CN110157374A - A kind of organic pressure-sensitive gel and preparation method thereof - Google Patents
A kind of organic pressure-sensitive gel and preparation method thereof Download PDFInfo
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- CN110157374A CN110157374A CN201810252793.4A CN201810252793A CN110157374A CN 110157374 A CN110157374 A CN 110157374A CN 201810252793 A CN201810252793 A CN 201810252793A CN 110157374 A CN110157374 A CN 110157374A
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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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- 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
- 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
Abstract
The invention discloses a kind of organic pressure-sensitive gels and preparation method thereof, belong to organic pressure-sensitive gel field of material technology, and spy is standby to be related to a kind of organic pressure-sensitive gel and preparation method thereof of ultralow peeling force.Organic pressure-sensitive gel in the present invention uses the vinyl polysiloxane of two kinds of different molecular weights, and pressure sensitive adhesive can be made to have preferable levelability, good operability；By control contents of ethylene and hydroxy radical content, it can make pressure sensitive adhesive that there is ultralow peeling force；Selection can participate in the Anchor Agent of crosslinking, and the not degumming in 4 hours of the bonding force of pressure sensitive adhesive and PET base material and boiling can be improved and do not lose powder.The organic pressure-sensitive gel can be widely used in the related fieldss such as the pressure sensitive adhesive tape, protective film of electronic product or isolation film for requiring low removing.
Description
Technical field
The present invention relates to silicone pressure sensitive field of material technology, in particular to a kind of silicone pressure sensitive of ultralow peel strength
Glue and preparation method thereof.
Background technique
Organic pressure-sensitive gel is a kind of novel tool adhesive with broad prospects for development, it not only has pressure sensitive adhesive must
The pressure-sensitive needed is difficult to the performance having there are many more other materials: (1) having to high energy and low energy surface material good viscous
Attached property, therefore it has preferable glue to untreated difficult adhesion material, such as polytetrafluoroethylene (PTFE), polyimides, polycarbonate
Connect performance；(2) there is high and low temperature resistance outstanding, can be used for a long time between -50~200 DEG C, and under high temperature and low temperature
Still maintain its adhesive strength and flexibility；(3) there is good chemical inertness, long service life, while having outstanding resistance to
Moist and electrical property；(4) good chemical-resistance and solvent resistance outstanding and electrical property；(5) corrosion-free to metal；(6)
Dielectric properties are good.Especially with the fast development of the industries such as mobile phone, OLED display screen, associated mating industry-electricity
Sub- product screen and related protective film and isolation film industry are also developed rapidly therewith.
It is mainly traditionally initial bonding strength and holding power to the evaluation criterion of pressure sensitive adhesive service performance, and for mobile phone, electronics
For the protection of product screen and the isolation film of isolation cohesive material, more applicable evaluation method is 180 ° of peel strengths, removing
Strength stability, water boiling resistance ageing properties etc..
Different electronic products and different display substrates and different purposes, to the performance requirement of organic pressure-sensitive gel
Also different, current organic pressure-sensitive gel has been achieved for biggish progress, highest peeling force in the technical aspect of high peeling force
Up to 1800g/25mm or so, but reach stable low removing, the ultralow peeling force of especially 180 ° peeling force < 0.8g has
Machine silicon pressure sensitive adhesive emerges still without large-scale product.
Summary of the invention
The purpose of the present invention is to provide a kind of organic pressure-sensitive gels and preparation method thereof, to solve in above-mentioned background technique
The problem of proposition.
To achieve the above object, the invention provides the following technical scheme:
A kind of organic pressure-sensitive gel, including base rubber component, catalyst component, cross-linking agent component and Anchor Agent component；
The preparation method of the base rubber component, comprising the following steps: the poly- silicon oxygen of vinyl for being 50~700,000 by molecular weight
The vinyl polysiloxane that alkane and molecular weight are 5000~20,000 is added in reaction kettle, add diluent into reaction kettle and
Vinyl polysiloxane sufficiently dissolves dispersion, adds 0.1~2% basic catalyst of vinyl polysiloxane total amount to instead
It answers in kettle, reacts 2~6 hours, then carry out distillation water removal, react in a kettle under conditions of 60~90 DEG C and nitrogen protection
0.04~0.4 part of inhibitor is added in kettle, stirs evenly；
The catalyst component is the platinum metal catalyst of 2000~7000ppm of platinum content；
The cross-linking agent component is hydrogen-based content in 1.0~1.6% hydrogen-based polysiloxanes；
The Anchor Agent component is to contain one of epoxy group, ether, acyloxy or a variety of hydrogen-based polysiloxanes.
As a further solution of the present invention: further including independent chuck, the independent chuck includes base in parts by weight
100 parts of glue component, catalyst component are 0.5~2 part, cross-linking agent component is 0.5~2 part, bonding agent component is 0.5~1.5 part.
As further scheme of the invention: the vinyl for the vinyl polysiloxane that the molecular weight is 50~700,000
Content is 0.15~0.6wt%；The contents of ethylene for the vinyl polysiloxane that the molecular weight is 5000~20,000 is 0.5~
2.0wt%.
As further scheme of the invention: the structural formula of the vinyl polysiloxane are as follows:
Wherein m, n are the natural number greater than 1.
As further scheme of the invention: the structural formula of the Anchor Agent component are as follows:
Wherein R1And R2For H or alkyl；X is epoxy group, ether or acyloxy；X, y are natural number and 1≤x≤7；1≤y≤4.
As further scheme of the invention: the inhibitor is t etram-ethyltetravinylcyclotetrasiloxane, divinyl
Base tetramethyl disiloxane, allylene alcohol, ethynylcyclohexanol, methyl butynol, 3,5- dimethyl -1- hexin base -3- alcohol,
One of which or any combination in 3- methyl-1-dodecyne-3- alcohol.
As further scheme of the invention: the diluent is volatile solvents.
As further scheme of the invention: the volatile solvents are petroleum ether, toluene, dimethylbenzene, solvent naphtha
Or ethyl acetate.
As further scheme of the invention: the structural formula of the hydrogen-based polysiloxanes are as follows:
Wherein R3, R4,R5,R6For H or methyl；K is the natural number more than or equal to 0；J is the natural number more than or equal to 0 and less than 2.
As further scheme of the invention: the basic catalyst is ammonium hydroxide, tetramethylammonium hydroxide, hexamethyl two
The one or more of silazane etc..
A kind of preparation method of above-mentioned organic pressure-sensitive gel, comprising the following steps:
1) it prepares base rubber component: being 50~700,000 vinyl polysiloxane and 20~40 parts points by 60~80 parts of molecular weight
Son amount is added in reaction kettle for 5000~20,000 vinyl polysiloxane, adds 60~120 parts of diluents, is stirred, is made second
Alkenyl polysiloxanes sufficiently dissolves dispersion, and 0.1~2% basic catalyst of vinyl polysiloxane total amount is added, 60~
It 80 DEG C, is reacted 2~6 hours under conditions of nitrogen protection, then is warming up to solvent boiling, distill out the water reflected, reaction kettle
Cooling, 0.04~0.4 part of inhibitor is added in reaction kettle, stirs evenly, as base rubber component；
2) preparation of pressure sensitive adhesive: by 100 parts of base rubber components, 50~150 parts of diluents is added, stir evenly；Successively exist again
0.5~2 part of cross-linking agent component, 0.5~1.5 part of Anchor Agent component and 0.5~2 part of catalyst group are slowly added under conditions of stirring
Part, 5~10min is stirred after all adding, pressure sensitive adhesive, which is prepared, to be completed；
3) solidification of pressure sensitive adhesive: by prepared pressure-sensitive adhesives, on a pet film, coating thickness is according to specific requirement
It determines, places into and solidify 1~2min in 120~150 DEG C of baking ovens or be directly entered setting maximum temperature as the baking no more than 165 DEG C
Solidify in road.
Compared with prior art, the beneficial effects of the present invention are:
1, the ultralow peel strength of organic pressure-sensitive gel and vinyldimethicone used in the present invention
Molecular structure is related with contents of ethylene, and the hydroxyl quantity in the molecular structure of vinyldimethicone is lower, ethylene
Base content is higher, then 180 ° of peel strengths are lower.But due to inevitably containing one in the synthesis process of vinyl silicone oil
Quantitative hydroxyl, thus by the termination process of hydroxyl, the hydroxy radical content in molecular structure can be reduced to a certain extent.This
Outside, contents of ethylene is higher, and crosslink density is higher, can also be substantially reduced when being bonded to 180 ° of peel strengths of substrate.
But since contents of ethylene is more than certain ratio, the bonding force of substrate can be decreased obviously, to cause initial adhesion
Relatively low, degumming or shedding after boiling aging, therefore, the present invention should control the content of vinyl in a certain range, both may be used
Guarantee that there is stable low peel strength, and guarantee that initial adhesion is good, water boiling resistance ageing properties are excellent；
2, vinyldimethicone weight molecule chain length has apparent influence to the cohesive strength of pressure sensitive adhesive, point
Subchain is longer, and viscosity is bigger, and cohesive strength is higher.But the viscosity that molecular weight height will cause organic pressure-sensitive gel is higher, to lead
Operability is caused to be deteriorated, thus the present invention selects the vinyldimethicone of high low molecular weight collocation, it can be organic in guarantee
Under conditions of silicon pressure sensitive adhesive has good operability, there is excellent ontology cohesive strength；
3, the present invention in inhibitor using t etram-ethyltetravinylcyclotetrasiloxane, divinyl tetramethyl disiloxane,
Allylene alcohol, ethynylcyclohexanol, methyl butynol, 3,5- dimethyl-1- hexin base-3- alcohol, 3- methyl-1-dodecyne-
Or mixtures thereof 3- alcohol etc., by adjusting the type and content of inhibitor, it is long to can reach the normal temperature storage time, can be quick after heating
Cured effect.The especially inhibitor of alkynol class belongs to the polymerization inhibitor that low temperature polymerization inhibition effect is very good, high temperature quickly volatilizees
Agent, in the present invention by control its additive amount at 0.04~0.2 part, can make product of the present invention at normal temperature within 8 hours not
Meeting gel, and can be quickly evaporated completely under the conditions of 120 DEG C without influencing to solidify；
4, the Anchor Agent in the present invention be containing bonding group epoxy group, ether, acyloxy hydrogen-based polysiloxanes, it is special
Point is that Anchor Agent can participate in the cross-linking reaction of pressure sensitive adhesive and play the role of good interfacial bonding, will not be because of moisture
It penetrates into and is detached from pressure sensitive adhesive ontology, to be not in the phenomenon that whitening mist or degumming after boiling aging；
5, organic pressure-sensitive gel of the present invention has the characteristics that ultralow peeling force, peeling force stabilization, high-temp resisting high-humidity resisting, can be extensive
The related fields of low removing is needed applied to protective film of electronic product and isolation film etc..
Specific embodiment
Combined with specific embodiments below, the organic pressure-sensitive gel technical solution in the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
A kind of organic pressure-sensitive gel, including base rubber component, catalyst component, cross-linking agent component and Anchor Agent component；
The preparation method of the base rubber component, comprising the following steps: the poly- silicon oxygen of vinyl for being 50~700,000 by molecular weight
The vinyl polysiloxane that alkane and molecular weight are 5000~20,000 is added in reaction kettle, add diluent into reaction kettle and
Vinyl polysiloxane sufficiently dissolves dispersion, adds 0.1~2% basic catalyst of vinyl polysiloxane total amount to instead
It answers in kettle, reacts 2~6 hours, then carry out distillation water removal, react in a kettle under conditions of 60~90 DEG C and nitrogen protection
0.04~0.4 part of inhibitor is added in kettle, stirs evenly；It further include independent chuck, the independent chuck wraps in parts by weight
Include 100 parts of base rubber component, catalyst component is 0.5~2 part, cross-linking agent component is 0.5~2 part, bonding agent component be 0.5~
1.5 part.
The catalyst component is the platinum metal catalyst of 2000~7000ppm of platinum content；
The cross-linking agent component is hydrogen-based content in 1.0~1.6% hydrogen-based polysiloxanes；
The Anchor Agent component is to contain one of epoxy group, ether, acyloxy or a variety of hydrogen-based polysiloxanes.
The contents of ethylene for the vinyl polysiloxane that the molecular weight is 50~700,000 is 0.15~0.6wt%；It is described
The contents of ethylene for the vinyl polysiloxane that molecular weight is 5000~20,000 is 0.5~2.0wt%.
The structural formula of the vinyl polysiloxane are as follows:Wherein m, n are the nature greater than 1
Number.
The structural formula of the Anchor Agent component are as follows:Wherein R1And R2For H or alkyl；X is ring
Oxygroup, ether or acyloxy；X, y are natural number and 1≤x≤7；1≤y≤4.
The inhibitor is t etram-ethyltetravinylcyclotetrasiloxane, divinyl tetramethyl disiloxane, allylene
Alcohol, ethynylcyclohexanol, methyl butynol, 3,5- dimethyl-1- hexin base-3- alcohol, in 3- methyl-1-dodecyne-3- alcohol
One of or any combination.
The diluent is volatile solvents.
The volatile solvents are petroleum ether, toluene, dimethylbenzene, solvent naphtha or ethyl acetate.
The structural formula of the hydrogen-based polysiloxanes are as follows:Wherein R3, R4,R5,R6For H or first
Base；K is the natural number more than or equal to 0；J is the natural number more than or equal to 0 and less than 2.
The basic catalyst is the one or more of ammonium hydroxide, tetramethylammonium hydroxide, hexamethyldisilazane etc..
Point of vinyldimethicone used in the ultralow peel strength and the present invention of organic pressure-sensitive gel
Minor structure is related with contents of ethylene, and the hydroxyl quantity in the molecular structure of vinyldimethicone is lower, vinyl
Content is higher, then 180 ° of peel strengths are lower.But it is certain due to inevitably containing in the synthesis process of vinyl silicone oil
The hydroxyl of amount, thus pass through the alkoxy end-capped processing of hydroxyl, the hydroxy radical content in molecular structure can be reduced to a certain extent.
In addition, contents of ethylene is higher, crosslink density is higher, also can obviously drop when being bonded to 180 ° of peel strengths of substrate
It is low.But since contents of ethylene is more than certain ratio, the bonding force of substrate can be decreased obviously, to cause initially to adhere to
Power is relatively low, comes unglued after boiling aging, and therefore, the present invention should control the content of vinyl in a certain range, both can guarantee
With stable low peel strength, and guarantee that initial adhesion is good, water boiling resistance ageing properties are excellent；
Vinyldimethicone weight molecule chain length has apparent influence, molecule to the cohesive strength of pressure sensitive adhesive
Chain is longer, and viscosity is bigger, and cohesive strength is higher.But the viscosity that molecular weight height will cause organic pressure-sensitive gel is higher, so as to cause
Operability is deteriorated, thus the present invention selects the vinyldimethicone of high low molecular weight collocation, can guarantee organosilicon
Under conditions of pressure sensitive adhesive has good operability, there is excellent cohesive strength；
Inhibitor uses t etram-ethyltetravinylcyclotetrasiloxane, divinyl tetramethyl disiloxane, first in the present invention
Ethyl-acetylene alcohol, ethynylcyclohexanol, methyl butynol, 3,5- dimethyl-1- hexin base-3- alcohol, 3- methyl-1-dodecyne-3-
Or mixtures thereof alcohol etc., by adjusting the type and content of inhibitor, it is long to can reach the normal temperature storage time, can quickly consolidate after heating
The effect of change.The especially inhibitor of alkynol class belongs to the polymerization inhibitor that low temperature polymerization inhibition effect is very good, high temperature quickly volatilizees,
In the present invention by controlling its additive amount at 0.04~0.2 part, product of the present invention can be made not coagulate within 8 hours at normal temperature
Glue, and can be quickly evaporated completely under the conditions of 120 DEG C without influencing to solidify；
Anchor Agent in the present invention be containing bonding group epoxy group, ether, acyloxy hydrogen-based polysiloxanes, feature
It is that Anchor Agent can participate in the cross-linking reaction of pressure sensitive adhesive and play the role of good interfacial bonding, it will not be because of the infiltration of moisture
Enter and be detached from pressure sensitive adhesive ontology, to be not in the phenomenon that whitening mist or degumming after boiling aging；
Organic pressure-sensitive gel of the present invention has the characteristics that ultralow peeling force, peeling force stabilization, high-temp resisting high-humidity resisting, can answer extensively
The related fields of low removing is needed for protective film of electronic product and isolation film etc..
It is described in detail below by way of preparation method of the specific embodiment to the organic pressure-sensitive gel in the present invention, each reality
Example is applied to be illustrated for including base rubber, catalyst component, bonding agent component and the organic pressure-sensitive gel of cross-linking agent component.
In embodiments, unless otherwise stated, all numbers are by weight；In order to express easily, in each embodiment, molecular weight is
50~700,000 vinyldimethicone indicates that molecular weight is 5000~20,000 with vinyldimethicone A
Vinyl polysiloxane is indicated with vinyldimethicone B.
Embodiment 1:
1) base rubber component is prepared:
By 80 parts of contents of ethylene be 0.2% vinyldimethicone A and 20 parts of contents of ethylene be 0.6%
Vinyldimethicone B be added in reaction kettle, add 120 parts of diluents, stir, make vinyl polysiloxane
Sufficiently dissolution dispersion, is added 0.1% basic catalyst of vinyl polysiloxane total amount, at 60~80 DEG C, nitrogen protection
Under the conditions of react 6 hours, then be warming up to solvent boiling, distill out the water reflected, it is cooling, 0.04 part of inhibitor is added, stirs
It mixes uniformly, as base rubber component.
2) preparation of pressure sensitive adhesive:
By 100 parts of base rubbers, 150 parts of diluents are added, stir evenly；Successively it is slowly added to 2 parts under stirring conditions again
Crosslinking agent, 1.5 parts of Anchor Agents and 2 parts of catalyst stir 5~10min after all adding, pressure sensitive adhesive, which is prepared, to be completed.
3) solidification of pressure sensitive adhesive:
On a pet film by prepared pressure-sensitive adhesives, it places into 120 DEG C of baking ovens and solidifies 2min.
Base rubber component, prepared pressure sensitive adhesive and the pressure sensitive adhesive tape being cured are tested, performance parameter is shown in Table 1.
Embodiment 2:
1) base rubber component is prepared:
By 60 parts of contents of ethylene be 0.6% vinyldimethicone A and 20 parts of contents of ethylene be 2.0%
Vinyldimethicone B be added in reaction kettle, add 60 parts of diluents, stir, make vinyl polysiloxane
Sufficiently dissolution dispersion, adds 2% basic catalyst of vinyl polysiloxane total amount, at 60~80 DEG C, nitrogen protection
Under the conditions of react 3 hours, then be warming up to solvent boiling, distill out the water reflected, it is cooling, 0.4 part of inhibitor is added, stirs
Uniformly, as base rubber component.
2) preparation of pressure sensitive adhesive:
By 100 parts of base rubbers, 50~150 parts of diluents are added, stir evenly；It is successively slowly added under stirring conditions again
0.5 part of crosslinking agent, 1.5 parts of Anchor Agents and 2 parts of catalyst stir 5~10min after all adding, pressure sensitive adhesive, which is prepared, to be completed.
3) solidification of pressure sensitive adhesive:
On a pet film by prepared pressure-sensitive adhesives, coating thickness is determined according to specific requirement, places into 120
Solidify 1~2min in~150 DEG C of baking ovens or is directly entered setting maximum temperature to solidify in the drying tunnel no more than 165 DEG C.
Base rubber component, prepared pressure sensitive adhesive and the pressure sensitive adhesive tape being cured are tested, performance parameter is shown in Table 1.
Embodiment 3:
1) base rubber component is prepared:
By 70 parts of contents of ethylene be 0.3% vinyldimethicone A and 30 parts of contents of ethylene be 2.0%
Vinyldimethicone B be added in reaction kettle, add 120 parts of diluents, stir, make vinyl polysiloxane
Sufficiently dissolution dispersion, adds 1% silazane of vinyl polysiloxane total amount, at 60~80 DEG C, the condition of nitrogen protection
Lower reaction 4 hours, then it is warming up to solvent boiling, the water reflected is distilled out, it is cooling, 0.2 part of inhibitor is added, stirring is equal
It is even, as base rubber component.
2) preparation of pressure sensitive adhesive:
By 100 parts of base rubbers, 100 parts of diluents are added, stir evenly；Successively it is slowly added to 1.0 under stirring conditions again
Part crosslinking agent, 1.5 parts of Anchor Agents and 1.2 parts of catalyst stir 5~10min after all adding, pressure sensitive adhesive, which is prepared, to be completed.
3) solidification of pressure sensitive adhesive:
On a pet film by prepared pressure-sensitive adhesives, coating thickness is determined according to specific requirement, places into 150
Solidify 1min in DEG C baking oven.
Base rubber component, prepared pressure sensitive adhesive and the pressure sensitive adhesive tape being cured are tested, performance parameter is shown in Table 1.
Embodiment 4:
1) base rubber component is prepared:
By 65 parts of contents of ethylene be 0.2% vinyldimethicone A and 40 parts of contents of ethylene be 1.0%
Vinyldimethicone B be added in reaction kettle, add 100 parts of diluents, stir, make vinyl polysiloxane
Sufficiently dissolution dispersion, adds 0.1% silazane of vinyl polysiloxane total amount, at 60~80 DEG C, the item of nitrogen protection
It is reacted 5 hours under part, then is warming up to solvent boiling, distill out the water reflected, it is cooling, 0.1 part of inhibitor is added, stirring is equal
It is even, as base rubber component.
2) preparation of pressure sensitive adhesive
By 100 parts of base rubbers, 50 parts of diluents are added, stir evenly；Successively it is slowly added to 0.8 part under stirring conditions again
Crosslinking agent, 1.0 parts of Anchor Agents and 0.8 part of catalyst stir 5~10min after all adding, pressure sensitive adhesive, which is prepared, to be completed.
3) solidification of pressure sensitive adhesive
On a pet film by prepared pressure-sensitive adhesives, coating thickness is determined according to specific requirement, places into 120
Solidify 1~2min in~150 DEG C of baking ovens or is directly entered setting maximum temperature to solidify in the drying tunnel no more than 165 DEG C.
Base rubber component, prepared pressure sensitive adhesive and the pressure sensitive adhesive tape being cured are tested, performance parameter is shown in Table 1.
Embodiment 5:
1) base rubber component is prepared:
By 75 parts of contents of ethylene be 0.2% vinyldimethicone A and 25 parts of contents of ethylene be 1.8%
Vinyldimethicone B be added in reaction kettle, add 120 parts of diluents, stir, make vinyl polysiloxane
Sufficiently dissolution dispersion, adds 0.5% silazane of vinyl polysiloxane total amount, at 60~80 DEG C, the item of nitrogen protection
It is reacted 3 hours under part, then is warming up to solvent boiling, distill out the water reflected, it is cooling, 0.25 part of inhibitor is added, stirs
Uniformly, as base rubber component.
2) preparation of pressure sensitive adhesive
By 100 parts of base rubbers, 150 parts of diluents are added, stir evenly；Successively it is slowly added to 1.5 under stirring conditions again
Part crosslinking agent, 0.8 part of Anchor Agent and 1.2 parts of catalyst stir 5~10min after all adding, pressure sensitive adhesive, which is prepared, to be completed.
3) solidification of pressure sensitive adhesive
On a pet film by prepared pressure-sensitive adhesives, coating thickness is determined according to specific requirement, places into 120
Solidify 1~2min in~150 DEG C of baking ovens or is directly entered setting maximum temperature to solidify in the drying tunnel no more than 165 DEG C.
Base rubber component, prepared pressure sensitive adhesive and the pressure sensitive adhesive tape being cured are tested, performance parameter is shown in Table 1.
The performance test results of 1 embodiment 1-5 of table
Table 2 is other Specifeca tion speeifications of organic pressure-sensitive gel of the present invention
Examination criteria used by above-mentioned organic pressure-sensitive gel performance detection and detection method are as follows: method for detecting viscosity ginseng
Examine GB/T 10247-2008；Operating time detection method: start timing after proportionally mixing, until mixed colloid starts
Time needed for there is peeling or cotton-shaped colloid；Curing time detection method: by coated PET film under the conditions of fixed temperature
It is put into baking oven, is taken out after being put into a period of time, is tested using pencil hardometer (1H), until the time required for glue-line no marking is
Curing time；180 ° of peel strength detection methods refer to GB/T2792-1998, boiling method for testing performance: will be coated in PET film
Upper and completion of cure pressure sensitive adhesive tape (pressure sensitive adhesive is with a thickness of 10-20 μm) is put into the distilled water boiled, after continuously boiling 4 hours
It takes out, glue-line edge not degumming does not lose powder, as qualified.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (10)
1. a kind of organic pressure-sensitive gel, it is characterised in that: including base rubber component, catalyst component, cross-linking agent component and Anchor Agent
Component；
The preparation method of the base rubber component, comprising the following steps: by molecular weight be 50~700,000 vinyl polysiloxane and
The vinyl polysiloxane that molecular weight is 5000~20,000 is added in reaction kettle, adds diluent into reaction kettle and ethylene
Based polysiloxane sufficiently dissolves dispersion, adds 0.1~2% basic catalyst of vinyl polysiloxane total amount to reaction kettle
In, it is reacted in a kettle 2~6 hours under conditions of 60~90 DEG C and nitrogen protection, then carry out distillation water removal, in reaction kettle
0.04~0.4 part of inhibitor is added, stirs evenly；
The catalyst component is the platinum metal catalyst of 2000~7000ppm of platinum content；
The cross-linking agent component is hydrogen-based content in 1.0~1.6% hydrogen-based polysiloxanes；
The Anchor Agent component is to contain one of epoxy group, ether, acyloxy or a variety of hydrogen-based polysiloxanes.
2. organic pressure-sensitive gel according to claim 1, which is characterized in that it further include independent chuck, the independent chuck
Include in parts by weight 100 parts of base rubber component, catalyst component be 0.5~2 part, cross-linking agent component is 0.5~2 part, bonding
Agent component is 0.5~1.5 part.
3. organic pressure-sensitive gel according to claim 1, which is characterized in that the vinyl that the molecular weight is 50~700,000
The contents of ethylene of polysiloxanes is 0.15~0.6wt%；The second for the vinyl polysiloxane that the molecular weight is 5000~20,000
Amount vinyl content is 0.5~2.0wt%.
4. organic pressure-sensitive gel according to claim 1, which is characterized in that the structural formula of the vinyl polysiloxane
Are as follows:Wherein m, n are the natural number greater than 1.
5. organic pressure-sensitive gel according to claim 1, which is characterized in that the structural formula of the Anchor Agent component are as follows:Wherein R1And R2For H or alkyl；X is epoxy group, ether or acyloxy；X, y be natural number and
1≤x≤7；1≤y≤4.
6. organic pressure-sensitive gel according to claim 1, which is characterized in that the inhibitor is tetramethyl tetravinyl ring
Tetrasiloxane, divinyl tetramethyl disiloxane, allylene alcohol, ethynylcyclohexanol, methyl butynol, 3,5- diformazan
One of which or any combination in base-1- hexin base-3- alcohol, 3- methyl-1-dodecyne-3- alcohol.
7. organic pressure-sensitive gel according to claim 1, which is characterized in that the diluent is volatile solvents, institute
Stating volatile solvents is petroleum ether, toluene, dimethylbenzene, solvent naphtha or ethyl acetate.
8. organic pressure-sensitive gel according to claim 1, which is characterized in that the structural formula of the hydrogen-based polysiloxanes are as follows:Wherein R3, R4,R5,R6For H or methyl；K is the natural number more than or equal to 0；J is more than or equal to 0
And the natural number less than 2.
9. organic pressure-sensitive gel according to claim 1, which is characterized in that the basic catalyst is ammonium hydroxide, tetramethyl
The one or more of ammonium hydroxide, hexamethyldisilazane etc..
10. the preparation method of -9 any organic pressure-sensitive gels according to claim 1, which is characterized in that including following step
It is rapid:
1) base rubber component is prepared: the vinyl polysiloxane and 20~40 parts of molecular weight for being 50~700,000 by 60~80 parts of molecular weight
Vinyl polysiloxane for 5000~20,000 is added in reaction kettle, adds 60~120 parts of diluents, and stirring makes vinyl
Polysiloxanes sufficiently dissolves dispersion, and 0.1~2% basic catalyst of vinyl polysiloxane total amount is added, at 60~80 DEG C,
It being reacted 2~6 hours under conditions of nitrogen protection, then is warming up to solvent boiling, distill out the water reflected, reaction kettle is cooling,
0.04~0.4 part of inhibitor is added in reaction kettle, stirs evenly, as base rubber component；
2) preparation of pressure sensitive adhesive: by 100 parts of base rubber components, 50~150 parts of diluents is added, stir evenly；It is successively stirring again
Under conditions of be slowly added to 0.5~2 part of cross-linking agent component, 0.5~1.5 part of Anchor Agent component and 0.5~2 part of catalyst component,
5~10min is stirred after all adding, pressure sensitive adhesive, which is prepared, to be completed；
3) solidification of pressure sensitive adhesive: by prepared pressure-sensitive adhesives, on a pet film, coating thickness is true according to specific requirement
It is fixed, it places into and solidifies 1~2min in 120~150 DEG C of baking ovens or be directly entered setting maximum temperature as the drying tunnel no more than 165 DEG C
Middle solidification.
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| CN109294492A (en) * | 2018-09-29 | 2019-02-01 | 上海英诺威新材料科技有限公司 | A kind of ultra micro glues peeling force acrylate pressure sensitive adhesive and preparation method thereof |
| CN110684504A (en) * | 2019-10-31 | 2020-01-14 | 广东莱尔新材料科技股份有限公司 | High-temperature-resistant binder and high-temperature-resistant adhesive film for cables |
| CN113025265A (en) * | 2020-12-08 | 2021-06-25 | 江苏科琪高分子材料研究院有限公司 | Preparation method of solvent type organic silicon glue for manufacturing optical transparent adhesive film |
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| CN114196374A (en) * | 2022-01-13 | 2022-03-18 | 万华化学集团股份有限公司 | high-AF (AF) screen adhesion force organic silicon pressure-sensitive adhesive suitable for general curing of TPU (thermoplastic polyurethane) film, preparation method and application thereof |
| CN114958290A (en) * | 2022-05-13 | 2022-08-30 | 成都拓利科技股份有限公司 | Organic silicon pressure-sensitive adhesive and preparation method and application thereof |
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| CN113025265A (en) * | 2020-12-08 | 2021-06-25 | 江苏科琪高分子材料研究院有限公司 | Preparation method of solvent type organic silicon glue for manufacturing optical transparent adhesive film |
| CN114058290A (en) * | 2021-11-18 | 2022-02-18 | 四川富彩科技有限公司 | Solvent-free organic silicon release agent with ultralow release force and preparation method thereof |
| CN114058290B (en) * | 2021-11-18 | 2023-08-08 | 成都富彩新材料有限公司 | Solvent-free organosilicon release agent with ultralow release force and preparation method thereof |
| CN114196374A (en) * | 2022-01-13 | 2022-03-18 | 万华化学集团股份有限公司 | high-AF (AF) screen adhesion force organic silicon pressure-sensitive adhesive suitable for general curing of TPU (thermoplastic polyurethane) film, preparation method and application thereof |
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| CN114958290A (en) * | 2022-05-13 | 2022-08-30 | 成都拓利科技股份有限公司 | Organic silicon pressure-sensitive adhesive and preparation method and application thereof |
| CN115011305A (en) * | 2022-05-25 | 2022-09-06 | 江苏斯迪克新材料科技股份有限公司 | Organic silicon pressure-sensitive adhesive and preparation method thereof |
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