: the mass ratio of the solvent is (5-30): (1-15).
4. The preparation method of the environment-friendly modified EVA adhesive according to claim 1, wherein the preparation method comprises the following steps: the first temperature is 30-40 ℃, and the reaction time is 10-30 min.
5. The preparation method of the environment-friendly modified EVA adhesive according to claim 1 or 4, wherein: the second temperature is 60-80 ℃, and the reaction time is 30-90 min.
6. The preparation method of the environment-friendly modified EVA adhesive according to claim 1, wherein the preparation method comprises the following steps: the titanium acetylacetonate is a uniform solution formed by dispersing the titanium acetylacetonate into toluene or xylene, heating to the temperature of 150-180 ℃, and stirring for 10-30min to fully dissolve the titanium acetylacetonate.
7. The environment-friendly modified EVA adhesive is prepared by the method for preparing the environment-friendly modified EVA adhesive of claim 1.
8. The environment-friendly modified EVA adhesive of claim 7, wherein: the environment-friendly modified EVA adhesive is white viscous liquid, and the shear strength of an adhesive layer formed after drying is more than or equal to 160N.
9. A packaging article bonded by the environment-friendly modified EVA adhesive of claim 7 or 8.
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| CN202110080013.4A CN112812710A (en) | 2021-01-21 | 2021-01-21 | Preparation method of environment-friendly modified EVA (ethylene-vinyl acetate) adhesive, adhesive and packaging product |
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| CN202110080013.4A CN112812710A (en) | 2021-01-21 | 2021-01-21 | Preparation method of environment-friendly modified EVA (ethylene-vinyl acetate) adhesive, adhesive and packaging product |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1072058A (en) * | 1963-09-14 | 1967-06-14 | Basf Ag | Production of copolymers of vinyl glycols and other ethylenically unsaturated compounds |
| CN87101990A (en) * | 1986-03-17 | 1987-11-25 | 武田药品工业株式会社 | The composition that is used for carpet backings |
| CN109927146A (en) * | 2017-12-18 | 2019-06-25 | 万华化学集团股份有限公司 | A kind of isocyanate adhesive system and the method for wood-based plate and the wood-based plate of preparation are prepared with it |
| CN110494463A (en) * | 2017-03-29 | 2019-11-22 | Sika技术股份公司 | With the aqueous composition for improving mechanical performance |
-
2021
- 2021-01-21 CN CN202110080013.4A patent/CN112812710A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1072058A (en) * | 1963-09-14 | 1967-06-14 | Basf Ag | Production of copolymers of vinyl glycols and other ethylenically unsaturated compounds |
| CN87101990A (en) * | 1986-03-17 | 1987-11-25 | 武田药品工业株式会社 | The composition that is used for carpet backings |
| CN110494463A (en) * | 2017-03-29 | 2019-11-22 | Sika技术股份公司 | With the aqueous composition for improving mechanical performance |
| CN109927146A (en) * | 2017-12-18 | 2019-06-25 | 万华化学集团股份有限公司 | A kind of isocyanate adhesive system and the method for wood-based plate and the wood-based plate of preparation are prepared with it |
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