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CN106497497B - Antiacid peelable glue and its preparation method and application - Google Patents

Antiacid peelable glue and its preparation method and application Download PDF

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Publication number
CN106497497B
CN106497497B CN201610883725.9A CN201610883725A CN106497497B CN 106497497 B CN106497497 B CN 106497497B CN 201610883725 A CN201610883725 A CN 201610883725A CN 106497497 B CN106497497 B CN 106497497B
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Prior art keywords
antiacid
glass
oligomer
peelable
agent
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CN106497497A (en
Inventor
于爱霞
黄仁杰
林毅豪
张云柱
郑长利
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Guangzhou Hui Li Electron Material Co Ltd
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Guangzhou Hui Li Electron Material Co Ltd
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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
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • C09J175/14Polyurethanes having carbon-to-carbon unsaturated bonds
    • 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
    • C09J11/06Non-macromolecular additives organic
    • 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
    • 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

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

Abstract

The present invention relates to a kind of antiacid peelable glues and preparation method thereof, belong to chemical material technical field, which is mainly prepared by the raw material of following weight part ratio: 45~70 parts of oligomer, 25~55 parts of activated monomer, 3~10 parts of photoinitiator, 0.1~10 part of auxiliary agent;Wherein, the oligomer is at least one of urethane acrylate and polybutadiene acrylic acid ester;The activated monomer is at least one of monofunctional acrylates' ester, bifunctional acrylate and multi-functional acrylate.Antiacid peelable glue of the invention has the advantage that wire mark is glued, and simple process can be coated different dimension glass surfaces;And configuration of surface is good, UV light rapid curing, is suitble to batch processing;Bonding force is strong, and CNC back edge will not be tilted or be removed, and is resistant to HF, HCl and H2SO4;Hot-water soak removing, it is at low cost.It can be widely used in the hf resi stant protection of the secondary hardening processing procedure of tempered glass, cover-plate glass, touch-control glass and simple glass.

Description

Antiacid peelable glue and its preparation method and application
Technical field
The present invention relates to chemical material technical fields, more particularly to a kind of antiacid peelable glue and preparation method thereof and answer With.
Background technique
In general, the theoretical strength of glass is up to 10000MPa or more, but the practical application intensity of glass is very low, deficiency reason It by the 1% of intensity, is slightly impacted in actual use, it is possible to crack or defect, so as to cause under strength of glass Drop.To solve the above-mentioned problems, one of the main method that acid processing is strengthened glass, also known as secondary hardening are carried out to glass (the last two), principle are to be chemically reacted with acid solution and glass surface, are handled the micro-crack of glass surface, thus Improve strength of glass.The present common acid of acid treatment process is hydrofluoric acid (HF), hydrofluoric acid and hydrochloric acid (HCl) or sulfuric acid (H2SO4) Mixed acid.During acid processing, the glass contacted with acid can be corroded, thus need for being not required to region to be processed It is protected.
Common way is in the market, after big glass-cutting is at small glass, using CNC (Computer Numerical Control, Numeric Control Technology) sander polishes to glass edge, then glass upper and lower surface be covered with peelable blue gel or Antiacid film is etched (secondary hardening) glass edge after polishing with HF or mixed acid, and lye moves back film or manual demoulding. Peelable blue gel or antiacid film are using the mode directly fitted after curing molding, and fitting is cumbersome, by screen size and type Face is limited, and higher cost, and has membrane removal inconvenient or defect not environmentally.
Summary of the invention
Based on this, it is necessary in view of the above-mentioned problems, providing a kind of antiacid peelable glue, using the peelable glue, wire mark can be passed through UV light rapid curing after sizing, have it is strong to glass bonding force, CNC can be crossed, be resistant to HF or mixed acid, can hot-water soak remove The characteristics of.
A kind of antiacid peelable glue, is mainly prepared by the raw material of following weight part ratio:
The oligomer is at least one of urethane acrylate and polybutadiene acrylic acid ester;
The activated monomer is monofunctional acrylates' ester, bifunctional acrylate and multi-functional acrylate At least one of.
The peelable glue is mainly prepared by the raw material of following parts by weight in one of the embodiments:
Monofunctional acrylates' ester is that isobornyl methacrylate, acrylic acid are different in one of the embodiments, Norbornene ester or 3,3,5- trimethyl-cyclohexane acrylate;
The bifunctional acrylate is Tricyclodecane Dimethanol diacrylate, tripropylene glycol diacrylate Ester or 1,6 hexanediol diacrylate;
The multi-functional acrylate is trimethylolpropane trimethacrylate, two-trimethylolpropane tris acrylic acid Ester or ethoxyquin trimethylolpropane trimethacrylate.
The photoinitiator is at least one of free radical photo-initiation in one of the embodiments,.
The free radical photo-initiation is 2- hydroxy-2-methyl -1- phenyl -1- acetone, 1- in one of the embodiments, Hydroxy-cyciohexyl Benzophenone, 2,4,6- trimethylbenzoy-dipheny phosphine oxides, bis- (2,4,6- trimethylbenzoyls) At least one of phenyl phosphine oxide, 2,4,6- tri-methyl benzophenone and 4- methyl benzophenone.
The auxiliary agent is adhesion promoter, defoaming agent, wetting agent, levelling agent and antioxygen in one of the embodiments, At least one of agent.
In one of the embodiments, the adhesion promoter be γ-glycidyl ether oxygen propyl trimethoxy silicane, Gamma-aminopropyl-triethoxy-silane, γ-methacryloxypropyl trimethoxy silane, γ-methacryloxypropyl At least one of triethoxysilane and N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane;
The defoaming agent is silicone defoaming agent;
The wetting agent is modified dimethyl silicone polymer;
The levelling agent is silicone levelling agent;
The antioxidant is Hinered phenols antioxidant.
This law is bright to also disclose the preparation method of above-mentioned antiacid peelable glue, which comprises the following steps:
Preheating: the oligomer is preheated;
Hot mixing: keeping preheating temperature, the activated monomer be added, and so that the oligomer is dissolved completely in the activity single In body, mixed glue solution is obtained;
Mixing: stop heating, the photoinitiator and auxiliary agent is added, stirred evenly under waste heat to get.
In one of the embodiments, in the preheating step, the oligomer is heated to 45-60 DEG C and is preheated. It is preferred that 50-55 DEG C.
The bright application for also disclosing above-mentioned antiacid peelable glue in the peracid strengthening processing of glass of this law.
Compared with prior art, the invention has the following advantages:
A kind of antiacid peelable glue of the invention, can be substituted for peelable blue gel or antiacid film, handle (the last two) mistake in acid Cheng Zhongke protects glass not corroded by HF.Also, the usage mode of the peelable glue is to be uniformly coated on to need to protect by wire mark Glass surface, UV light rapid curing, by glass CNC polish and steep acid processing after, glue-line is removed using hot-water soak.
Therefore, which has the advantage that wire mark is glued, and simple process can be to different dimension glass surfaces It is coated, is not influenced by glass size and shape;It can quickly be defoamed after wire mark, configuration of surface is good;UV light rapid curing is suitble to Batch processing, efficiently;Strong to glass bonding force, CNC processing procedure back edge will not be tilted or be removed, and be resistant to HF, HCl and H2SO4Deng more Kind acid;Hot-water soak, that is, peelable, it is environmentally protective;It is at low cost, about 1/10th of peelable blue gel.
The antiacid peelable glue can be used for during tempered glass, cover-plate glass, touch-control glass and simple glass secondary hardening Hf resi stant protection, have the advantages that have wide range of applications.
Specific embodiment
It to facilitate the understanding of the present invention, below will be to invention is more fully described.But the present invention can be to be permitted Mostly different form is realized, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes It is more thorough and comprehensive to the understanding of the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool The purpose of the embodiment of body, it is not intended that in the limitation present invention.
The glass that antiacid peelable glue of the present invention is applicable in includes tempered glass, cover-plate glass, touch-control glass and common Glass includes quartz glass and sapphire glass by material point.The color of the antiacid peelable glue is usually colorless and transparent, can be slightly Show milky white.The coating method of the antiacid peelable glue is wire mark.The curing mode of the antiacid peelable glue is UV photocuring.
Embodiment 1
A kind of antiacid peelable glue is colorless and transparent UV photocuring product, by being prepared with raw material:
Oligomer: total 66.11g.
Urethane acrylate 66.11g.
Activated monomer: total 28.44g.
Monofunctional acrylates' ester, isobornyl acrylate (IBOA) 9.48g,
Multi-functional acrylate, trimethylolpropane trimethacrylate 9.48g,
Multi-functional acrylate, ethoxyquin trimethylolpropane trimethacrylate 9.48g.
Photoinitiator: total 3.8g.
2- hydroxy-2-methyl-phenylacetone -1 3.8.
Auxiliary agent: total 1.65g.
Adhesion promoter (γ-methacryloxypropyl) 0.95g,
Defoaming agent (silicone defoaming agent, model 6632) 0.3g,
Levelling agent (silicone levelling agent, model SIVEL 5525) 0.2g,
Antioxidant (hydroquinone) 0.2g.
The antiacid peelable glue of the present embodiment, is prepared by the following method to obtain:
One, it preheats.
The oligomer is preheated.It is specific as follows:
66.11g oligomer urethane acrylate is put into coppers, is heated to 55 DEG C.
Two, hot mixing.
Keeping temperature is 55 DEG C, and activated monomer is added while stirring, oligomer is made to be dissolved completely in activated monomer (simple function Activated monomer isobornyl acrylate (IBOA) 9.48g of group's acrylate, three hydroxyl of activated monomer of multi-functional acrylate Propane tri 9.48g, the activated monomer ethoxyquin trimethylolpropane tris acrylic acid of multi-functional acrylate Ester 9.48g) in, obtain mixed glue solution.
Three, it mixes.
Stop heating, photoinitiator and auxiliary agent (2- hydroxy-2-methyl--1 3.8g of phenylacetone, adhesive force promotion is added Agent (γ-methacryloxypropyl) 0.95g, defoaming agent (SIVEL 6632) 0.3g, levelling agent (SIVEL 5525) 0.2g, antioxidant (hydroquinone) 0.2g), it is stirred until homogeneous in the waste heat high speed of previous step;It vacuumizes, Packing, can be obtained colorless and transparent antiacid peelable glue.
Above-mentioned antiacid peelable glue is tested for the property, as a result as follows:
The viscosity of the antiacid peelable glue is about 8800cps, density 1.072g/cm3;It can quickly be defoamed after wire mark, surface Form is good;Solidification energy is 1000mj/cm2, hardness is about 68D after solidification;Can cross CNC, cross HF (8%HF+8%HCl, 30 DEG C, Without peeling off without tilting after 8min), 80 DEG C of hot-water soak 8min can be completely stripped, and be specifically shown in the following table 1.
Embodiment 2
A kind of antiacid peelable glue is colorless and transparent UV photocuring product, by being prepared with raw material:
Oligomer: total 47.11g.
Polybutadiene acrylic acid ester 47.11g.
Activated monomer: total 47.44g.
Monofunctional acrylates' ester, isobornyl acrylate (IBOA) 18.98g,
Bifunctional acrylate, Tricyclodecane Dimethanol diacrylate 18.98g
Multi-functional acrylate, ethoxyquin trimethylolpropane trimethacrylate 9.48g.
Photoinitiator: total 3.8g.
2- hydroxy-2-methyl-phenylacetone -1 3.8.
Auxiliary agent: total 1.65g.
Adhesion promoter (γ-methacryloxypropyl) 0.95g,
Defoaming agent (silicone defoaming agent, model 6632) 0.3g,
Levelling agent (silicone levelling agent, model SIVEL 5525) 0.2g,
Antioxidant (hydroquinone) 0.2g.
The antiacid peelable glue of the present embodiment, is prepared by the following method to obtain:
One, it preheats.
The oligomer is preheated.It is specific as follows:
47.11g oligomer polybutadiene acrylic acid ester is put into coppers, is heated to 55 DEG C.
Two, hot mixing.
Keeping temperature is 55 DEG C, and activated monomer is added while stirring, oligomer is made to be dissolved completely in activated monomer (simple function Activated monomer isobornyl acrylate (IBOA) 18.98g of group's acrylate, the activated monomer tricyclic of bifunctional acrylate Decane dimethanol diacrylate 18.98g, the activated monomer ethoxyquin trimethylolpropane tris propylene of multi-functional acrylate Acid esters 9.48g) in, obtain mixed glue solution.
Three, it mixes.
Stop heating, photoinitiator and auxiliary agent (2- hydroxy-2-methyl--1 3.8g of phenylacetone, adhesive force promotion is added Agent (γ-methacryloxypropyl) 0.95g, defoaming agent (SIVEL 6632) 0.3g, levelling agent (SIVEL 5525) 0.2g, antioxidant (hydroquinone) 0.2g), it is stirred until homogeneous in the waste heat high speed of previous step;It vacuumizes, Packing, can be obtained colorless and transparent antiacid peelable glue.
Above-mentioned antiacid peelable glue is tested for the property, as a result as follows:
The viscosity of the antiacid peelable glue is about 20550cps, density 0.969g/cm3;It can quickly be defoamed after wire mark, surface Form is good;Solidification energy is 700-1000mj/cm2, hardness is about 40D after solidification;Can cross CNC, cross HF (8%HF+8%HCl, 30 DEG C, 8min) after without peeling off without tilting, 80 DEG C of hot-water soak 10min can be completely stripped, and be specifically shown in the following table 1.
Comparative example 1
A kind of antiacid peelable glue, it is essentially identical with the peelable glue of embodiment 2, and prepared referring to the preparation method of embodiment 2 It obtains, difference is only that:
The activated monomer ethoxyquin trimethylolpropane trimethacrylate of multi-functional acrylate replaces with trihydroxy methyl Propane tri methylol triacrylate.
Comparative example 2
A kind of antiacid peelable glue, it is essentially identical with the peelable glue of embodiment 2, and prepared referring to the preparation method of embodiment 2 It obtains, difference is only that:
γ-methacryloxypropyl and other silane are not added, because adhesive force NG (does not meet and wants Ask), in CNC can monolith peel off, not CNC directly steep it is sour also can monolith fall off.
Comparative example 3
A kind of antiacid peelable glue, it is essentially identical with the peelable glue of embodiment 2, and prepared referring to the preparation method of embodiment 2 It obtains, difference is only that:
Polybutadiene-acrylate replaces with epoxy acrylate or polyester acrylate, and in CNC, edge can collapse It is bad, not CNC directly steep sorrel also can monolith peel off.
Embodiment
It is tested for the property after the peelable glue that above-described embodiment and comparative example are prepared is passed through wire mark, the method is as follows:
Viscosity: 25 DEG C of viscosity, standard " GB/T 22314-2008 plastics epoxy resin viscosity test method ".
Specific gravity: 25 DEG C, standard " GB/T 15223-2008 plastic liquid resin measures density with bottle method ".
Hardness: 23 ± 2 DEG C, " GB/T 2411-2008 plastics and hard rubber use hardometer measurement identation hardness (Shao to standard Family name's hardness) ".
CNC: being polished using spark bistrique, revolving speed 1000r/min, is rinsed after mill with high-velocity flow, the glue of glass edge It is OK that water, which will not remove (corrugation tilts),.
Bubble acid: impregnating 8min in 30 DEG C of 8%HF+8%HCl mixed acid solution, is rinsed with water back edge without wrinkling, stick up It rises or falls off as OK.
Hot water removing: splitting time, which refers to, to be impregnated in 80 DEG C of hot water and (can be aided with ultrasonic oscillation and accelerate removing), glue It can monolith or time for all removing.
Test result is as follows:
1. the performance test results of table
As can be seen that the antiacid peelable glue of 1-2 of the embodiment of the present invention, UV light after being glued by wire mark in from the above Rapid curing, have it is strong to glass bonding force, CNC can be crossed, be resistant to HF or mixed acid, can hot-water soak removing the characteristics of, energy Enough it is suitable for Hyaluronic Acid and handles secondary hardening process.And the peelable glue of comparative example 1-3, effect are poor.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.

Claims (6)

1. a kind of antiacid peelable glue, which is characterized in that during the peracid strengthening for glass is handled, by the raw material system of following weight part ratio It is standby to form:
The oligomer is selected from: urethane acrylate;The activated monomer are as follows: isobornyl acrylate, trimethylolpropane Triacrylate and ethoxyquin trimethylolpropane trimethacrylate;The photoinitiator is selected from: 2- hydroxy-2-methyl -1- benzene Base -1- acetone;The auxiliary agent are as follows: γ-methacryloxypropyl, defoaming agent, levelling agent and antioxidant;
Or
The oligomer is selected from: polybutadiene acrylic acid ester;The activated monomer are as follows: isobornyl acrylate, tristane two Methanol diacrylate and ethoxyquin trimethylolpropane trimethacrylate;The photoinitiator is selected from: 2- hydroxy-2-methyl- 1- phenyl -1- acetone;The auxiliary agent are as follows: γ-methacryloxypropyl, defoaming agent, levelling agent and anti- Oxygen agent.
2. antiacid peelable glue according to claim 1, which is characterized in that mainly by following parts by weight raw material preparation and At:
3. antiacid peelable glue according to claim 1, which is characterized in that the defoaming agent is silicone defoaming agent;
The levelling agent is silicone levelling agent;
The antioxidant is Hinered phenols antioxidant.
4. the preparation method of the described in any item antiacid peelable glues of claim 1-3, which comprises the following steps:
Preheating: the oligomer is preheated;
Hot mixing: preheating temperature is kept, the activated monomer is added, the oligomer is made to be dissolved completely in the activated monomer In, obtain mixed glue solution;
Mixing: stop heating, the photoinitiator and auxiliary agent is added, stirred evenly under waste heat to get.
5. the preparation method of antiacid peelable glue according to claim 4, which is characterized in that in the preheating step, by institute It states oligomer and is heated to 45-60 DEG C and preheated.
6. application of the described in any item antiacid peelable glues of claim 1-3 in the peracid strengthening processing of glass.
CN201610883725.9A 2016-10-09 2016-10-09 Antiacid peelable glue and its preparation method and application Active CN106497497B (en)

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