CN110540819A - Preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive - Google Patents
Preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
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- 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
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- 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]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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- 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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- C09J2433/00—Presence of (meth)acrylic polymer
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- C09J2479/00—Presence of polyamine or polyimide
- C09J2479/08—Presence of polyamine or polyimide polyimide
- C09J2479/086—Presence of polyamine or polyimide polyimide in the substrate
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Abstract
the invention discloses a preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive, which comprises the following steps: (1) weighing the material raw materials; (2) preparing a mixed solution A; (3) surface treatment of nano titanium nitride; (4) preparing modified particles B; (5) preparing glue solution C; (6) and (5) preparing a finished product. The invention provides a preparation method of acrylate pressure-sensitive adhesive, which has simple integral process and easy popularization and application, and the prepared acrylate pressure-sensitive adhesive has good strength, strong bonding force, high temperature resistance, ageing resistance and long service life.
Description
Technical Field
The invention belongs to the technical field of pressure-sensitive adhesive processing, and particularly relates to a preparation method of a high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive.
background
with the gradual development of economy and scientific technology, the demand of pressure-sensitive adhesives (PSA) for industry, agriculture, transportation, medical treatment, national defense and daily life of people is increasing, and the requirement is higher and higher. The national fifteen program also clearly proposes to research high-performance and high-quality pressure-sensitive adhesive and products. In view of the practical application of the pressure-sensitive adhesive at present, it is difficult to obtain a good effect by using only one type of resin for preparing the pressure-sensitive adhesive with high strength and good heat resistance, and modification is necessary. The polyacrylate pressure-sensitive adhesive is widely applied due to the advantages of excellent adhesive property and chemical stability, no toxicity, no harm, low cost and the like. However, the polyacrylate pressure-sensitive adhesive has general heat resistance, the maximum service temperature of the crosslinked acrylate pressure-sensitive adhesive is only used at 150 ℃ for a short time, and the crosslinked acrylate pressure-sensitive adhesive has poor thermo-oxidative aging performance and is easy to lose pressure sensitivity at higher temperature, so that the application of the acrylate pressure-sensitive adhesive is greatly limited. The organic silicon pressure-sensitive adhesive not only has the characteristics of common pressure-sensitive adhesives, but also has the advantages of wider application temperature range (-70-250 ℃), excellent chemical inertness and the like, but the peeling strength of the organic silicon pressure-sensitive adhesive is low, and the adhesive requirements of high peeling strength are difficult to meet. Therefore, the organic silicon is adopted to chemically modify the polyacrylate pressure-sensitive adhesive, and the organic silicon pressure-sensitive adhesive has the advantages of high temperature resistance of the organic silicon pressure-sensitive adhesive, high stripping performance of the polyacrylate pressure-sensitive adhesive and the like, so that a certain stripping strength can be ensured, the high temperature resistance and the medium resistance of the polyacrylate pressure-sensitive adhesive can be improved, and the organic silicon pressure-sensitive adhesive has practical application value.
japanese patent laid-open No. 60-197780 reports that 100 parts by weight of acrylate pressure-sensitive adhesive and 1-30 parts by weight of organosilicon pressure-sensitive adhesive are blended in organic solvent to obtain organosilicon modified acrylate pressure-sensitive adhesive, and the blending modification of the method is easy to generate phase separation because no bonding exists between acrylate and organosilicon, and the stability of the product is poor.
The application numbers are: 200510060865.8 discloses a pressure-sensitive adhesive of polyacrylate modified by organosilicon monomer, which is prepared by polymerizing monomer mixture such as acrylate by stepwise dripping under the condition of solution polymerization to prepare prepolymer, and adjusting the molecular weight and distribution of the product by adjusting solvent; by adding a cross-linking agent, excellent properties can be obtained.
the application numbers are: 02134207.5 discloses a method for preparing organosilicon modified polyacrylate high temperature resistant, insulating pressure sensitive adhesive and adhesive tape, which comprises synthesizing a graft interpenetrating polymer network pressure sensitive adhesive prepolymer by solution polymerization, and then obtaining organosilicon modified polyacrylate pressure sensitive adhesive by post-treatment. And the polyacrylate pressure-sensitive adhesive is modified by adopting the organic silicon monomer, the peel strength of 180 degrees at room temperature is lower, generally 4N/25 mm-6N/25 mm, the polyacrylate pressure-sensitive adhesive can be only used for a short time or instantly at the high temperature of 200 ℃, and the temperature resistance is poor.
the application numbers are: chinese patent CN201010521734.6 reports a preparation method of high-strength heat-resistant silicone resin modified acrylate pressure-sensitive adhesive, in which hard monomers and soft monomers are used in combination with application of MQ silicone resin, etc., so that the pressure-sensitive adhesive can be used in high temperature field within 200 ℃, the peel strength at 180 ° at room temperature reaches 15N/25 mm-18N/25 mm, although the adhesive has good use effect, the qualities of holding power, aging resistance, etc. still need to be improved.
Disclosure of Invention
the invention aims to provide a preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive aiming at the existing problems.
the invention is realized by the following technical scheme:
a preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive comprises the following steps:
(1) weighing the following substances in parts by weight: 50-55 parts of butyl acrylate, 30-35 parts of isooctyl acrylate, 20-25 parts of methyl methacrylate, 1.5-2.5 parts of dibenzoyl peroxide, 8-10 parts of MQ silicon resin, 80-90 parts of ethyl acetate, 10-15 parts of xylene, 3-6 parts of isocyanate and 1-3 parts of hexamethylene diamine;
(2) Putting the purified hexafluorobutyl acrylate and a silane coupling agent into a reaction kettle together, introducing argon while stirring and mixing, dropwise adding azodiisobutyronitrile, performing reflux treatment for 4-6 hours, and taking out to obtain a mixed solution A for later use;
(3) Putting the nano titanium nitride into a hydrochloric acid solution for soaking for 10-12 min, then filtering out, washing with deionized water once, and finally drying for 1-2 h and taking out for later use;
(4) Adjusting the pH value of the mixed solution A prepared in the step (2) to 5-6, then putting the nano titanium nitride treated in the step (3) into the mixed solution A, then carrying out heating magnetic stirring treatment for 6-7 h, discharging, then carrying out extraction treatment for 20-24 h, then putting into a vacuum drier for drying treatment for 3-5 h, taking out, then putting into an irradiation box for microwave irradiation treatment, and taking out after 2-3 min to obtain modified particles B for later use;
(5) putting all the substances weighed in the step (1) into a reaction kettle together, adding the modified particles B prepared in the step (4) into the reaction kettle, heating and stirring the reaction kettle, controlling the temperature in the reaction kettle to be 85-90 ℃ during the heating and stirring, stirring for 6-8 hours, and taking out the mixture to obtain glue solution C for later use;
(6) And (3) uniformly coating the glue solution C prepared in the step (5) on a polyimide film substrate, then drying for 2-4 h at the temperature of 80-90 ℃, and taking out to obtain a finished product.
Further, the MQ silicon resin in the step (1) is methyl vinyl MQ silicon resin or methyl phenyl MQ silicon resin.
further, the silane coupling agent in the step (2) is any one of a silane coupling agent kh550, a silane coupling agent kh560 and a silane coupling agent kh 570; the weight ratio of the hexafluorobutyl acrylate to the silane coupling agent is 2.5-3: 1; the addition amount of the azodiisobutyronitrile is 2-4% of the total mass of the hexafluorobutyl acrylate and the silane coupling agent.
further, the mass fraction of the hydrochloric acid solution in the step (3) is 1-1.5%; and the temperature for controlling drying during drying treatment is 100-110 ℃.
Further, the input amount of the nano titanium nitride in the step (4) is 5-7% of the total mass of the mixed solution A; the heating temperature is controlled to be 70-75 ℃ during the heating magnetic stirring treatment; the extraction solvent used in the extraction treatment is tetrahydrofuran; the temperature in the vacuum drier is controlled to be 65-70 ℃ during the drying treatment; and during microwave irradiation treatment, the frequency in the irradiation box is controlled to be 2-2.2 GHz, and the power is controlled to be 2000-2200W.
Further, the adding amount of the modified particles B in the step (5) to the reaction kettle is 4-6% of the total mass of all the substances weighed in the step (1); and during stirring treatment, the rotating speed of stirring is controlled to be 200-220 r/min.
The invention carries out special improvement treatment on the preparation method of the acrylate pressure-sensitive adhesive, wherein MQ silicon resin is still selected to compound the acrylate pressure-sensitive adhesive for reinforcement treatment, in order to further improve the overall quality, the invention also specially prepares a modified particle B on the raw material component, the modified particle B is a modified nano titanium nitride component, in the prior art, an inorganic filler is added to carry out the treatment method for reinforcing the pressure-sensitive adhesive, but the dispersion is not uniform, the bonding capability is not strong and the structure performance is unstable due to the self characteristics of the inorganic filler, although the surface modification treatment by utilizing a silane coupling agent and the like can improve the filling performance, the invention still has larger improvement space. Modified particle B that this application prepared is one kind and has good surface properties, the granule composition that can abundant homodisperse and combine in pressure sensitive adhesive base body, under the effect of hexafluorobutyl acrylate, silane coupling agent etc., a large amount of fluorine-containing molecular chains and coupling group have combined on the surface of nanometer titanium nitride granule, later microwave treatment has carried out again, under the effect of microwave, the fracture takes place for partial fluorine-containing polymer chain on nanometer titanium nitride granule surface, the branching degree has been improved, can further strengthen its and acrylate etc. composition binding strength, compactness and stability between, thereby fine improvement holistic intensity, high temperature resistant, ageing resistance, quality such as bonding strength.
compared with the prior art, the invention has the following advantages:
the invention provides a preparation method of acrylate pressure-sensitive adhesive, which has simple integral process and easy popularization and application, and the prepared acrylate pressure-sensitive adhesive has good strength, strong bonding force, high temperature resistance and ageing resistance, long service life, and good economic benefit and market competitiveness.
Detailed Description
Example 1
A preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive comprises the following steps:
(1) weighing the following substances in parts by weight: 50 parts of butyl acrylate, 30 parts of isooctyl acrylate, 20 parts of methyl methacrylate, 1.5 parts of dibenzoyl peroxide, 8 parts of MQ silicon resin, 80 parts of ethyl acetate, 10 parts of dimethylbenzene, 3 parts of isocyanate and 1 part of hexamethylenediamine;
(2) Putting the purified hexafluorobutyl acrylate and a silane coupling agent into a reaction kettle together, introducing argon while stirring and mixing, dropwise adding azodiisobutyronitrile, performing reflux treatment for 4 hours, and taking out to obtain a mixed solution A for later use;
(3) putting the nano titanium nitride into a hydrochloric acid solution for soaking for 10min, then filtering out and washing with deionized water, and finally drying for 1h and taking out for later use;
(4) Adjusting the pH value of the mixed solution A prepared in the step (2) to 5, then putting the nano titanium nitride treated in the step (3) into the mixed solution A, then carrying out heating magnetic stirring treatment for 6h, carrying out extraction treatment for 20h after discharging, then putting into a vacuum drier for drying treatment for 3h, taking out, then putting into an irradiation box for microwave irradiation treatment, and taking out after 2min to obtain modified particles B for later use;
(5) Putting all the substances weighed in the step (1) into a reaction kettle together, adding the modified particles B prepared in the step (4) into the reaction kettle, heating and stirring the reaction kettle, controlling the temperature in the reaction kettle to be 85 ℃ during the heating and stirring, stirring for 6 hours, and taking out the mixture to obtain glue solution C for later use;
(6) And (3) uniformly coating the glue solution C prepared in the step (5) on a polyimide film substrate, then placing the polyimide film substrate at the temperature of 80 ℃ for drying treatment for 2h, and taking out the polyimide film substrate after the drying treatment to obtain a finished product.
Further, the MQ silicone resin in the step (1) is methyl vinyl MQ silicone resin.
Further, the silane coupling agent in the step (2) is a silane coupling agent kh 550; the weight ratio of the hexafluorobutyl acrylate and the silane coupling agent is 2.5: 1; the addition amount of the azodiisobutyronitrile is 2 percent of the total mass of the hexafluorobutyl acrylate and the silane coupling agent.
further, the mass fraction of the hydrochloric acid solution in the step (3) is 1%; the temperature for drying is controlled to be 100 ℃ during the drying treatment.
further, the input amount of the nano titanium nitride in the step (4) is 5% of the total mass of the mixed solution A; the heating temperature is controlled to be 70 ℃ during the heating magnetic stirring treatment; the extraction solvent used in the extraction treatment is tetrahydrofuran; the temperature in the vacuum drier is controlled to be 65 ℃ during the drying treatment; and during microwave irradiation treatment, the frequency in the irradiation box is controlled to be 2GHz and the power is controlled to be 2000W.
Further, the adding amount of the modified particles B in the step (5) to the reaction kettle is 4% of the total mass of all the substances weighed in the step (1); the rotating speed of stirring is controlled to be 200 r/min during the stirring treatment.
example 2
a preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive comprises the following steps:
(1) weighing the following substances in parts by weight: 53 parts of butyl acrylate, 32 parts of isooctyl acrylate, 22 parts of methyl methacrylate, 2 parts of dibenzoyl peroxide, 9 parts of MQ silicon resin, 85 parts of ethyl acetate, 13 parts of xylene, 5 parts of isocyanate and 2 parts of hexamethylene diamine;
(2) putting the purified hexafluorobutyl acrylate and a silane coupling agent into a reaction kettle together, introducing argon while stirring and mixing, dropwise adding azodiisobutyronitrile, performing reflux treatment for 5 hours, and taking out to obtain a mixed solution A for later use;
(3) putting the nano titanium nitride into a hydrochloric acid solution for soaking for 11min, then filtering out and washing with deionized water, and finally drying for 1.6h and taking out for later use;
(4) Adjusting the pH value of the mixed solution A prepared in the step (2) to 5.5, then putting the nano titanium nitride treated in the step (3) into the mixed solution A, then carrying out heating magnetic stirring treatment for 6.5h, discharging, then carrying out extraction treatment for 22h, then putting into a vacuum drier for drying treatment for 4h, taking out, then putting into an irradiation box for microwave irradiation treatment, and taking out after 2.5min to obtain modified particles B for later use;
(5) Putting all the substances weighed in the step (1) into a reaction kettle together, adding the modified particles B prepared in the step (4) into the reaction kettle, heating and stirring the reaction kettle, controlling the temperature in the reaction kettle to be 88 ℃ during the heating and stirring, and taking out the mixture after stirring for 7 hours to obtain glue solution C for later use;
(6) and (3) uniformly coating the glue solution C prepared in the step (5) on a polyimide film substrate, then putting the polyimide film substrate into the condition of 85 ℃ for drying treatment for 3h, and taking out the polyimide film substrate after the drying treatment to obtain a finished product.
further, the MQ silicone resin in the step (1) is methyl vinyl MQ silicone resin.
Further, the silane coupling agent in the step (2) is a silane coupling agent kh 560; the weight ratio of the hexafluorobutyl acrylate and the silane coupling agent is 2.8: 1; the addition amount of the azodiisobutyronitrile is 3 percent of the total mass of the hexafluorobutyl acrylate and the silane coupling agent.
Further, the mass fraction of the hydrochloric acid solution in the step (3) is 1.3%; the drying temperature is controlled to be 105 ℃ during the drying treatment.
Further, the input amount of the nano titanium nitride in the step (4) is 6% of the total mass of the mixed solution A; the heating temperature is controlled to be 72 ℃ during the heating magnetic stirring treatment; the extraction solvent used in the extraction treatment is tetrahydrofuran; the temperature in the vacuum drier is controlled to be 68 ℃ during the drying treatment; and during microwave irradiation treatment, the frequency in the irradiation box is controlled to be 2.1GHz and the power is controlled to be 2100W.
Further, the adding amount of the modified particles B in the step (5) to the reaction kettle is 5% of the total mass of all the substances weighed in the step (1); the rotating speed of stirring is controlled to be 210 r/min during the stirring treatment.
example 3
a preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive comprises the following steps:
(1) Weighing the following substances in parts by weight: 55 parts of butyl acrylate, 35 parts of isooctyl acrylate, 25 parts of methyl methacrylate, 2.5 parts of dibenzoyl peroxide, 10 parts of MQ silicon resin, 90 parts of ethyl acetate, 15 parts of dimethylbenzene, 6 parts of isocyanate and 3 parts of hexamethylene diamine;
(2) putting the purified hexafluorobutyl acrylate and a silane coupling agent into a reaction kettle together, introducing argon while stirring and mixing, dropwise adding azodiisobutyronitrile, performing reflux treatment for 6 hours, and taking out to obtain a mixed solution A for later use;
(3) Putting the nano titanium nitride into a hydrochloric acid solution for soaking for 12min, then filtering out and washing with deionized water once, and finally drying for 2h and taking out for later use;
(4) adjusting the pH value of the mixed solution A prepared in the step (2) to 6, then putting the nano titanium nitride treated in the step (3) into the mixed solution A, then carrying out heating magnetic stirring treatment for 7 hours, carrying out extraction treatment for 24 hours after discharging, then putting into a vacuum drier for drying treatment for 5 hours, taking out, then putting into an irradiation box for microwave irradiation treatment, and taking out after 3min to obtain modified particles B for later use;
(5) putting all the substances weighed in the step (1) into a reaction kettle together, adding the modified particles B prepared in the step (4) into the reaction kettle, heating and stirring the reaction kettle, wherein the temperature in the reaction kettle is controlled to be 90 ℃, and taking out the modified particles B after stirring for 8 hours to obtain glue solution C for later use;
(6) And (3) uniformly coating the glue solution C prepared in the step (5) on a polyimide film substrate, then putting the polyimide film substrate into a condition of 90 ℃ for drying treatment for 4h, and taking out the polyimide film substrate after the drying treatment to obtain a finished product.
further, the MQ silicon resin in the step (1) is methyl phenyl MQ silicon resin.
further, the silane coupling agent in the step (2) is a silane coupling agent kh 570; the weight ratio of the hexafluorobutyl acrylate to the silane coupling agent is 3: 1; the addition amount of the azodiisobutyronitrile is 4 percent of the total mass of the hexafluorobutyl acrylate and the silane coupling agent.
further, the mass fraction of the hydrochloric acid solution in the step (3) is 1.5%; the drying temperature is controlled to be 110 ℃ during the drying treatment.
Further, the input amount of the nano titanium nitride in the step (4) is 7% of the total mass of the mixed solution A; the heating temperature is controlled to be 75 ℃ during the heating magnetic stirring treatment; the extraction solvent used in the extraction treatment is tetrahydrofuran; the temperature in the vacuum drier is controlled to be 70 ℃ during the drying treatment; and during the microwave irradiation treatment, the frequency in the irradiation box is controlled to be 2.2GHz and the power is 2200W.
Further, the adding amount of the modified particles B in the step (5) to the reaction kettle is 6% of the total mass of all the substances weighed in the step (1); the rotating speed of stirring is controlled to be 220 r/min during the stirring treatment.
Comparative Experimental example 1
A preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive comprises the following steps:
(1) Weighing the following substances in parts by weight: 53 parts of butyl acrylate, 32 parts of isooctyl acrylate, 22 parts of methyl methacrylate, 2 parts of dibenzoyl peroxide, 9 parts of MQ silicon resin, 85 parts of ethyl acetate, 13 parts of xylene, 5 parts of isocyanate and 2 parts of hexamethylene diamine;
(2) putting the purified hexafluorobutyl acrylate and a silane coupling agent into a reaction kettle together, introducing argon while stirring and mixing, dropwise adding azodiisobutyronitrile, performing reflux treatment for 5 hours, and taking out to obtain a mixed solution A for later use;
(3) Putting the nano titanium nitride into a hydrochloric acid solution for soaking for 11min, then filtering out and washing with deionized water, and finally drying for 1.6h and taking out for later use;
(4) Adjusting the pH value of the mixed solution A prepared in the step (2) to 5.5, then putting the nano titanium nitride treated in the step (3) into the mixed solution A, then carrying out heating magnetic stirring treatment for 6.5h, discharging, then carrying out extraction treatment for 22h, then putting into a vacuum drier for drying treatment for 4h, and taking out after 2.5min to obtain modified particles B for later use;
(5) Putting all the substances weighed in the step (1) into a reaction kettle together, adding the modified particles B prepared in the step (4) into the reaction kettle, heating and stirring the reaction kettle, controlling the temperature in the reaction kettle to be 88 ℃ during the heating and stirring, and taking out the mixture after stirring for 7 hours to obtain glue solution C for later use;
(6) and (3) uniformly coating the glue solution C prepared in the step (5) on a polyimide film substrate, then putting the polyimide film substrate into the condition of 85 ℃ for drying treatment for 3h, and taking out the polyimide film substrate after the drying treatment to obtain a finished product.
In this comparative example 1, the microwave irradiation treatment in the step (4) was omitted as compared with example 2, except that the steps of the method were the same.
Comparative experiment example 2
A preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive comprises the following steps:
(1) Weighing the following substances in parts by weight: 53 parts of butyl acrylate, 32 parts of isooctyl acrylate, 22 parts of methyl methacrylate, 2 parts of dibenzoyl peroxide, 9 parts of MQ silicon resin, 85 parts of ethyl acetate, 13 parts of xylene, 5 parts of isocyanate and 2 parts of hexamethylene diamine;
(2) Putting all the substances weighed in the step (1) into a reaction kettle together, adding the nano titanium nitride into the reaction kettle, heating and stirring the reaction kettle, controlling the temperature in the reaction kettle to be 88 ℃ during the heating and stirring, stirring for 7 hours, and taking out the mixture to obtain a glue solution C for later use;
(3) And (3) uniformly coating the glue solution C prepared in the step (2) on a polyimide film substrate, then putting the polyimide film substrate into the condition of 85 ℃ for drying treatment for 3 hours, and taking out the polyimide film substrate after the drying treatment to obtain a finished product.
In comparative example 2, the modified particle B component obtained in the previous step (4) was replaced with an equal mass portion of nano titanium nitride, as compared with example 2, except that the other steps were the same.
control group
The application numbers are: the CN201010521734.6 chinese patent reports a preparation method of a high-strength heat-resistant silicone resin modified acrylate pressure-sensitive adhesive, specifically selecting a technical scheme with a fourteenth specific implementation mode.
in order to compare the effects of the invention, the performance of the pressure-sensitive adhesive prepared by the embodiment 2, the comparative experiment example 1, the comparative experiment example 2 and the control group is tested, 10 samples are set in each group, the experiment is repeated for 3 times, and finally the data are summarized and averaged correspondingly, wherein the specific comparative data are shown in the following table 1:
TABLE 1
Note: the permanent adhesion test described in the above table 1 is performed by selecting a temperature type tape retention tester (MIDEL KJ-6012, measuring instruments, Inc. of department of Dongguan), and performing a test according to GB/T4851-1998, and calculating the permanent adhesion by the time when the tape falls off due to shear failure; the pressure-sensitive adhesive is placed at the temperature of 150 ℃ for 2h at the temperature of 150 ℃/2h, and the state of the pressure-sensitive adhesive is observed; the 180-degree peel strength test is carried out by selecting a computer type tensile testing machine (MIDEL KJ-1065A, detection instrument Co. Ltd. of Dongguan city) according to GB/T2792-1998, wherein the corresponding room temperature is carried out at room temperature, and the corresponding 200 ℃ and aging treatment for 25h are carried out after the pressure-sensitive adhesive is aged at 200 ℃ for 25 h.
As can be seen from the above table 1, the comprehensive performance of the pressure-sensitive adhesive prepared by the invention is obviously improved, the temperature resistance and the bonding capability are obviously enhanced, and the pressure-sensitive adhesive has good use value and economic benefit.
Claims (6)
1. A preparation method of high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive is characterized by comprising the following steps:
(1) Weighing the following substances in parts by weight: 50-55 parts of butyl acrylate, 30-35 parts of isooctyl acrylate, 20-25 parts of methyl methacrylate, 1.5-2.5 parts of dibenzoyl peroxide, 8-10 parts of MQ silicon resin, 80-90 parts of ethyl acetate, 10-15 parts of xylene, 3-6 parts of isocyanate and 1-3 parts of hexamethylene diamine;
(2) Putting the purified hexafluorobutyl acrylate and a silane coupling agent into a reaction kettle together, introducing argon while stirring and mixing, dropwise adding azodiisobutyronitrile, performing reflux treatment for 4-6 hours, and taking out to obtain a mixed solution A for later use;
(3) Putting the nano titanium nitride into a hydrochloric acid solution for soaking for 10-12 min, then filtering out, washing with deionized water once, and finally drying for 1-2 h and taking out for later use;
(4) Adjusting the pH value of the mixed solution A prepared in the step (2) to 5-6, then putting the nano titanium nitride treated in the step (3) into the mixed solution A, then carrying out heating magnetic stirring treatment for 6-7 h, discharging, then carrying out extraction treatment for 20-24 h, then putting into a vacuum drier for drying treatment for 3-5 h, taking out, then putting into an irradiation box for microwave irradiation treatment, and taking out after 2-3 min to obtain modified particles B for later use;
(5) Putting all the substances weighed in the step (1) into a reaction kettle together, adding the modified particles B prepared in the step (4) into the reaction kettle, heating and stirring the reaction kettle, controlling the temperature in the reaction kettle to be 85-90 ℃ during the heating and stirring, stirring for 6-8 hours, and taking out the mixture to obtain glue solution C for later use;
(6) And (3) uniformly coating the glue solution C prepared in the step (5) on a polyimide film substrate, then drying for 2-4 h at the temperature of 80-90 ℃, and taking out to obtain a finished product.
2. the method for preparing a high temperature resistant, high strength acrylate pressure sensitive adhesive according to claim 1, wherein the MQ silicone resin in step (1) is methyl vinyl MQ silicone resin or methyl phenyl MQ silicone resin.
3. the method for preparing the high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive according to claim 1, wherein the silane coupling agent in the step (2) is any one of a silane coupling agent kh550, a silane coupling agent kh560 and a silane coupling agent kh 570; the weight ratio of the hexafluorobutyl acrylate to the silane coupling agent is 2.5-3: 1; the addition amount of the azodiisobutyronitrile is 2-4% of the total mass of the hexafluorobutyl acrylate and the silane coupling agent.
4. The preparation method of the high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive according to claim 1, wherein the mass fraction of the hydrochloric acid solution in the step (3) is 1-1.5%; and the temperature for controlling drying during drying treatment is 100-110 ℃.
5. the preparation method of the high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive according to claim 1, wherein the input amount of the nano titanium nitride in the step (4) is 5-7% of the total mass of the mixed solution A; the heating temperature is controlled to be 70-75 ℃ during the heating magnetic stirring treatment; the extraction solvent used in the extraction treatment is tetrahydrofuran; the temperature in the vacuum drier is controlled to be 65-70 ℃ during the drying treatment; and during microwave irradiation treatment, the frequency in the irradiation box is controlled to be 2-2.2 GHz, and the power is controlled to be 2000-2200W.
6. The preparation method of the high-temperature-resistant and high-strength acrylate pressure-sensitive adhesive according to claim 1, wherein the addition amount of the modified particles B in the step (5) to the reaction kettle is 4-6% of the total mass of all substances weighed in the step (1); and during stirring treatment, the rotating speed of stirring is controlled to be 200-220 r/min.
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