CN110343483A - A kind of rapid curing silicone pressure sensitive gluing agent and adhesive tape - Google Patents
A kind of rapid curing silicone pressure sensitive gluing agent and adhesive tape Download PDFInfo
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- CN110343483A CN110343483A CN201910629412.4A CN201910629412A CN110343483A CN 110343483 A CN110343483 A CN 110343483A CN 201910629412 A CN201910629412 A CN 201910629412A CN 110343483 A CN110343483 A CN 110343483A
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
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- 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
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- 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
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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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
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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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
- C09J2483/00—Presence of polysiloxane
Abstract
The invention discloses a kind of rapid curing silicone pressure sensitive gluing agent, belong to adhesive field, the sub- quick adhesive of the organosilicon is by the way that by the polysiloxanes methyl vinyl MQ organic silicon rigidity-increasing stick containing vinyl, addition reaction is obtained under the effect of crosslinking agent, reaction suppressor and platinum catalyst, pass through the selection to monomer, the especially selection of function monomer functional group and ratio;To the Optimal improvements of technique;Selection to catalyst and function monomer functional group arranging effect.Glue use directly winds quick-setting target after can reach substrate coating gluing, and also ensures good viscous force and peeling force.
Description
Technical field
The present invention relates to a kind of adhesive more particularly to a kind of rapid curing silicone pressure sensitive gluing agent and adhesive tapes.
Background technique
Organic pressure-sensitive gel is the kind of a kind of top grade of fine quality in pressure sensitive adhesive.When encountering severe condition, such as harsh temperature
Degree, contact chemicals, moisture, radiation, when high temperature resistant, long service life etc. being needed to require, organic pressure-sensitive gel has and can not replace
The advantage in generation, has a vast market application prospect.
Organic pressure-sensitive gel is usually by organic silicon rubber, organic siliconresin, crosslinking agent and the groups such as other additives and solvent
At.Wherein main glue ingredient is two parts of polymer elastomer (organic silicon rubber) and tackifying resin (MQ resin).
There are many affecting parameters for influencing organic pressure-sensitive gel adhesive property.Wherein most direct affecting parameters are to increase in formula
The dosage of viscous MQ resin.Generally, pass through the ratio of reduction MQ resin, thus it is possible to vary the main performance of organic pressure-sensitive gel refers to
Mark, such as peeling force, initial bonding strength, holding power.
But conventional glue curing rate is partially slow, and upper machine coating machine speed is not high, leads to that production capacity is low, product coating cost is higher.
Summary of the invention
The purpose of the present invention is to provide a kind of rapid curing silicone pressure sensitive gluing agent, special by the selection to monomer
It is not the selection of function monomer functional group;To the Optimal improvements of technique;To catalyst and function monomer functional group arranging effect
Selection.Glue use directly winds quick-setting target after can reach substrate coating gluing.
To achieve the goals above, The technical solution adopted by the invention is as follows:
In a first aspect, the present invention discloses a kind of rapid curing silicone pressure sensitive gluing agent, the adhesive is by following raw material
Addition reaction obtains in a kettle:
The polysiloxanes containing vinyl of 20-30 parts by weight;
The methyl vinyl MQ organic silicon rigidity-increasing stick of 0-35 parts by weight;
1.0-1.2 the crosslinking agent of parts by weight;
The platinum catalyst of 0.6-0.7 parts by weight;
The reaction suppressor of 0.1-0.2 parts by weight;
And the solvent of 100-200 parts by weight;
So that the solid content of obtained silicone pressure sensitive gluing agent is 10%-25%;And under 160 DEG C of solidification temperature,
10S-60S, which can be realized, to be fully cured;Quick-setting target is directly wound after can reach substrate coating gluing.
Preferably, a kind of rapid curing silicone pressure sensitive gluing agent of the present invention, the weight average molecular weight of polysiloxanes
For 450000-650000;Vinyl is end group and mass percent is 0.07%-0.08%;Fugitive constituent≤1.30%;
The general structure of the polysiloxanes are as follows:
R(CH3)2SiO[Si(CH3)2O]n[Si(CH3) (CH=CH2)O]mSi(CH3)2R, wherein R is vinyl.
Preferably, a kind of rapid curing silicone pressure sensitive gluing agent of the present invention, the structure of MQ organic silicon rigidity-increasing stick
Formula are as follows: [(CH3)2(CH2=CH) SiO1/2]a[(CH3)3SiO1/2]b[SiO4/2]c,
Wherein [(CH3)2(CH2=CH) SiO1/2]a[(CH3)3SiO1/2]bFor M unit, [SiO4/2]cFor Q unit;M unit with
The ratio of Q unit is that the value of (a+b)/c is 0.7-0.8;Contents of ethylene 0.15%-0.2%;Bulk density is 0.2-0.3g/
cm3;Average particle size is 90-110 μm;After the MQ organic silicon rigidity-increasing stick is mixed with toluene solution by 1:1, viscosity 2-
20mm2/s。
Preferably, a kind of rapid curing silicone pressure sensitive gluing agent of the present invention, crosslinking agent are to contain silicon hydrogen (SiH)
The silicone oil of group, molecular structure are as follows:
(CH3)3SiO[(CH3)2SiO]m[(CH3)(H)SiO]nSi(CH3)3;
Wherein the mass percent of H is 1.0%-1.2%;25 DEG C of viscosity is 30-100mpas;Fugitive constituent < 1%.
Preferably, a kind of rapid curing silicone pressure sensitive gluing agent of the present invention, platinum content is in platinum catalyst
2000ppm-3000ppm;The platinum catalyst is the platinum catalyst being coordinated with methyl vinyl silicone, and at 80 DEG C or more
It can effective catalytic addition reaction.
Preferably, a kind of rapid curing silicone pressure sensitive gluing agent of the present invention, platinum catalyst are using containing length
To karr, this special catalyst carries out ligand exchange to the siloxane oligomer of alkyl group and vinyl, is made into platinum-a, (n- is pungent by w- bis-
Base) Polymethyl methacrylate complex catalyst;The catalytic activity of platinum-vinyl siloxane complex can be improved.
Preferably, a kind of rapid curing silicone pressure sensitive gluing agent of the present invention, solvent are toluene, dimethylbenzene, second
One of acetoacetic ester or a variety of mixing.
Preferably, a kind of rapid curing silicone pressure sensitive gluing agent of the present invention, reaction suppressor are that alkynol class is urged
Change reaction suppressor.
Second aspect, the present invention disclose a kind of preparation method of rapid curing silicone pressure sensitive gluing agent, be used to prepare as
The agent of silicone pressure sensitive gluing, mainly comprises the steps that described in first aspect
1) solvent and polysiloxanes containing vinyl are added in reaction kettle, it is small in 40-50 DEG C of at a temperature of stirring 3
When, obtain the Silicone Rubber Dispersion A that solid content is 24.5%-25.5%;
2) solvent is taken again, is stirred and is mixed for 1:1 by mass parts ratio with the Silicone Rubber Dispersion A in step 1);
3) in whipping process, methyl vinyl MQ organic silicon rigidity-increasing stick, crosslinking agent, reaction suppressor is sequentially added and is urged
Agent, and be sufficiently mixed and uniformly obtain the silicone pressure sensitive gluing agent.
The third aspect, invention additionally discloses a kind of adhesive tapes, include at least: substrate layer and adhesive layer;The adhesive layer
One or both sides coated on the substrate layer;Adhesive layer preparation method as disclosed in second aspect is prepared organic
The agent of silicon pressure-sensitive adhesive is obtained in 160 DEG C of solidification 10S-60S.
Preferably, a kind of adhesive tape of the present invention, the substrate layer are PET base material.
Compared with prior art, the invention has the following beneficial effects:
1, cross-linked speed is fast, and production completion is i.e. cured complete, and peeling force is more stable
2, adhesion strength range is wide, can meet the product of different viscosity
3, this goal in research synthesizes rapid curing glue, by the selection to monomer, especially function monomer functional group and
The selection of ratio;To the Optimal improvements of technique;Selection to catalyst and function monomer functional group arranging effect.Glue use can
Quick-setting target is directly wound after reaching substrate coating gluing.
4, this programme particularity is the arranging effect of function monomer specific functional groups and organic catalyst characteristic, Ji Yaobao
Quick-setting ability is demonstrate,proved, and cannot solidify too fast and can not produce, also meeting productibility, (glue normal temperature storage is stablized
Property), meet matter of time existing for production process and production equipment condition.
5, glue synthetic operation process is simple, facilitates production and application.And solidification rate is fast, production cost is low.
Laboratory simulation coating can reach: 160 DEG C/20S is to steel sheet peeling off power and 160 DEG C/1min to steel sheet peeling off power base
This is identical, reaches final removing force parameter.
Specific embodiment
With reference to embodiment, the embodiment of the present invention is furthur described in detail.Following embodiment is used for
Illustrate the present invention, but is not intended to limit the scope of the invention.
The present invention discloses a kind of rapid curing silicone pressure sensitive gluing agent, passes through the selection to monomer, especially function
The selection of monomer, at the same to catalyst, crosslinking agent it is reasonably combined, can be realized coating after quick-setting purpose,
It improves production efficiency, increase production capacity.
Existing adhesive is usually made of main glue ingredient, crosslinking agent and other additives and solvent, and main glue ingredient mainly wraps
Polymer elastomer and tackifying resin two large divisions are included, conventional, the usage ratio of tackifier is higher to will lead to peeling force, bonding
The increase of power.But the present invention the experimental results showed that, to organic pressure-sensitive gel of the present invention, when tackifier are more than setting range
Afterwards, to the Efficient Adhesive Promotion of glue entirety without significant change.In the following, illustrating beneficial effects of the present invention in conjunction with documents.
Documents 1:CN107057633A discloses a kind of preparation method of quick cured silicone adhesive of two-component,
In this scheme, by by the organic silicon rubber of set amount, modified carbon nano-tube, dimethyl silicone polymer, ethyl orthosilicate and different
Propyl alcohol is stirred to obtain component A;Silane coupling agent, dibutyl tin dilaurate and ethyl acetate etc. are mixed by part simultaneously
Component B;Two-component constitutes rapid curing organosilicon adhesive.Two-component complicated component, the solidified body of one side the technical program
System is complicated, poor controllability;Another aspect preparation method is cumbersome, and higher cost, pressure sensitive adhesive synthesis cycle are longer.
Documents 2:CN108531126B, a kind of organic pressure-sensitive gel containing boron modification MQ organic silicon rigidity-increasing stick, this
In scheme, by selecting the polysiloxanes containing vinyl and organosilicon MQ resin composition mixture, and it is a certain amount of to arrange in pairs or groups
Boron modification MQ organic silicon rigidity-increasing stick shows excellent peeling force after crosslinking curing under platinum catalyst heat effect, just glues
Power and holding power.But this programme needs special boron modification raw material, synthetic operation is more complicated;In addition, in documents 2
The percentage composition of organosilicon MQ resin is higher, and without obvious Efficient Adhesive Promotion for the application, the organosilicon MQ of the application is viscosified
Resin percentage composition is low, and guarantees excellent peeling force, initial bonding strength and holding power, and can also be achieved quick-setting effect
Fruit.
The present invention discloses a kind of rapid curing silicone pressure sensitive gluing agent, wherein adhesive by following raw material in a kettle
Addition reaction obtains:
The polysiloxanes containing vinyl of 20-30 parts by weight;
The methyl vinyl MQ organic silicon rigidity-increasing stick of 0-35 parts by weight;
1.0-1.2 the crosslinking agent of parts by weight;
The platinum catalyst of 0.6-0.7 parts by weight;
The reaction suppressor of 0.1-0.2 parts by weight;
And the solvent of 100-200 parts by weight;
The solid content of the adhesive obtained simultaneously is 10%-25%;And under 160 DEG C of solidification temperature, 10S-60S
It can be realized and be fully cured.
As the above-mentioned polysiloxanes containing vinyl, weight average molecular weight 450000-650000, preferably
500000-600000;More preferably 550000-600000;
Vinyl is end group and mass percent is 0.07%-0.08%, preferably 0.075%-0.08%, more preferably
0.075%-0.078%.
Fugitive constituent≤1.30%, preferably≤1.00%, more preferably≤0.50%;
The general structure of polysiloxanes are as follows:
RbMe3-bSiO(SiMe2O)n(SiMe2-aViaO)mSiMe3-bRb, wherein R is vinyl;M, n is positive integer, and full
Foot makes polysiloxanes weight average molecular weight 450000-650000;A is the integer of 0-2, and b is the integer of 1-3.
The polysiloxanes that vinyl is located at end group is more advantageous to raising catalytic rate.
The specific example of polysiloxanes containing vinyl is following several, but is not limited to:
ViMe2SiO(SiMe2O)n(SiMeViO)mSiMe2Vi;
ViMe2SiO(SiMe2O)n(SiVi2O)mSiMe2Vi;
ViMe2SiO(SiMe2O)n(SiMeViO)0.9m(SiVi2O)0.1mSiMe2Vi;
ViMe2SiO(SiMe2O)n(SiMeViO)0.1m(SiVi2O)0.9mSiMe2Vi;
ViMe2SiO(SiMe2O)n(SiMeViO)0.5m(SiVi2O)0.5mSiMe2Vi;
Vi2MeSiO(SiMe2O)n(SiMeViO)mSiMeVi2;
Vi2MeSiO(SiMe2O)n(SiMeViO)0.5m(SiVi2O)0.5mSi MeVi2;
Vi2MeSiO(SiMe2O)n(SiVi2O)mSiMeVi2Deng
As above-mentioned methyl vinyl MQ organic silicon rigidity-increasing stick, general structure are as follows:
(MemVi3-mSiO1/2)a(Me3SiO1/2)b(SiO4/2)c,
Wherein (MemVi3-mSiO1/2)a(Me3SiO1/2)bFor M unit, (SiO4/2)cFor Q unit;M is the integer of 1-3.M is mono-
The ratio of member and Q unit is that the value of (a+b)/c is 0.7-0.8;Preferably 0.75-0.8, more preferably 0.78-0.8.
Contents of ethylene 0.15%-0.2%;Preferably 0.15%-0.18%, more preferably 0.15%-0.16%.
Bulk density is 0.2-0.3g/cm3;Preferably 0.2-0.28g/cm3, more preferably 0.2-0.25g/cm.
Average particle size is 90-110 μm;Preferably 90-100 μm, more preferably 95-100 μm.
The specific example of methyl vinyl MQ organic silicon rigidity-increasing stick is following several, but is not limited to:
(MeVi2SiO1/2)a(Me3SiO1/2)b(SiO4/2)c;
(MeVi2SiO1/2)0.9a(Me2ViSiO1/2)0.1a(Me3SiO1/2)b(SiO4/2)c;
(MeVi2SiO1/2)0.1a(Me2ViSiO1/2)0.9a(Me3SiO1/2)b(SiO4/2)c;
(MeVi2SiO1/2)0.05a(Me2ViSiO1/2)0.95a(Me3SiO1/2)b(SiO4/2)c;
(MeVi2SiO1/2)0.95a(Me2ViSiO1/2)0.05a(Me3SiO1/2)b(SiO4/2)c;
(MeVi2SiO1/2)0.5a(Me2ViSiO1/2)0.5a(Me3SiO1/2)b(SiO4/2)c;
(MeVi2SiO1/2)0.3a(Me2ViSiO1/2)0.7a(Me3SiO1/2)b(SiO4/2)c;
(Me2ViSiO1/2)a(Me3SiO1/2)b(SiO4/2)cDeng.
The selection of 0-30 parts of MQ organic silicon rigidity-increasing stick such as promotes peeling force more than 30 parts unobvious.
It is the silicone oil containing silicon hydrogen (SiH) group, molecular structure as above-mentioned crosslinking agent are as follows:
Me3SiO(Me2SiO)m(Me2-aHaSiO)nSiMe3;A is the integer of 1-2
Wherein the mass percent of hydrogen (H) is 1.0%-1.2%;Preferably 1.0%-1.1%, more preferably 1.05%-
1.1%;
25 DEG C of viscosity is 30-100mpas;Preferably 30-80mpas, more preferably 50-80mpas;
Fugitive constituent < 1%, preferably < 0.8%, more preferably < 0.5%.
The specific example of silicone oil crosslinking agent containing silicon hydrogen (SiH) group is following several, but is not limited to:
Me3SiO(Me2SiO)m(MeHSiO)nSiMe3;
Me3SiO(Me2SiO)m(MeHSiO)0.1n(H2SiO)0.9n SiMe3;
Me3SiO(Me2SiO)m(MeHSiO)0.9n(H2SiO)0.1n SiMe3;
Me3SiO(Me2SiO)m(MeHSiO)0.45n(H2SiO)0.55n SiMe3;
Me3SiO(Me2SiO)m(MeHSiO)0.5n(H2SiO)0.5n SiMe3;
Me3SiO (Me2SiO) m (H2SiO) n SiMe etc..
As above-mentioned platinum catalyst, wherein platinum content is 2000ppm-3000ppm;Platinum catalyst is and ethylene methacrylic
The platinum catalyst of radical siloxane coordination, and can effective catalytic addition reaction at 80 DEG C or more.
The catalytic activity that ligand exchange is carried out to catalyst, improves platinum-vinyl siloxane complex;Using containing long alkane
To karr, this special catalyst carries out ligand exchange to the siloxane oligomer of base and vinyl, is made into platinum-a, w- bis- (n- octyl) is poly-
The catalyst of methyl vinyl silicone complex.
One of toluene, dimethylbenzene, ethyl acetate or a variety of mixing are chosen as above-mentioned solvent;Preferably toluene,
The a variety of mixing of dimethylbenzene, ethyl acetate;More preferably ethyl acetate is a kind of;Most preferably toluene, ethyl acetate mixing.
It is that alkynol class is catalyzed reaction suppressor, optional inhibitor as above-mentioned reaction suppressor are as follows:
Phenylacetylene, 1 one acetenyl, one 1 one cyclohexanol, t etram-ethyltetravinylcyclotetrasiloxane, 2 monomethyl, one 3 one butine
One 2 one alcohol of base, 3 monomethyl, one 1 one acetenyl, one 3 one alcohol, 3,5 1 dimethyl, one 1 one hexin base, one 3 one alcohol, 3 monomethyls 1
One of which or any combination in one dodecyne, one 3 one alcohol.
Meanwhile the invention also discloses a kind of preparation method of rapid curing silicone pressure sensitive gluing agent, it is used to prepare
The silicone pressure sensitive gluing agent stated, mainly comprises the steps that
1) solvent and polysiloxanes containing vinyl are added in reaction kettle, it is small in 40-50 DEG C of at a temperature of stirring 3
When, obtain the Silicone Rubber Dispersion that solid content is 24.5%-25.5%;
2) solvent is taken again, is stirred and is mixed for 1:1 by mass parts ratio with the Silicone Rubber Dispersion in step 1);
3) in whipping process, methyl vinyl MQ organic silicon rigidity-increasing stick, crosslinking agent, reaction suppressor is sequentially added and is urged
Agent, and be sufficiently mixed and uniformly obtain the silicone pressure sensitive gluing agent.
The preparation method of above-mentioned adhesive and adhesive in the present invention, can be used for PET base material silicone protective film, is suitable for
Material is posted, the surface protection of metal and general plastic front board, is very suitable to the use of electronic manufacture processing industry.
Wherein, it invention additionally discloses a kind of adhesive tape, includes at least: substrate layer and adhesive layer;Adhesive layer is coated on base
The one or both sides of material layer;Wherein the silicone pressure sensitive gluing agent of adhesive layer preparation method as described in aforementioned present invention preparation exists
160 DEG C of solidification 10S-60S are obtained.
Layer is chosen as PET base material, PE substrate, PI substrate etc. as above-mentioned base material.
In order to preferably guarantee the quality and preparation process controllability of adhesive;Parameter detecting side in the application described below
Method and effective evaluation method:
<1>rapid curing is evaluated:
Benchmark: 160 DEG C of baking different times is evaluated, peeling force stability is tested;
Use equipment: baking oven;
Device parameter: 160 DEG C;
Sample parameters: 50PET+10um glue is thick;
Points for attention: coated sample glue thickness is consistent.
<2>peel strength test:
Test method: the experimental method of GB/T 2792-2014 adhesive tape peel strength;
Adhesive tape: being cut into the standard test piece sticking steel plate of wide 25.4mm, long 300mm by test condition, tests environment: 1. temperature 23
±2℃;65 ± 5RH of relative humidity;
Points for attention: it is noted that bubble cannot be had in adhesive tape after having pressed.
<3>fugitive constituent is tested:
Test method: ASTM E595 fugitive constituent test;
Test condition: 125 DEG C of temperature, the humidity 5% of environment, vacuum state 10-12Pa.Test 8 hours;
Points for attention: the substance of low molecular weight is most volatile.
<4>bulk density is tested:
Test method: loose material is under stacking states, the quality of unit volume;
Test condition: be calculated as follows: ρ '=m/V ', in formula: ρ ' is bulk density, kg/m;M is material in a constant volume device
Interior quality, kg;V ' is the stacking volume of material, that is, is packed into the volume of container;
Points for attention: volume m is comprising the total volume including void among particles and particle internal void.
<5>average particle size is tested:
Test method: microscopic method;
Test condition: narrow dynamic range, 1:20;Time of measuring is long, and about 20 minutes;
Points for attention: being dispersed with certain difficulty to submicron-sized particulate, be limited by diffraction limit, and can not detect ultra-fine
Grain.
<6>viscosity test:
Test method: 2794-81 adhesive viscosity measurement method of GB;
Test condition: it is measured at (25 ± 0.5) DEG C;
Points for attention: test result is calculated by instrument requirements.It should indicate that the model of rotational viscometer, rotor number, revolving speed
And measuring temperature.
<7>molecular weight test:
Test method: exclusion chromatography (GPC);
Test condition: molecular weight is measured according to different size of molecule residence time difference in the medium;
Points for attention: being a kind of relative manner, must combine the cooperation of other methods.
The present invention is described in detail is come with specific embodiment below:
Embodiment 1:
Taking 25 parts of weight average molecular weight is the ethenyl blocking silicon rubber of 550000, contents of ethylene 0.08%, is scattered in 75
The in the mixed solvent of part toluene and ethyl acetate mass ratio 1:1 obtain the Silicone Rubber Dispersion that solid content is 25%, carry out abundant
Swelling;The silicone oil and 0.5 part of reaction suppressor of 1 part of silicon hydrogen content 1.1mol/100g are added, it is fully dispersed;Add 1 part
Disperse in 10 parts of toluene solutions in advance diluted platinum catalyst fully dispersed 30 minutes, it, will by pumping stirring to obtain glue
Glue enters slit type coating head and is coated in 50 microns of thick PET bases, controls wet 80 μm of glue thickness, obtains adhesive tape.
By above-mentioned adhesive tape be sent into 7 section, 40 meters of air blast drying tunnels, 110 DEG C of temperature gradient, 135 DEG C, 150 DEG C, 160 DEG C, 165 DEG C,
160 DEG C, 120 DEG C, linear speed 20m/min obtain final silicone pressure sensitive adhesive tape.
Embodiment 2:
Taking 25 parts of weight average molecular weight is 550000, the ethenyl blocking silicon rubber of contents of ethylene 0.08% and 4.5 parts of second
Amount vinyl content 0.2%, the MQ organic silicon rigidity-increasing stick that M/Q ratio is 0.7, are scattered in 140 parts of toluene and ethyl acetate mass ratio 1:1
In the mixed solvent obtain solid content be 25% Silicone Rubber Dispersion, be sufficiently swollen;Add 1 part of silicon hydrogen content
The silicone oil of 1.1mol/100g and 0.5 part of reaction suppressor, it is fully dispersed;1 part is added to divide in 10 parts of toluene solutions in advance
It dissipates diluted platinum catalyst fully dispersed 30 minutes, by pumping stirring to obtain glue, glue is entered into slit type coating head coating
It is 70 μm thick in 50 microns of thick PET bases, controlling wet glue, obtain adhesive tape.
By above-mentioned adhesive tape be sent into 7 section, 40 meters of air blast drying tunnels, 110 DEG C of temperature gradient, 135 DEG C, 150 DEG C, 160 DEG C, 165 DEG C,
160 DEG C, 120 DEG C, linear speed 20m/min obtain final silicone pressure sensitive adhesive tape.
Embodiment 3:
Taking 25 parts of weight average molecular weight is 550000, the ethenyl blocking silicon rubber of contents of ethylene 0.08% and 35 parts of second
Amount vinyl content 0.2%, the MQ organic silicon rigidity-increasing stick that M/Q ratio is 0.7, are scattered in 140 parts of toluene and ethyl acetate mass ratio 1:1
In the mixed solvent obtain solid content be 25% Silicone Rubber Dispersion, be sufficiently swollen;Add 1 part of silicon hydrogen content
The silicone oil of 1.1mol/100g and 0.5 part of reaction suppressor, it is fully dispersed;1 part is added to divide in 10 parts of toluene solutions in advance
It dissipates diluted platinum catalyst fully dispersed 30 minutes, by pumping stirring to obtain glue, glue is entered into slit type coating head coating
It is 50 μm thick in 50 microns of thick PET bases, controlling wet glue, obtain adhesive tape.
By above-mentioned adhesive tape be sent into 7 section, 40 meters of air blast drying tunnels, 110 DEG C of temperature gradient, 135 DEG C, 150 DEG C, 160 DEG C, 165 DEG C,
160 DEG C, 120 DEG C, linear speed 20m/min obtain final silicone pressure sensitive adhesive tape.
Comparative example 1:
Taking 25 parts of weight average molecular weight is 550000, the ethenyl blocking silicon rubber of contents of ethylene 0.08% and 45 parts of second
Amount vinyl content 0.2%, the MQ organic silicon rigidity-increasing stick that M/Q ratio is 0.7, are scattered in 100 parts of toluene and ethyl acetate mass ratio 1:1
In the mixed solvent obtain solid content be 25% Silicone Rubber Dispersion, be sufficiently swollen;Add 0.8 part of silicon hydrogen content
The silicone oil of 1.1mol/100g and 0.5 part of reaction suppressor, it is fully dispersed;0.6 part is added in advance in 10 parts of toluene solutions
Disperse diluted platinum catalyst fully dispersed 30 minutes, by pumping stirring to obtain glue, glue is entered into slit type coating head and is applied
It is distributed in 50 microns of thick PET bases, controls wet 50 μm of glue thickness, obtain adhesive tape.
By above-mentioned adhesive tape be sent into 7 section, 40 meters of air blast drying tunnels, 110 DEG C of temperature gradient, 135 DEG C, 150 DEG C, 160 DEG C, 165 DEG C,
160 DEG C, 120 DEG C, linear speed 20m/min obtain final silicone pressure sensitive adhesive tape.
Comparative example 2:
Taking 25 parts of weight average molecular weight is 550000, the ethenyl blocking silicon rubber of contents of ethylene 0.08% and 4.5 parts of second
Amount vinyl content 0.2%, the MQ organic silicon rigidity-increasing stick that M/Q ratio is 0.7, are scattered in 140 parts of toluene and ethyl acetate mass ratio 1:1
In the mixed solvent obtain solid content be 25% Silicone Rubber Dispersion, be sufficiently swollen;Add 1 part of silicon hydrogen content
The silicone oil of 1.1mol/100g and 0.5 part of reaction suppressor, it is fully dispersed;0.4 part is added in advance in 10 parts of toluene solutions
Disperse diluted platinum catalyst fully dispersed 30 minutes, by pumping stirring to obtain glue, glue is entered into slit type coating head and is applied
It is distributed in 50 microns of thick PET bases, controls wet 50 μm of glue thickness, obtain adhesive tape.
By above-mentioned adhesive tape be sent into 7 section, 40 meters of air blast drying tunnels, 110 DEG C of temperature gradient, 135 DEG C, 150 DEG C, 160 DEG C, 165 DEG C,
160 DEG C, 120 DEG C, linear speed 20m/min obtain final silicone pressure sensitive adhesive tape.
The adhesive tape in 1-3 of the embodiment of the present invention and comparative example 1-2 is taken, respectively in the test data result of condition 1 and condition 2
It is as shown in table 1:
Condition 1: be statically placed in 23 ± 1 DEG C, humidity be 2h in 50 ± 5% environment, it is strong to test 180 ° of different baking times removings
It spends (gf/inch).
Condition 2: after being placed at room temperature for 72h, be statically placed in 23 ± 1 DEG C, humidity be 50 ± 5% environment in 2h, test different bakings
180 ° of peel strengths (gf/inch) of time.
Table 1:
In summary (data analysis):
By embodiment 1,2,3, it can be seen that cross-linked speed is fast, production complete it is i.e. cured completely, and 10S and 1min stripping
It is not different from power;Peeling force is more stable, unchanged after 72 hours;Adhesion strength range is wide, can meet the production of different viscosity
Product.
It is right by embodiment 3 and comparative example 1 it can be seen that after methyl vinyl MQ organic silicon rigidity-increasing stick is more than 35 parts by weight
Efficient Adhesive Promotion is unhelpful.
By embodiment 2 and comparative example 2 it can be seen that platinum catalyst amount is added less, catalytic rate will affect;Catalyst
0.6 part of usage amount, rapid curing requirement can be met.
Specification described herein and general reason to the structure of various embodiments is desirable to provide to the explanation of embodiment
Solution.The specification and explanation are not intended to serve as all members of equipment and system using structures described herein or method
The exhaustive and comprehensive description of part and feature.Individual embodiment is provided in single embodiment in which can also be combined, and on the contrary,
For brevity, described in the context of single embodiment various features also discriminably or with any sub-portfolio mention
For.In addition, referring to that the value stated in range includes each value in the range.Only after reading this description,
Those skilled in the art can understand many other embodiments.Other embodiments can be used and the embodiment can be from this hair
Bright export, so that without departing from the scope of the invention, structure substitution, logic substitution or another variation can be carried out.Cause
This, the present invention should be considered as illustrative and not restrictive.
Claims (10)
1. a kind of rapid curing silicone pressure sensitive gluing agent, which is characterized in that the adhesive by following raw material in a kettle
Addition reaction obtains:
The polysiloxanes containing vinyl of 20-30 parts by weight;
The methyl vinyl MQ organic silicon rigidity-increasing stick of 0-35 parts by weight;
1.0-1.2 the crosslinking agent of parts by weight;
The platinum catalyst of 0.6-0.7 parts by weight;
The reaction suppressor of 0.1-0.2 parts by weight;
And the solvent of 100-200 parts by weight;
The solid content of the obtained adhesive is 10%-25%;And under 160 DEG C of solidification temperature, 10S-60S be can be realized
It is fully cured.
2. a kind of rapid curing silicone pressure sensitive gluing agent according to claim 1, which is characterized in that the polysiloxanes
Weight average molecular weight be 450000-650000;The vinyl is end group and mass percent is 0.07%-0.08%;Volatilization
Part≤1.30%;
The general structure of the polysiloxanes are as follows:
R(CH3)2SiO[Si(CH3)2O]n[Si(CH3) (CH=CH2)O]mSi(CH3)2R, wherein R is vinyl.
3. a kind of rapid curing silicone pressure sensitive gluing agent according to claim 1, which is characterized in that the MQ organosilicon
The structural formula of tackifier are as follows:
[(CH3)2(CH2=CH) SiO1/2]a[(CH3)3SiO1/2]b[SiO4/2]c,
Wherein [(CH3)2(CH2=CH) SiO1/2]a[(CH3)3SiO1/2]bFor M unit, [SiO4/2]cFor Q unit;M unit and Q are mono-
The ratio of member is that the value of (a+b)/c is 0.7-0.8;Contents of ethylene 0.15%-0.2%;
Bulk density is 0.2-0.3g/cm3;Average particle size is 90-110 μm.
4. a kind of rapid curing silicone pressure sensitive gluing agent according to claim 1, which is characterized in that the crosslinking agent is
Silicone oil containing silicon hydrogen (SiH) group, molecular structure are as follows:
(CH3)3SiO[(CH3)2SiO]m[(CH3)(H)SiO]nSi(CH3)3;
Wherein the mass percent of H is 1.0%-1.2%;25 DEG C of viscosity is 30-100mpas;Fugitive constituent < 1%.
5. a kind of rapid curing silicone pressure sensitive gluing agent according to claim 1, which is characterized in that the platinum catalysis
Platinum content is 2000ppm-3000ppm in agent;The platinum catalyst is the platinum catalyst being coordinated with methyl vinyl silicone,
And it can effective catalytic addition reaction at 80 DEG C or more.
6. a kind of rapid curing silicone pressure sensitive gluing agent according to claim 5, which is characterized in that the platinum catalysis
Agent is that karr, this special catalyst carries out ligand exchange using the siloxane oligomer containing chain alkyl and vinyl, is made into platinum-
The catalyst of a, w- bis- (n- octyl) Polymethyl methacrylate complex.
7. a kind of rapid curing silicone pressure sensitive gluing agent according to claim 1, which is characterized in that the solvent is first
One of benzene, dimethylbenzene, ethyl acetate or a variety of mixing.
8. a kind of rapid curing silicone pressure sensitive gluing agent according to claim 1, which is characterized in that the response inhabitation
Agent is that alkynol class is catalyzed reaction suppressor.
9. a kind of preparation method of rapid curing silicone pressure sensitive gluing agent, is used to prepare such as claim 1-8 any one institute
The silicone pressure sensitive gluing agent stated, it is characterised in that: the following steps are included:
1) solvent and polysiloxanes containing vinyl are added in reaction kettle, 40-50 DEG C at a temperature of stir 3 hours, obtain
The Silicone Rubber Dispersion A for being 24.5%-25.5% to solid content;
2) solvent is taken again, is stirred and is mixed for 1:1 by mass parts ratio with the Silicone Rubber Dispersion A in step 1);
3) in whipping process, methyl vinyl MQ organic silicon rigidity-increasing stick, crosslinking agent, reaction suppressor and catalysis are sequentially added
Agent, and be sufficiently mixed and uniformly obtain the silicone pressure sensitive gluing agent.
10. a kind of adhesive tape, which is characterized in that include at least: substrate layer and adhesive layer;The adhesive layer is coated on the base
The one or both sides of material layer;The adhesive layer is as the silicone pressure sensitive gluing by the preparation of preparation method described in claim 8
Agent is obtained in 160 DEG C of solidification 10S-60S.
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Cited By (9)
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CN111072712A (en) * | 2019-12-23 | 2020-04-28 | 东莞市贝特利新材料有限公司 | Organic silicon tackifier, preparation method thereof and high-transparency self-adhesive addition type organic silicon rubber composition |
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CN112708396A (en) * | 2020-12-29 | 2021-04-27 | 苏州添易朗科技有限公司 | Preparation of integrated black silica gel OCA |
CN114686140A (en) * | 2020-12-31 | 2022-07-01 | 太湖金张科技股份有限公司 | Silica gel protection film that low silicon shifted |
CN113388362A (en) * | 2021-07-22 | 2021-09-14 | 江苏斯迪克新材料科技股份有限公司 | Low-climbing organic silicon pressure-sensitive adhesive and preparation method and application thereof |
CN113667449A (en) * | 2021-09-10 | 2021-11-19 | 江苏斯迪克新材料科技股份有限公司 | Double-sided adhesive tape for low-surface-energy silicon rubber surface and preparation method thereof |
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CN114316893B (en) * | 2021-12-28 | 2023-08-11 | 万华化学集团股份有限公司 | Organosilicon pressure-sensitive adhesive composition and pressure-sensitive adhesive product |
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