CN115627134A - Low-temperature-resistant EVA hot melt adhesive and preparation method and application thereof - Google Patents

Low-temperature-resistant EVA hot melt adhesive and preparation method and application thereof Download PDF

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Publication number
CN115627134A
CN115627134A CN202211269661.5A CN202211269661A CN115627134A CN 115627134 A CN115627134 A CN 115627134A CN 202211269661 A CN202211269661 A CN 202211269661A CN 115627134 A CN115627134 A CN 115627134A
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China
Prior art keywords
parts
temperature
hot melt
melt adhesive
rosin
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CN202211269661.5A
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Chinese (zh)
Inventor
杨礼快
方晨
喻世华
朱健民
温正豹
王翔宇
陈斐
牛倩倩
王海伟
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Gettel Group Yunyang Plastic Co ltd
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Gettel Group Yunyang Plastic Co ltd
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Priority to CN202211269661.5A priority Critical patent/CN115627134A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04Homopolymers or copolymers of ethene
    • C09J123/08Copolymers of ethene
    • C09J123/0846Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C09J123/0853Vinylacetate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09FNATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
    • C09F1/00Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
    • C09F1/04Chemical modification, e.g. esterification
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention belongs to the technical field of hot melt adhesives, and particularly relates to a low-temperature-resistant EVA hot melt adhesive and a preparation method thereof, wherein the low-temperature-resistant EVA hot melt adhesive comprises the following components: 70-80 parts of ethylene-vinyl acetate copolymer, 5-9 parts of palmitic acid, 5-9 parts of rosin, 1-2 parts of antioxidant, 2-4 parts of glycerol, 1-2 parts of softener and 3-5 parts of petroleum resin, wherein the palmitic acid and the glycerol are used as raw materials to modify rosin powder, and the antioxidant is added to synthesize rosin glycerol palm ester, the rosin glycerol palm ester and the softener naphthenic oil are mixed with the ethylene-vinyl acetate copolymer together, the vitrification temperature of the obtained EVA hot melt adhesive is reduced through proper mixing temperature and time, so that the lowest temperature at which the chain segments of the EVA hot melt adhesive can move is reduced, the flexibility of the EVA hot melt adhesive is increased, the EVA hot melt adhesive can be normally used and stored under the low-temperature condition, and the EVA hot melt adhesive is more suitable for being used in regions with lower temperature.

Description

Low-temperature-resistant EVA hot melt adhesive and preparation method and application thereof
Technical Field
The invention relates to the technical field of hot melt adhesives, in particular to a low-temperature-resistant EVA hot melt adhesive and a preparation method thereof.
Background
In recent years, EVA hot melt adhesives have been widely used in many fields such as books, packaging and wood. The EVA hot melt adhesive system has wide adhesion applicability and good adhesion effect on non-polar materials such as polypropylene, polyethylene and the like, has the problem of poor aging resistance in the use and storage processes of the EVA hot melt adhesive, brings inconvenience to related users in use and storage, and particularly in a state of low room temperature, the aging resistance of the EVA hot melt adhesive is further reduced due to the influence of low ambient temperature, so that the peeling strength of the EVA hot melt adhesive is reduced when the EVA hot melt adhesive is used as a functional layer of a non-adhesive film, and the integral service performance of the non-adhesive film is influenced.
Disclosure of Invention
The invention aims to provide a low-temperature-resistant EVA hot melt adhesive and a preparation method thereof so as to solve the technical problems mentioned in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the low-temperature-resistant EVA hot melt adhesive comprises the following components in parts by weight: 70-80 parts of ethylene-vinyl acetate copolymer, 5-9 parts of palmitic acid, 5-9 parts of rosin, 1-2 parts of antioxidant, 2-4 parts of glycerol, 1-2 parts of softener and 3-5 parts of petroleum resin.
Preferably, the composition and the parts by weight are as follows: 72-79 parts of ethylene-vinyl acetate copolymer, 6-7 parts of palmitic acid, 6-7 parts of rosin, 1 part of antioxidant, 3 parts of glycerol, 1 part of softener and 4 parts of petroleum resin.
Preferably, the composition and the parts by weight are as follows: 74 parts of ethylene-vinyl acetate copolymer, 8 parts of palmitic acid, 8 parts of rosin, 1 part of antioxidant, 3 parts of glycerol, 1 part of softener and 4 parts of petroleum resin.
Preferably, the rosin is industrial horsetail rosin.
Preferably, the softening agent is naphthenic oil.
Preferably, the antioxidant is a phenolic antioxidant.
A preparation method of low-temperature-resistant EVA hot melt adhesive comprises the following steps:
step 1:
pulverizing rosin into powder, mixing palmitic acid, glycerol and rosin, adding antioxidant, stirring at 200-250 deg.C until the materials are uniformly stirred, keeping the temperature at 210 deg.C for 5h, and naturally cooling to obtain modified rosin glycerol palmitate;
step 2:
adding the modified rosin glycerol palm ester obtained in the step 1 and a softening agent into an ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 120-135 ℃, and the mixing time is 40-70min;
and step 3:
adding petroleum resin into the mixture obtained in the step 2, continuously mixing, keeping the mixing temperature of the step 2, continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
An application of a low-temperature-resistant EVA hot melt adhesive, which is applied to adhesive-free film lamination.
The invention has the beneficial effects that: the low-temperature resistant EVA hot melt adhesive and the preparation method thereof are characterized in that palmitic acid and glycerol are used as raw materials to modify rosin powder, and simultaneously antioxidant is added to synthesize rosin glycerol palm ester, the rosin glycerol palm ester and softening agent naphthenic oil are mixed with ethylene-vinyl acetate copolymer together, the vitrification temperature of the obtained EVA hot melt adhesive is reduced through proper mixing temperature and time, the lowest temperature at which an EVA hot melt adhesive chain segment can move is reduced, the flexibility of the EVA hot melt adhesive is increased, so that the EVA hot melt adhesive can be normally used and stored under the low-temperature condition, and the EVA hot melt adhesive is more suitable for being used in regions with lower air temperature.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
step 1:
crushing 5 parts of rosin into powder, mixing 5 parts of palmitic acid, 2 parts of glycerol and the rosin, adding 1 part of antioxidant, continuously stirring at 210 ℃ until the materials are uniformly stirred, preserving heat at 210 ℃ for 5 hours, and naturally cooling after the heat preservation is finished to obtain modified rosin glycerol palm ester;
step 2:
adding the modified rosin glycerol palm ester obtained in the step 1 and 1 part of softener into 70 parts of ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 120 ℃, and the mixing time is 70min;
and 3, step 3:
and 3, adding 3 parts of petroleum resin into the mixture obtained in the step 2, continuously mixing, keeping the mixing temperature of the step 2, continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
Wherein: the rosin is industrial horsetail rosin; the softener is naphthenic oil; the antioxidant is phenolic antioxidant.
Example 2:
step 1:
crushing 6 parts of rosin into powder, mixing 6 parts of palmitic acid, 3 parts of glycerol and the rosin, adding 1 part of antioxidant, continuously stirring at 210 ℃ until the materials are uniformly stirred, preserving heat at 210 ℃ for 5 hours, and naturally cooling after the heat preservation is finished to obtain modified rosin glycerol palmitate;
step 2:
adding the modified rosin glycerol palm ester obtained in the step 1 and 1 part of softener into 72 parts of ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 130 ℃, and the mixing time is 50min;
and 3, step 3:
and (3) adding 4 parts of petroleum resin into the mixture obtained in the step (2) and continuously mixing, keeping the mixing temperature in the step (2), continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
Wherein: the rosin is industrial horsetail rosin; the softener is naphthenic oil; the antioxidant is a phenolic antioxidant.
Example 3:
step 1:
crushing 6 parts of rosin into powder, mixing 6 parts of palmitic acid, 3 parts of glycerol and the rosin, adding 1 part of antioxidant, continuously stirring at 220 ℃, keeping the temperature for 5 hours at 210 ℃ until the materials are uniformly stirred, and naturally cooling to obtain modified rosin glycerol palm ester after the heat preservation is finished;
step 2:
adding the modified rosin glycerol palm ester obtained in the step 1 and 1 part of softener into 74 parts of ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 130 ℃, and the mixing time is 50min;
and step 3:
and (3) adding 4 parts of petroleum resin into the mixture obtained in the step (2) and continuously mixing, keeping the mixing temperature in the step (2), continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
Wherein: the rosin is industrial horsetail rosin; the softener is naphthenic oil; the antioxidant is phenolic antioxidant.
Example 4:
step 1:
crushing 7 parts of rosin into powder, mixing 7 parts of palmitic acid, 3 parts of glycerol and the rosin, adding 1 part of antioxidant, continuously stirring at the temperature of 250 ℃ until the materials are uniformly stirred, preserving heat at the temperature of 210 ℃ for 5 hours, and naturally cooling after the heat preservation is finished to obtain modified rosin glycerol palmitate;
and 2, step:
adding the modified rosin glycerol palm ester obtained in the step 1 and 1 part of softener into 79 parts of ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 135 ℃, and the mixing time is 40min;
and step 3:
and (3) adding 4 parts of petroleum resin into the mixture obtained in the step (2) and continuously mixing, keeping the mixing temperature in the step (2), continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
Wherein: the rosin is industrial horsetail rosin; the softener is naphthenic oil; the antioxidant is a phenolic antioxidant.
Example 5:
step 1:
crushing 9 parts of rosin into powder, mixing 9 parts of palmitic acid, 4 parts of glycerol and the rosin, adding 2 parts of antioxidant, continuously stirring at 240 ℃, keeping the temperature for 5 hours at 210 ℃ until the materials are uniformly stirred, and naturally cooling to obtain modified rosin glycerol palm ester after the heat preservation is finished;
and 2, step:
adding the modified rosin glycerol palm ester obtained in the step 1 and 2 parts of a softening agent into 80 parts of ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 130 ℃, and the mixing time is 50min;
and step 3:
and (3) adding 5 parts of petroleum resin into the mixture obtained in the step (2) for continuous mixing, keeping the mixing temperature in the step (2), continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
Wherein: the rosin is industrial horsetail rosin; the softener is naphthenic oil; the antioxidant is a phenolic antioxidant.
Comparative example 1:
step 1:
crushing 9 parts of rosin into powder, adding 2 parts of antioxidant, continuously stirring at 240 ℃ until the materials are uniformly stirred, preserving heat at 210 ℃ for 5 hours, and naturally cooling after heat preservation to obtain a mixture of the rosin and the antioxidant;
step 2:
adding the modified rosin glycerol palm ester obtained in the step 1 and 2 parts of a softening agent into 80 parts of ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 130 ℃, and the mixing time is 50min;
and step 3:
and (3) adding 5 parts of petroleum resin into the mixture obtained in the step (2) for continuous mixing, keeping the mixing temperature in the step (2), continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
Wherein: the rosin is industrial horsetail rosin; the softener is naphthenic oil; the antioxidant is a phenolic antioxidant.
Comparative example 2:
step 1:
crushing 9 parts of rosin into powder, mixing 9 parts of palmitic acid, 4 parts of glycerol and the rosin, adding 2 parts of antioxidant, continuously stirring at 240 ℃, keeping the temperature for 5 hours at 210 ℃ until the materials are uniformly stirred, and naturally cooling to obtain modified rosin glycerol palm ester after the heat preservation is finished;
and 2, step:
adding the modified rosin glycerol palm ester obtained in the step 1 and 2 parts of a softening agent into 80 parts of ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 130 ℃, and the mixing time is 90min;
and step 3:
and (3) adding 5 parts of petroleum resin into the mixture obtained in the step (2) for continuous mixing, keeping the mixing temperature in the step (2), continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
Wherein: the rosin is industrial horsetail rosin; the softener is naphthenic oil; the antioxidant is phenolic antioxidant.
Comparative example 3:
step 1:
crushing 9 parts of rosin into powder, mixing 9 parts of palmitic acid, 4 parts of glycerol and the rosin, adding 2 parts of antioxidant, continuously stirring at 240 ℃, keeping the temperature at 210 ℃ for 5 hours until the materials are uniformly stirred, and naturally cooling after the temperature is kept to obtain modified rosin glycerol palmitate;
step 2:
adding the modified rosin glycerol palm ester obtained in the step 1 and 2 parts of softener into 80 parts of ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 145 ℃, and the mixing time is 50min;
and 3, step 3:
and (3) adding 5 parts of petroleum resin into the mixture obtained in the step (2) for continuous mixing, keeping the mixing temperature in the step (2), continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
Wherein: the rosin is industrial horsetail rosin; the softener is naphthenic oil; the antioxidant is a phenolic antioxidant.
The low temperature resistant EVA hot melt adhesives prepared in the examples 1 to 5 and the comparative examples 1 to 3 are subjected to a test of peeling strength with a white paper card at the same temperature for measurement,
the results are as follows:
Figure BDA0003894642020000091
example 5 differs from comparative example 1 in that: the rosin is not treated;
example 5 differs from comparative example 2 in that: mixing time is different;
example 5 differs from comparative example 3 in that: the mixing temperature is different;
from the test results, it can be seen that the examples exhibited better peel strength than the comparative examples, and particularly, the peel strength was excellent at a lower room temperature, and the peel strength was more slowly decreased as the temperature was decreased.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. The utility model provides a low temperature resistant EVA hot melt adhesive which characterized in that: the composition comprises the following components in parts by weight: 70-80 parts of ethylene-vinyl acetate copolymer, 5-9 parts of palmitic acid, 5-9 parts of rosin, 1-2 parts of antioxidant, 2-4 parts of glycerol, 1-2 parts of softener and 3-5 parts of petroleum resin.
2. The low-temperature-resistant EVA hot melt adhesive of claim 1, which is characterized in that: the composition comprises the following components in parts by weight: 72-79 parts of ethylene-vinyl acetate copolymer, 6-7 parts of palmitic acid, 6-7 parts of rosin, 1 part of antioxidant, 3 parts of glycerol, 1 part of softener and 4 parts of petroleum resin.
3. The low-temperature-resistant EVA hot melt adhesive of claim 2, wherein: the composition comprises the following components in parts by weight: 74 parts of ethylene-vinyl acetate copolymer, 8 parts of palmitic acid, 8 parts of rosin, 1 part of antioxidant, 3 parts of glycerol, 1 part of softener and 4 parts of petroleum resin.
4. A low temperature resistant EVA hot melt adhesive according to any one of claims 1 to 3, characterized in that: the rosin is industrial horsetail rosin.
5. The low-temperature-resistant EVA hot melt adhesive according to any one of claims 1 to 3, characterized in that: the softener is naphthenic oil.
6. The low-temperature-resistant EVA hot melt adhesive according to any one of claims 1 to 3, characterized in that: the antioxidant is a phenolic antioxidant.
7. The preparation method of the low temperature resistant EVA hot melt adhesive according to any one of claims 1 to 3, characterized by comprising the following steps: the preparation method comprises the following steps:
step 1:
pulverizing rosin into powder, mixing glycerol, palmitic acid and rosin, adding antioxidant, stirring at 200-250 deg.C until the materials are uniformly stirred, keeping the temperature at 210 deg.C for 5h, and naturally cooling to obtain modified rosin glycerol palmitate;
step 2:
adding the modified rosin glycerol palm ester obtained in the step 1 and a softening agent into an ethylene-vinyl acetate copolymer for mixing, wherein the mixing temperature is 120-135 ℃, and the mixing time is 40-70min;
and 3, step 3:
adding petroleum resin into the mixture obtained in the step 2, continuously mixing, keeping the mixing temperature of the step 2, continuously mixing for 20min, and discharging to obtain the low-temperature-resistant EVA hot melt adhesive.
8. The application of the low-temperature-resistant EVA hot melt adhesive according to claim 7, wherein: the low-temperature-resistant EVA hot melt adhesive is applied to laminating of non-adhesive films.
CN202211269661.5A 2022-10-18 2022-10-18 Low-temperature-resistant EVA hot melt adhesive and preparation method and application thereof Pending CN115627134A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0255783A (en) * 1988-08-22 1990-02-26 Arakawa Chem Ind Co Ltd Hot melt adhesive composition
CN102676062A (en) * 2012-05-15 2012-09-19 普洱科茂林化有限公司 Low-temperature resistant rosin thickening resin, preparation method and usage thereof
CN102925080A (en) * 2012-11-29 2013-02-13 无锡市万力粘合材料有限公司 Book thermoplastic binding hot melt glue used at low temperature and preparation method thereof
CN108977123A (en) * 2018-06-29 2018-12-11 浙江固特热熔胶有限公司 A kind of low temperature resistant books and periodicals glue and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0255783A (en) * 1988-08-22 1990-02-26 Arakawa Chem Ind Co Ltd Hot melt adhesive composition
CN102676062A (en) * 2012-05-15 2012-09-19 普洱科茂林化有限公司 Low-temperature resistant rosin thickening resin, preparation method and usage thereof
CN102925080A (en) * 2012-11-29 2013-02-13 无锡市万力粘合材料有限公司 Book thermoplastic binding hot melt glue used at low temperature and preparation method thereof
CN108977123A (en) * 2018-06-29 2018-12-11 浙江固特热熔胶有限公司 A kind of low temperature resistant books and periodicals glue and preparation method thereof

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