CN110607133A - Thick-adhesive-layer ultra-low-viscosity protective film glue and preparation method thereof - Google Patents

Thick-adhesive-layer ultra-low-viscosity protective film glue and preparation method thereof Download PDF

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Publication number
CN110607133A
CN110607133A CN201910386775.XA CN201910386775A CN110607133A CN 110607133 A CN110607133 A CN 110607133A CN 201910386775 A CN201910386775 A CN 201910386775A CN 110607133 A CN110607133 A CN 110607133A
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China
Prior art keywords
parts
glue
mixing
protective film
acrylate polymer
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Application number
CN201910386775.XA
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Chinese (zh)
Inventor
姜欣
黄新波
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Nantong Kangerle Composite Material Co Ltd
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Nantong Kangerle Composite Material Co Ltd
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Priority to CN201910386775.XA priority Critical patent/CN110607133A/en
Publication of CN110607133A publication Critical patent/CN110607133A/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
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • 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
    • C09J4/00Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C09J4/06Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
    • 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
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • 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
    • C09J2433/00Presence of (meth)acrylic polymer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a thick-adhesive-layer ultra-low-viscosity protective film glue and a preparation method thereof, wherein the protective film glue comprises 30-60 parts by weight of isooctyl acrylate polymer, 20-40 parts by weight of butyl acrylate polymer, 5-10 parts by weight of isobornyl methacrylate, pet 3-5 parts by weight of photoinitiator, 1840.1-2 parts by weight of silica sol and 1-3 parts by weight of curing agent.

Description

Thick-adhesive-layer ultra-low-viscosity protective film glue and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of protective film glue, in particular to thick-glue-layer ultra-low-viscosity protective film glue and a preparation method thereof.
Background
The glue is an intermediate for connecting two materials, mostly appears as a water aqua, belongs to the fine chemical industry, is various in types, and is mainly classified by a bonding material, a physical form, a hardening method and a material of an adherend. At present, no product which can be made by a protective film glue layer and is not peeled off constantly by 0.1 to 0.2mm is available in domestic markets.
Disclosure of Invention
The invention aims to provide glue for a thick-glue-layer ultra-low-viscosity protective film and a preparation method thereof, and aims to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: the protective film glue with the thick glue layer and the ultra-low viscosity comprises, by weight, 30-60 parts of isooctyl acrylate polymer, 20-40 parts of butyl acrylate polymer, 5-10 parts of isobornyl methacrylate, 5-5 parts of petat3, 1840.1-2 parts of photoinitiator, 4-12 parts of silica sol and 1-3 parts of curing agent.
Preferably, the preferable component proportion of the protective film glue component comprises 45 parts of isooctyl acrylate polymer, 30 parts of butyl acrylate polymer, 8 parts of isobornyl methacrylate, pet 4 parts, 1841 part of photoinitiator, 8 parts of silica sol and 2 parts of curing agent.
Preferably, the silica sol adopts a siloxane coupling agent modified nano-silica dispersion liquid.
Preferably, the curing agent consists of 30% of triethanolamine, 20% of tamarix chinensis bark powder, 25% of lignin and 25% of isophorone diamine.
Preferably, the preparation method comprises the following steps:
A. mixing isooctyl acrylate polymer, butyl acrylate polymer, isobornyl methacrylate, pet and photoinitiator 184, adding into a stirring tank, and mixing and stirring at high and low speeds to obtain a mixture A;
B. sequentially adding silica sol, a curing agent and a mixing agent A into a mixing roll, fully mixing and then mixing, wherein the mixing temperature is 180 ℃ and 220 ℃, and the mixing time is 30-50 min to obtain a mixing agent B;
C. adding the mixture B into a reaction kettle for heating reaction at the temperature of 80-95 ℃ for 4-6 h, preserving the temperature for 20min, and cooling to room temperature to obtain the protective film glue.
Preferably, in the step A, low-speed stirring is adopted, the stirring speed is 100-.
Compared with the prior art, the invention has the beneficial effects that: the preparation method is simple, the prepared protective film glue has high curing speed, good stability, good function of filling up segment difference and good weather resistance, the peeling force of the protective film glue can not change along with the increase of the thickness of the glue layer, and the peeling force value of the glue layer from 0.01mm to 0.2mm is always kept about 1g/in +/-10%; in addition, the added silica sol provides a microporous structure for the glue, and the density of the glue is reduced, so that the aim of reducing the dielectric constant is fulfilled, and the yellowing resistance and the aging resistance of the glue are further improved; in addition, the curing agent added in the invention can enhance the curing strength of the glue and shorten the curing time.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The invention provides the following technical scheme: the protective film glue with the thick glue layer and the ultra-low viscosity comprises, by weight, 30-60 parts of isooctyl acrylate polymer, 20-40 parts of butyl acrylate polymer, 5-10 parts of isobornyl methacrylate, 5-5 parts of petat3, 1840.1-2 parts of photoinitiator, 4-12 parts of silica sol and 1-3 parts of curing agent; wherein, the silica sol adopts siloxane coupling agent modified nano-silica dispersion liquid; the curing agent consists of 30% of triethanolamine, 20% of tamarix chinensis bark powder, 25% of lignin and 25% of isophorone diamine.
The first embodiment is as follows:
the protective film glue comprises, by weight, 30 parts of isooctyl acrylate polymer, 20 parts of butyl acrylate polymer, 5 parts of isobornyl methacrylate, 3 parts of petat, 1840.1 parts of photoinitiator, 4 parts of silica sol and 1 part of curing agent.
The preparation method of this example includes the following steps:
A. mixing isooctyl acrylate polymer, butyl acrylate polymer, isobornyl methacrylate, pet and photoinitiator 184, adding into a stirring tank, and mixing and stirring at high and low speeds to obtain a mixture A;
B. sequentially adding silica sol, a curing agent and a mixing agent A into a mixing roll, fully mixing, and then mixing for 30min at the mixing temperature of 180 ℃ to obtain a mixing agent B;
C. and adding the mixture B into a reaction kettle for heating reaction at the temperature of 80 ℃ for 4 hours, preserving the temperature for 20min, and cooling to room temperature to obtain the protective film glue.
In this embodiment, in the step a, low-speed stirring is first adopted, the stirring speed is 100 rpm, and high-speed stirring is carried out after 10min of stirring, the stirring speed is 3000 rpm, and the stirring time is 20 min.
Example two:
the protective film glue comprises 60 parts of isooctyl acrylate polymer, 40 parts of butyl acrylate polymer, 10 parts of isobornyl methacrylate, 5 parts of pet, 1842 parts of photoinitiator, 12 parts of silica sol and 3 parts of curing agent.
The preparation method of this example includes the following steps:
A. mixing isooctyl acrylate polymer, butyl acrylate polymer, isobornyl methacrylate, pet and photoinitiator 184, adding into a stirring tank, and mixing and stirring at high and low speeds to obtain a mixture A;
B. sequentially adding silica sol, a curing agent and a mixing agent A into a mixing roll, fully mixing, and then mixing at 220 ℃ for 50min to obtain a mixing agent B;
C. and adding the mixture B into a reaction kettle for heating reaction at the temperature of 95 ℃ for 6 hours, preserving the temperature for 20min, and cooling to room temperature to obtain the protective film glue.
In this embodiment, in the step a, low-speed stirring is firstly adopted, the stirring speed is 300 rpm, and high-speed stirring is carried out after 10min of stirring, the stirring speed is 4000 rpm, and the stirring time is 40 min.
Example three:
the protective film glue comprises 35 parts of isooctyl acrylate polymer, 25 parts of butyl acrylate polymer, 6 parts of isobornyl methacrylate, 4 parts of petat, 1841.1 parts of photoinitiator, 6 parts of silica sol and 2 parts of curing agent in parts by weight.
The preparation method of this example includes the following steps:
A. mixing isooctyl acrylate polymer, butyl acrylate polymer, isobornyl methacrylate, pet and photoinitiator 184, adding into a stirring tank, and mixing and stirring at high and low speeds to obtain a mixture A;
B. sequentially adding silica sol, a curing agent and a mixing agent A into a mixing roll, fully mixing, and then mixing at 185 ℃ for 35min to obtain a mixing agent B;
C. and adding the mixture B into a reaction kettle for heating reaction at 82 ℃ for 4 hours, preserving the temperature for 20min, and cooling to room temperature to obtain the protective film glue.
In this embodiment, in the step a, low-speed stirring is firstly adopted, the stirring speed is 150 rpm, and high-speed stirring is carried out after 10min of stirring, the stirring speed is 3200 rpm, and the stirring time is 25 min.
Example four:
the protective film glue comprises 55 parts of isooctyl acrylate polymer, 35 parts of butyl acrylate polymer, 9 parts of isobornyl methacrylate, 5 parts of petat, 1841.6 parts of photoinitiator, 10 parts of silica sol and 2 parts of curing agent in parts by weight.
The preparation method of this example includes the following steps:
A. mixing isooctyl acrylate polymer, butyl acrylate polymer, isobornyl methacrylate, pet and photoinitiator 184, adding into a stirring tank, and mixing and stirring at high and low speeds to obtain a mixture A;
B. sequentially adding silica sol, a curing agent and a mixing agent A into a mixing roll, fully mixing, and then mixing, wherein the mixing temperature is 210 ℃, and the mixing time is 45min, so as to obtain a mixing agent B;
C. and adding the mixture B into a reaction kettle for heating reaction at 92 ℃ for 6 hours, preserving the temperature for 20min, and cooling to room temperature to obtain the protective film glue.
In this embodiment, in the step a, low-speed stirring is performed at a stirring speed of 280 rpm, and high-speed stirring is performed after 10min, wherein the stirring speed is 3800 rpm and the stirring time is 35 min.
Example five:
the protective film glue comprises 50 parts of isooctyl acrylate polymer, 32 parts of butyl acrylate polymer, 7 parts of isobornyl methacrylate, 4 parts of petat, 1840.9 parts of photoinitiator, 9 parts of silica sol and 2 parts of curing agent in parts by weight.
The preparation method of this example includes the following steps:
A. mixing isooctyl acrylate polymer, butyl acrylate polymer, isobornyl methacrylate, pet and photoinitiator 184, adding into a stirring tank, and mixing and stirring at high and low speeds to obtain a mixture A;
B. sequentially adding silica sol, a curing agent and a mixing agent A into a mixing roll, fully mixing, and then mixing at 195 ℃ for 42min to obtain a mixing agent B;
C. and adding the mixture B into a reaction kettle for heating reaction at 88 ℃ for 6 hours, preserving the temperature for 20min, and cooling to room temperature to obtain the protective film glue.
In this embodiment, in step a, low-speed stirring is performed at a stirring speed of 180 rpm, and high-speed stirring is performed after 10min, wherein the stirring speed is 3600 rpm and the stirring time is 28 min.
Example six:
the protective film glue comprises 45 parts of isooctyl acrylate polymer, 30 parts of butyl acrylate polymer, 8 parts of isobornyl methacrylate, 4 parts of pet, 1841 parts of photoinitiator, 8 parts of silica sol and 2 parts of curing agent.
The preparation method of this example includes the following steps:
A. mixing isooctyl acrylate polymer, butyl acrylate polymer, isobornyl methacrylate, pet and photoinitiator 184, adding into a stirring tank, and mixing and stirring at high and low speeds to obtain a mixture A;
B. sequentially adding silica sol, a curing agent and a mixing agent A into a mixing roll, fully mixing, and then mixing at the mixing temperature of 200 ℃ for 40min to obtain a mixing agent B;
C. and adding the mixture B into a reaction kettle for heating reaction at the temperature of 90 ℃ for 5 hours, preserving the temperature for 20min, and cooling to room temperature to obtain the protective film glue.
In this embodiment, in step a, low-speed stirring is first performed, the stirring speed is 200 rpm, and high-speed stirring is performed after 10min, the stirring speed is 3500 rpm, and the stirring time is 30 min.
Experimental example:
the glue prepared by the embodiments of the invention is used for performance test, and the obtained data is as follows:
peel force (g/in)
Example one 0.9
Example two 0.9
EXAMPLE III 1.1
Example four 1.2
EXAMPLE five 1.1
EXAMPLE six 1.0
In conclusion, the preparation method is simple, the prepared protective film glue is high in curing speed, good in stability, good in function of filling up segment differences and good in weather resistance, the peeling force of the protective film glue cannot change along with the increase of the thickness of the glue layer, and the peeling force value of the glue layer from 0.01mm to 0.2mm is always kept at about 1g/in +/-10%; in addition, the added silica sol provides a microporous structure for the glue, and the density of the glue is reduced, so that the aim of reducing the dielectric constant is fulfilled, and the yellowing resistance and the aging resistance of the glue are further improved; in addition, the curing agent added in the invention can enhance the curing strength of the glue and shorten the curing time.
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 (6)

1. The glue for the thick-glue-layer ultra-low-viscosity protective film is characterized in that: the protective film glue comprises, by weight, 30-60 parts of isooctyl acrylate polymer, 20-40 parts of butyl acrylate polymer, 5-10 parts of isobornyl methacrylate, 5-5 parts of pet 3, 1840.1-2 parts of photoinitiator, 4-12 parts of silica sol and 1-3 parts of curing agent.
2. The glue with thick glue layer and ultra-low viscosity protective film as claimed in claim 1, wherein: the preferable component proportion of the protective film glue comprises 45 parts of isooctyl acrylate polymer, 30 parts of butyl acrylate polymer, 8 parts of isobornyl methacrylate, pet 4 parts, 1841 parts of photoinitiator, 8 parts of silica sol and 2 parts of curing agent.
3. The glue with thick glue layer and ultra-low viscosity protective film as claimed in claim 1, wherein: the silica sol adopts a siloxane coupling agent modified nano-silica dispersion liquid.
4. The glue with thick glue layer and ultra-low viscosity protective film as claimed in claim 1, wherein: the curing agent consists of 30% of triethanolamine, 20% of tamarix chinensis bark powder, 25% of lignin and 25% of isophorone diamine.
5. The preparation method of the thick-glue-layer ultralow-viscosity protective film glue disclosed by the claim 1 is realized, and is characterized in that: the preparation method comprises the following steps:
A. mixing isooctyl acrylate polymer, butyl acrylate polymer, isobornyl methacrylate, pet and photoinitiator 184, adding into a stirring tank, and mixing and stirring at high and low speeds to obtain a mixture A;
B. sequentially adding silica sol, a curing agent and a mixing agent A into a mixing roll, fully mixing and then mixing, wherein the mixing temperature is 180 ℃ and 220 ℃, and the mixing time is 30-50 min to obtain a mixing agent B;
C. adding the mixture B into a reaction kettle for heating reaction at the temperature of 80-95 ℃ for 4-6 h, preserving the temperature for 20min, and cooling to room temperature to obtain the protective film glue.
6. The preparation method of the thick-glue-layer ultralow-viscosity protective film glue according to claim 5, characterized in that: in the step A, low-speed stirring is adopted firstly, the stirring speed is 100-.
CN201910386775.XA 2019-05-10 2019-05-10 Thick-adhesive-layer ultra-low-viscosity protective film glue and preparation method thereof Pending CN110607133A (en)

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Application Number Priority Date Filing Date Title
CN201910386775.XA CN110607133A (en) 2019-05-10 2019-05-10 Thick-adhesive-layer ultra-low-viscosity protective film glue and preparation method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112322207A (en) * 2020-11-04 2021-02-05 湖南弘擎电子材料科技有限公司 UV curing double-sided adhesive tape applied to pasting low-surface-energy material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112322207A (en) * 2020-11-04 2021-02-05 湖南弘擎电子材料科技有限公司 UV curing double-sided adhesive tape applied to pasting low-surface-energy material and preparation method thereof

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Application publication date: 20191224