CN112322232A - Ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive - Google Patents

Ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive Download PDF

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Publication number
CN112322232A
CN112322232A CN202011167668.7A CN202011167668A CN112322232A CN 112322232 A CN112322232 A CN 112322232A CN 202011167668 A CN202011167668 A CN 202011167668A CN 112322232 A CN112322232 A CN 112322232A
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China
Prior art keywords
hot melt
ethylene
melt adhesive
sbc
parts
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CN202011167668.7A
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Chinese (zh)
Inventor
王文敏
杭祖圣
朱志祥
寇波
明丹
沈丽琴
涂先兵
熊超
陈恩生
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Jiangsu Jaour Hot Melt Adhesive Co ltd
Nanjing Institute of Technology
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Jiangsu Jaour Hot Melt Adhesive Co ltd
Nanjing Institute of Technology
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Priority to CN202011167668.7A priority Critical patent/CN112322232A/en
Publication of CN112322232A publication Critical patent/CN112322232A/en
Pending legal-status Critical Current

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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
    • C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J153/02—Vinyl aromatic monomers and conjugated dienes
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • 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
    • C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J153/02—Vinyl aromatic monomers and conjugated dienes
    • C09J153/025—Vinyl aromatic monomers and conjugated dienes modified
    • 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
    • C09J157/00—Adhesives based on unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09J157/02—Copolymers of mineral oil hydrocarbons
    • 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
    • C09J193/00—Adhesives based on natural resins; Adhesives based on derivatives thereof
    • C09J193/04—Rosin
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to an ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive, belonging to the field of hot melt adhesive manufacture; the hot melt adhesive comprises the following raw materials in parts by weight: styrene Block Copolymers (SBC): 28-36 parts; ethylene-acrylic ionic polymer: 11-19 parts; tackifying resin: 15-35 parts; diluent agent: 16-24 parts; 0.5-3 parts of antioxidant. The ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive prepared by the invention has excellent peel strength, ageing resistance and durability, and meets the performance requirements of hot melt adhesives.

Description

Ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive
Technical Field
The invention relates to the field of hot melt adhesive manufacturing, in particular to an ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
Background
The hot melt adhesive has the outstanding advantages of environmental protection, safety, rapid curing, suitability for automatic production and the like, and is rapidly developed in more than ten years as a large variety with the most development potential in the adhesive industry. The hot melt adhesive is prepared by taking thermoplastic plastics or elastomers as a matrix and adding tackifying resin, antioxidant and the like. Hot melt adhesives melt and solidify rapidly during cooling, resulting in excellent mechanical strength. Compared with other adhesives, the hot melt adhesive does not contain a solvent, is convenient to synthesize, short in curing time, wide in bonding range, convenient to store and transport, free of environmental pollution and in line with the leading direction of green chemistry. Thermoplastic elastomer SBS has attracted considerable attention since the advent of 1963. Because of its good solubility, it can simplify the process and save energy, and is very suitable for preparing hot-melt adhesive, sealant and coating material. Therefore, SBC hot melt adhesives have the advantages of increasing varieties, improving performances and expanding application, have wide prospects, and are worthy of deep research and development.
Disclosure of Invention
The invention discloses an ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive, which aims at solving the problems of low heat resistance and poor aging resistance in the prior art.
The ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive is characterized by being prepared from the following components in parts by mass: styrene Block Copolymers (SBC): 28-36 parts; ethylene-acrylic ionic polymer: 11-19 parts; 15-35 parts of tackifying resin; diluent agent: 16-24 parts; 0.5-3 parts of antioxidant. Further, the SBC is one or a combination of SIS, SBS, SEBS, and SEPS.
The ethylene-acrylic acid ionic polymer is unsaturated sodium salt or zinc salt of copolymer of ethylene and acrylic acid, methacrylic acid and the like, and combination thereof.
Further the tackifying resin is rosin resin, petroleum resin or a combination thereof.
Further, 1-5 parts of maleic anhydride grafted styrene block copolymer as a compatilizer can be added.
Further the diluent is naphthenic oil, paraffinic oil or a combination.
Further, the antioxidant is amine and phenol antioxidants, phosphite and thiol antioxidants, or a combination of a plurality of antioxidants.
The invention also discloses a preparation method of the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive, which is characterized in that the preparation method can adopt a kneader or a reaction kettle, and the preparation method is as follows.
The preparation method adopts a kneader. Step one, setting the temperature of a kneader to be 160 ℃, and starting heating; step two, after the set temperature is reached, setting the rotating speed of a rotor to be 60rpm, then pouring SBC, the ethylene-acrylic acid ionic polymer and the antioxidant from a feed inlet, pressing a compression bar into the feed inlet, and mixing for 10 minutes; step three, continuously adding the compatilizer and the tackifying resin, and mixing for 5 minutes; continuously adding the diluent, and mixing for 5 minutes; and step four, stopping mixing uniformly, discharging and cooling to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
The preparation method adopts a reaction kettle. The method comprises the following steps: adding SBC, an ethylene-acrylic acid ionic polymer, an antioxidant, a compatilizer and a diluent into a stirring kettle, and stirring for 30-50 min at the temperature of 80-150 ℃ to obtain a mixture; step two: and (3) adding tackifying resin into the mixture obtained in the step one, stirring for 1-2 h at the temperature of 170-200 ℃, and filtering and removing bubbles to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
Compared with the prior art, the invention has the beneficial effects that:
1. in the invention, the ethylene-acrylic acid ionic polymer is added, so that the peel strength of the hot melt adhesive is improved, the application field of the ionic polymer is favorably expanded, and the ethylene-acrylic acid ionic polymer has important significance;
2. according to the invention, the addition of the ethylene-acrylic acid ionic polymer improves the damage self-healing capability and improves the aging resistance and durability of the hot melt adhesive.
3. The performance index of the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive prepared by the kneader or the reaction kettle meets the relevant standard specification, the whole production and preparation process of the product is simple, the manufacturing cost is reduced, the production efficiency is improved, and the economic benefit is improved.
Detailed Description
In order to better illustrate the invention, the following examples are given. It should be emphasized that the examples are not meant to limit the scope of the invention to the conditions described in the examples, which are intended to further illustrate the content of the invention and its feasibility.
Example 1:
the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive in the embodiment 1 is characterized in that the hot melt adhesive is prepared from the following components in parts by mass: styrene-butadiene-styrene copolymer (SBS): 28 parts of (1); ethylene-acrylic acid ionic polymer: 19 parts of a mixture; tackifying resin: 35 parts of (B); a compatilizer: 3 parts of a mixture; diluent agent: 24 parts of (1); and 1 part of antioxidant.
Wherein, the diluent is naphthenic oil; the antioxidant is an amine antioxidant.
The preparation method comprises the following steps:
step one, setting the temperature of a kneader to be 160 ℃, and starting heating;
step two, after the set temperature is reached, setting the rotating speed of a rotor to be 60rpm, then pouring SBS, the ethylene-acrylic acid ionic polymer and the antioxidant from a feeding port, and mixing for 20 minutes;
step three, continuously adding the compatilizer and the tackifying resin, and mixing for 10 minutes; continuously adding the diluent, and mixing for 10 minutes;
and step four, stopping mixing uniformly, discharging and cooling to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
Example 2:
the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive in embodiment 2 is characterized in that the hot melt adhesive is prepared from the following components in parts by mass: styrene-isoprene-styrene copolymer (SIS): 30 parts of (1); ethylene-methacrylic acid ionic polymer: 17 parts of (1); tackifying resin: 30 parts of (1); a compatilizer: 4 parts of a mixture; diluent agent: 22 parts of (A); and 2 parts of an antioxidant.
Wherein the diluent is paraffin oil; the antioxidant is a phenol antioxidant.
The preparation method comprises the following steps:
the method comprises the following steps: adding SIS, ethylene-methacrylic acid ionic polymer, antioxidant, compatilizer and diluent into a stirring kettle, and stirring at 150 ℃ for 30min to obtain a mixture;
step two: and (3) adding tackifying resin into the mixture obtained in the step one, stirring for 1-2 h at the temperature of 180 ℃, and filtering and removing bubbles to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
Example 3:
the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive in embodiment 3 is characterized in that the hot melt adhesive is prepared from the following components in parts by mass: styrene- (ethylene-butylene) -styrene copolymer (SEBS): 32 parts of (1); ethylene-acrylic ionic polymer: 15 parts of (1); tackifying resin: 25 parts of (1); a compatilizer: 2 parts of (1); diluent agent: 20 parts of (1); and 3 parts of an antioxidant.
Wherein the diluent is white wax oil; the antioxidant is phosphite ester antioxidant.
The preparation method comprises the following steps:
step one, setting the temperature of a kneader to be 160 ℃, and starting heating;
step two, after the set temperature is reached, setting the rotating speed of a rotor to be 60rpm, then pouring the SEBS, the ethylene-acrylic acid ionic polymer and the antioxidant from a feeding port, and mixing for 20 minutes;
step three, continuously adding the compatilizer and the tackifying resin, and mixing for 10 minutes; continuously adding the diluent, and mixing for 10 minutes;
and step four, stopping mixing uniformly, discharging and cooling to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
Example 4:
the SBC-based hot melt adhesive modified by an ethylene-acrylic acid ionic polymer in this example 4 is characterized in that the hot melt adhesive is prepared from the following components in parts by mass: styrene- (ethylene-propylene) -styrene copolymer (SEPS): 34 parts of (a); ethylene-methacrylic acid ionomer: 13 parts; 20 parts of tackifying resin; a compatilizer: 3 parts of a mixture; diluent agent: 18 parts of a mixture; and 1 part of antioxidant.
Wherein, the diluent is naphthenic oil; the antioxidant is thiol antioxidant.
The preparation method comprises the following steps:
the method comprises the following steps: adding SEPS, an ethylene-methacrylic acid ionic polymer, an antioxidant, a compatilizer and a diluent into a stirring kettle, and stirring for 30min at the temperature of 120 ℃ to obtain a mixture;
step two: and (3) adding tackifying resin into the mixture obtained in the step one, stirring for 1-2 h at the temperature of 170 ℃, and filtering and removing bubbles to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
Example 5:
the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive in this example 5 is characterized by being prepared from the following components in parts by mass: SBS: 18 parts of a mixture; SIS: 18 parts of a mixture; ethylene-acrylic ionic polymer: 11 parts of (1); tackifying resin: 15 parts of (1); a compatilizer: 4 parts of a mixture; diluent agent: 16 parts of a mixture; and 2 parts of an antioxidant.
Wherein, the diluent is naphthenic oil; the antioxidant is a combined antioxidant.
The preparation method comprises the following steps:
the method comprises the following steps: adding SBC, an ethylene-methacrylic acid ionic polymer, an antioxidant, a compatilizer and a diluent into a stirring kettle, and stirring for 30min at the temperature of 110 ℃ to obtain a mixture;
step two: and (3) adding tackifying resin into the mixture obtained in the step one, stirring for 1-2 h at the temperature of 190 ℃, and filtering and removing bubbles to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
Comparative example:
the SBC-based hot melt adhesive in the comparative example is characterized by being prepared from the following components in parts by mass: styrene-butadiene-styrene copolymer (SBS): 36 parts of (A); tackifying resin: 15 parts of (1); diluent agent: 16 parts of a mixture; 0.5 part of antioxidant.
Wherein, the diluent is naphthenic oil; the antioxidant is antioxidant 1010.
The preparation method comprises the following steps:
the method comprises the following steps: adding SBC, an ethylene-methacrylic acid ionic polymer, an antioxidant, a compatilizer and a diluent into a stirring kettle, and stirring for 30min at the temperature of 120 ℃ to obtain a mixture;
step two: and (3) adding tackifying resin into the mixture obtained in the step one, stirring for 1-2 h at the temperature of 180 ℃, and filtering and removing bubbles to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
The hot melt adhesives prepared in the above examples 1 to 5 and comparative example were subjected to performance tests, and the test results are shown in the following table. Wherein the softening point is tested according to the GB/T15332 standard; the 180-degree peel strength is tested according to the GB/T2790 standard; the heat ageing test was carried out according to the GB/T7141 standard.
Figure BSA0000222806430000051
From the above table, the ethylene-acrylic acid ionic polymer is added into the SBC-based hot melt adhesive formula material, so that the peel strength, the aging resistance and the durability of the hot melt adhesive are effectively improved.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (9)

1. The ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive is characterized by being prepared from the following components in parts by mass: styrene Block Copolymers (SBC): 28-36 parts; ethylene-acrylic ionic polymer: 11-19 parts; tackifying resin: 15-35 parts; diluent agent: 16-24 parts; 0.5-3 parts of antioxidant.
2. The modified SBC based hot melt adhesive of claim 1, wherein said SBC is one or a combination of SIS, SBS, SEBS and SEPS.
3. The modified SBC-based hot melt adhesive according to claim 1, wherein said ethylene-acrylic acid ionic polymer is unsaturated sodium salt or zinc salt of copolymer of ethylene and acrylic acid, methacrylic acid and the like, and combination thereof.
4. The ethylene-acrylic ionic polymer modified SBC-based hot melt adhesive according to claim 1, wherein said tackifying resin is rosin resin, petroleum resin or a combination thereof.
5. The modified SBC-based hot melt adhesive according to claim 1, wherein 1-5 parts of maleic anhydride grafted styrene block copolymer as a compatibilizer is added.
6. The modified SBC based hot melt adhesive according to claim 1, wherein said diluent is naphthenic oil, paraffinic oil or a combination thereof.
7. The ethylene-acrylic acid ionic polymer modified SBC based hot melt adhesive according to claim 1, wherein said antioxidant is amine and phenolic antioxidant, phosphite and thiol antioxidant, or a combination thereof.
8. The modified SBC-based hot melt adhesive of any one of claims 1 to 7, further comprising the following preparation method using a kneader:
step one, setting the temperature of a kneader to be 160 ℃, and starting heating;
step two, after the set temperature is reached, setting the rotating speed of a rotor to be 60rpm, then pouring SBC, the ethylene-acrylic acid ionic polymer and the antioxidant from a feed inlet, and mixing for 20 minutes;
step three, continuously adding the compatilizer and the tackifying resin, and mixing for 10 minutes; continuously adding the diluent, and mixing for 10 minutes;
and step four, stopping mixing uniformly, discharging and cooling to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
9. The modified SBC based hot melt adhesive according to any one of claims 1 to 7, further comprising the following preparation method using a reaction kettle:
the method comprises the following steps: adding SBC, an ethylene-acrylic acid ionic polymer, an antioxidant, a compatilizer and a diluent into a stirring kettle, and stirring for 30-50 min at the temperature of 80-150 ℃ to obtain a mixture;
step two: and (3) adding tackifying resin into the mixture obtained in the step one, stirring for 1-2 h at the temperature of 170-200 ℃, and filtering and removing bubbles to obtain the ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive.
CN202011167668.7A 2020-10-27 2020-10-27 Ethylene-acrylic acid ionic polymer modified SBC-based hot melt adhesive Pending CN112322232A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113292952A (en) * 2021-06-30 2021-08-24 佛山南宝高盛高新材料有限公司 Peelable hot melt adhesive for electric appliance packaging and preparation method thereof
CN113969518A (en) * 2021-03-26 2022-01-25 浙江科技学院 Water-based coating heat-sealing adhesive for medical dialyzing paper and coating method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113969518A (en) * 2021-03-26 2022-01-25 浙江科技学院 Water-based coating heat-sealing adhesive for medical dialyzing paper and coating method thereof
CN113969518B (en) * 2021-03-26 2023-01-13 浙江科技学院 Water-based coating heat-sealing adhesive for medical dialyzing paper and coating method thereof
CN113292952A (en) * 2021-06-30 2021-08-24 佛山南宝高盛高新材料有限公司 Peelable hot melt adhesive for electric appliance packaging and preparation method thereof

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