CN112812733A - Low-modulus high-elongation transparent pouring sealant composition and preparation method thereof - Google Patents

Low-modulus high-elongation transparent pouring sealant composition and preparation method thereof Download PDF

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CN112812733A
CN112812733A CN202011617176.3A CN202011617176A CN112812733A CN 112812733 A CN112812733 A CN 112812733A CN 202011617176 A CN202011617176 A CN 202011617176A CN 112812733 A CN112812733 A CN 112812733A
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parts
pouring sealant
mixture
linking agent
self
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CN112812733B (en
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黄文哲
刘光华
黄琪
陈永隆
陈建军
黄恒超
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Guangzhou Baiyun Technology Co ltd
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Guangzhou Baiyun Chemical Industry Co Ltd
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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
    • 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
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/10—Transparent films; Clear coatings; Transparent materials
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • 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
    • 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
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sealing Material Composition (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to the field of pouring sealant, in particular to a transparent pouring sealant composition with low modulus and high elongation and a preparation method thereof. According to the preparation method, 90-110 parts by mass of micromolecule hydroxyl silicone oil is used for modifying 5-40 parts by mass of common dealcoholization type cross-linking agent to prepare the cross-linking agent, and the self-prepared cross-linking agent is used for preparing the condensed type transparent pouring sealant composition, so that the curing speed and the deep curing speed of the pouring sealant composition can be greatly improved, the breaking elongation of the pouring sealant colloid is improved, the modulus of the colloid is reduced, the hardness is controlled in a reasonable range, and the transparency of the colloid is not influenced.

Description

Low-modulus high-elongation transparent pouring sealant composition and preparation method thereof
Technical Field
The invention relates to the field of pouring sealant, in particular to a transparent pouring sealant composition with low modulus and high elongation and a preparation method thereof.
Background
The pouring sealant is widely applied to the fields of lamps, electronic communication, wearable equipment and the like, has the functions of shock absorption, water prevention, moisture prevention, dust prevention and the like, and therefore the pouring sealant is generally required to have better waterproof and ageing-resistant performances, needs lower viscosity at the same time, is convenient for filling and sealing fine slits, has higher elongation at break, has stronger displacement resistance and needs lower modulus, so that the pouring sealant can meet higher anti-seismic requirements and can not cause damage to components due to overlarge displacement; of course, it is one of the requirements for the potting adhesive to have better adhesive property. In addition, with the improvement of living standard, besides the functional requirements, the requirements of aesthetic appearance are also rising day by day, so that certain requirements are also provided for the light transmittance and transparency of the pouring sealant.
However, the current pouring sealant cannot meet the above requirements, and the pouring sealant with better transparency usually sacrifices physical properties to a certain extent, and has too high hardness and too high viscosity. Low elongation and high modulus, and cannot achieve the effects of damping and protecting electronic components.
Disclosure of Invention
Therefore, a pouring sealant composition with low modulus, high elongation and high transparency and a preparation method thereof are needed.
In one aspect of the invention, a transparent pouring sealant composition is provided, which comprises a base polymer, a self-made cross-linking agent and a first catalyst;
the base polymer is alkoxy-terminated alpha, omega-dihydroxy polydimethylsiloxane, the self-made cross-linking agent is prepared by modifying a dealcoholization cross-linking agent by first micromolecule hydroxyl silicone oil, and the dealcoholization cross-linking agent accounts for 5-40 parts by mass, and the first micromolecule hydroxyl silicone oil accounts for 90-110 parts by mass.
In one embodiment, the amount of the base polymer is 90-110 parts by mass, and the amount of the self-made crosslinking agent is 10-60 parts by mass.
In one embodiment, the viscosity of the base polymer is from 1000 to 100000 mPa-s at 25 ± 0.5 ℃ and the viscosity of the first small molecule hydroxy silicone oil is from 5 to 60 mPa-s at 25 ± 0.5 ℃.
In one embodiment, the dealcoholization type cross-linking agent is at least one of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane;
the first catalyst is at least one of dibutyltin dilaurate, dibutyltin diacetate, diisopropoxy bis (ethyl acetoacetate) titanium, di-tert-butoxy-bis (ethyl acetoacetate) titanium, 1, 3-propyldioxy-bis (ethyl acetoacetate) titanium, 1, 2-propyldioxy-bis (ethyl acetoacetate) titanium and dialkoxy bis (acetylacetone) titanium, and the amount of the first catalyst is 0.1-5 parts by mass.
In one embodiment, the paint further comprises 5-80 parts by mass of a toughening polymer, and the toughening polymer comprises the following raw material components:
Figure BDA0002872666250000021
the tri-functionality alkoxy silane is at least one of trimethoxy silane, methyl triethoxy silane, vinyl trimethoxy silane, vinyl triethoxy silane, ethyl trimethoxy silane and ethyl triethoxy silane; the viscosity of the second micromolecular hydroxyl silicone oil is 10mPa & s-60 mPa & s at 25 +/-0.5 ℃; the second catalyst is organic amine and/or organic phosphine.
In one embodiment, the silicone rubber further comprises 10-100 parts by mass of modified MQ silicone resin, and the modified MQ silicone resin comprises the following raw material components:
80-160 parts of MQ silicon resin;
50-160 parts of a toughening polymer; and
80-160 parts of an organic solvent;
the MQ value of the MQ silicon resin is 0.6-1, and the MQ silicon resin is selected from methyl MQ silicon resin, phenyl MQ silicon resin and vinyl MQ silicon resin; the toughening polymer is defined by the toughening polymer prepared in the previous example.
In one embodiment, the paint further comprises 1-10 parts by mass of a coupling agent, wherein the coupling agent is at least one of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane and gamma-aminoethylaminopropyltriethoxysilane.
According to the preparation method, 90-110 parts by mass of micromolecule hydroxyl silicone oil is used for modifying 5-40 parts by mass of common dealcoholization type cross-linking agent to prepare the cross-linking agent, and the self-prepared cross-linking agent is used for preparing the condensed type transparent pouring sealant composition, so that the curing speed and the deep curing speed of the pouring sealant composition can be greatly improved, the breaking elongation of the pouring sealant colloid is improved, the modulus of the colloid is reduced, the hardness is controlled in a reasonable range, and the transparency of the colloid is not influenced.
In another aspect of the present invention, a method for preparing the transparent potting adhesive composition is provided, which comprises the following steps:
under the protection of dry nitrogen or argon, the first catalyst and the self-made crosslinking agent are uniformly mixed in advance, and then the first catalyst and the rest components are uniformly stirred and mixed under the condition of vacuumizing.
The invention also provides another preparation method of the transparent pouring sealant composition, which comprises the following steps:
dividing the self-made cross-linking agent into two parts, and uniformly mixing the coupling agent and one part of the self-made cross-linking agent under the protection of dry nitrogen or argon to obtain a first mixture;
uniformly mixing the first catalyst and another part of self-made cross-linking agent under the protection of dry nitrogen or argon to obtain a second mixture;
under the protection of dry nitrogen or argon, uniformly stirring and mixing the first mixture and the other components except the first mixture and the second mixture under the condition of vacuumizing to obtain a third mixture;
and under the protection of dry nitrogen or argon, stirring and uniformly mixing the third mixture and the second mixture under the condition of vacuumizing.
The invention also provides an electronic component which comprises the cured transparent pouring sealant composition.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the accompanying examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise. In the description of the present invention, "a plurality" means at least one, e.g., one, two, etc., unless specifically limited otherwise.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In one aspect of the invention, a transparent pouring sealant composition is provided, which comprises a base polymer, a self-made cross-linking agent and a first catalyst;
the base polymer is alkoxy-terminated alpha, omega-dihydroxy polydimethylsiloxane, the self-made cross-linking agent is prepared by modifying a dealcoholization cross-linking agent by first micromolecule hydroxyl silicone oil, and the using amount of the dealcoholization cross-linking agent is 5-40 parts by mass, the using amount of the first micromolecule hydroxyl silicone oil is 90-110 parts by mass, preferably, the using amount of the dealcoholization cross-linking agent is 10-30 parts by mass, and the using amount of the first micromolecule hydroxyl silicone oil is 100 parts by mass. The common dealcoholization type cross-linking agent is a short-chain micromolecule, the prepared pouring sealant is usually low in elongation at break, and the self-made cross-linking agent obtained after modification of micromolecule hydroxyl silicone oil is higher in activity compared with the dealcoholization type cross-linking agent, so that the curing speed and the deep curing speed are greatly improved, the elongation at break of colloid is improved, and the hardness and the modulus are reduced.
In a specific example, the α, ω -dihydroxypolydimethylsiloxane-terminated alkoxy group is at least one of trimethoxy, methyldimethoxy, vinyldimethoxy, triethoxy, methyldiethoxy, vinyltriethoxy, tripropoxy, methyldipropyloxy, and vinyltripropoxy.
In a specific example, the amount of the base polymer is 90 to 110 parts by mass, and the amount of the self-made crosslinking agent is 10 to 60 parts by mass, alternatively, the amount of the base polymer may be, for example, 95 parts, 100 parts, and 105 parts by mass, and the amount of the self-made crosslinking agent may be, for example, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, and 45 parts, 50 parts, and 55 parts by mass. Preferably, the dosage of the base polymer is 100 parts, and the dosage of the self-made crosslinking agent is 20-40 parts. Suitable amounts of cross-linking agent can control the hardness and modulus of the colloid within the desired ranges, and do not affect the transparency of the colloid.
In a specific example, the viscosity of the base polymer is from 1000 to 100000mPa · s at 25 ± 0.5 ℃, the viscosity of the first small molecule hydroxy silicone oil is from 5 to 60mPa · s at 25 ± 0.5 ℃, optionally the viscosity of the base polymer is from 10000 to 80000mPa · s, and the viscosity of the first small molecule hydroxy silicone oil is from 15 to 50mPa · s. The reasonable viscosity range not only enables the colloid to have higher elongation at break, but also is easy to operate and use.
In one specific example, the dealcoholization type coupling agent is at least one of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane.
In one specific example, the method for preparing the self-made crosslinking agent comprises the following steps:
under the protection of nitrogen, heating the first micromolecular hydroxyl silicone oil to 60-100 ℃, then adding a catalyst and a dealcoholization type cross-linking agent, and stirring until the reaction is finished; heating to 150-180 deg.c to decompose the catalyst; heating to 160-180 ℃ and keeping the vacuum degree at 0.01-0.1 MPa to remove the micromolecule low-boiling-point substances.
In one particular example, the catalyst for the self-made crosslinker is an organic amine and/or an organic phosphine, which may be, for example, (CH)3)4NOH、(C4H9)4POH、(C4H9)4At least one of NF.
In a specific example, stirring takes 1 to 6 hours to complete the reaction.
In one specific example, the decomposition catalyst takes 6 to 10 hours.
In a specific example, the removal of the small-molecule low-boiling substance takes 4 to 6 hours.
In a specific example, the paint further comprises 5-80 parts by mass of a toughening polymer, and the toughening polymer comprises the following raw material components:
Figure BDA0002872666250000061
alternatively, the amount of the toughening polymer may be, for example, 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts by mass, and preferably, the toughening polymer is used in an amount of 50 to 80 parts. The raw material components of the toughened polymer comprise:
Figure BDA0002872666250000062
Figure BDA0002872666250000071
the certain amount of the toughening polymer can control the hardness of the colloid within a reasonable range; after the octamethylcyclotetrasiloxane is modified by the tri-functionality, the octamethylcyclotetrasiloxane can form a block branched chain, so that the elongation of the colloid can be increased, and meanwhile, exudation cannot be caused.
In one specific example, the tri-functional alkoxysilane is at least one of trimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane.
In a specific example, the viscosity of the second small-molecule hydroxy silicone oil is 10mPa · s to 60mPa · s.
In one particular example, the second catalyst is an organic amine and/or organic phosphine, which may be, for example, (CH)3)4NOH、(C4H9)4POH、(C4H9)4At least one of NF.
In one particular example, a method of preparing a toughened polymer comprises the steps of:
heating octamethylcyclotetrasiloxane and trifunctional alkoxysilane to 80-120 ℃, then adding a second catalyst for polymerization reaction, adding second micromolecule hydroxyl silicone oil for end capping reaction after the reaction is finished, heating to 160-200 ℃ after the reaction is finished to decompose the catalyst, heating to 180-210 ℃ and keeping the vacuum degree at 0.01-0.1 MPa to remove micromolecule low-boiling-point substances.
In one specific example, the polymerization reaction takes from 5 to 8 hours.
In one specific example, the capping reaction takes from 1 to 3 hours.
In one specific example, the decomposition catalyst takes 2 to 4 hours.
In a specific example, the removal of the small-molecule low-boiling substance takes 1 to 2 hours.
In a specific example, the modified MQ silicone resin further comprises 10-100 parts by mass of the modified MQ silicone resin, and the modified MQ silicone resin comprises the following raw material components:
80-160 parts of MQ silicon resin;
50-160 parts of a toughening polymer; and
80-160 parts of an organic solvent;
the toughening polymers are defined by the specific examples previously described.
Alternatively, the modified MQ silicone resin may be used in an amount of, for example, 20 parts, 30 parts, 40 parts, 50 parts, 60 parts, 70 parts, 80 parts, 90 parts by mass, and preferably, the modified MQ silicone resin is used in an amount of 50 to 100 parts. The raw material components of the modified MQ silicon resin comprise:
100-140 parts of MQ silicon resin;
60-150 parts of a toughening polymer; and
90-140 parts of an organic solvent;
the modified MQ resin is used for adjusting the strength of the colloid, and the modified MQ resin with a certain dosage can ensure that the colloid has better strength, and simultaneously, the modulus of the colloid is not increased, and the elongation at break is not reduced.
In one particular example, the MQ silicone has an MQ value of 0.6 to 1 and is selected from the group consisting of methyl MQ silicone, phenyl MQ silicone, and vinyl MQ silicone.
In one specific example, the preparation method of the modified MQ silicone resin comprises the following steps:
heating MQ silicon resin and an organic solvent under the protection of dry nitrogen or argon, stirring and refluxing until the MQ silicon resin is completely dissolved, and then setting the temperature to be 110-130 ℃ and keeping the vacuum degree to be 0.01-0.03 MPa to remove the organic solvent.
In one specific example, the first catalyst is at least one of dibutyltin dilaurate, dibutyltin diacetate, diisopropoxybis (ethyl acetoacetate) titanium, di-tert-butoxy-bis (ethyl acetoacetate) titanium, 1, 3-propyldioxy-bis (ethyl acetoacetate) titanium, 1, 2-propyldioxy-bis (ethyl acetoacetate) titanium, and dialkoxybis-bis (acetylacetonato) titanium, and the amount of the first catalyst is 0.1 to 5 parts by mass.
In a specific example, the paint further comprises 1-10 parts by mass of a coupling agent, wherein the coupling agent is at least one of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane and gamma-aminoethylaminopropyltriethoxysilane.
According to the preparation method, 90-110 parts by mass of micromolecule hydroxyl silicone oil is used for modifying 5-40 parts by mass of common dealcoholization type cross-linking agent to prepare the cross-linking agent, and the self-prepared cross-linking agent is used for preparing the condensed type transparent pouring sealant composition, so that the curing speed and the deep curing speed of the pouring sealant composition can be greatly improved, the breaking elongation of the pouring sealant colloid is improved, the modulus of the colloid is reduced, the hardness is controlled in a reasonable range, and the transparency of the colloid is not influenced.
In another aspect of the present invention, a method for preparing the transparent potting adhesive composition is provided, which comprises the following steps:
under the protection of dry nitrogen or argon, the first catalyst and the self-made cross-linking agent are uniformly mixed in advance, added into the base polymer, and then uniformly stirred and mixed under the condition of vacuum pumping to prepare the transparent pouring sealant composition. Preferably, the dry nitrogen or argon protective gas is nitrogen or argon.
In one specific example, the toughening polymer and/or the modified MQ silicone resin is pre-added to the base polymer and mixed to homogeneity prior to adding the mixture of the first catalyst and the self-made crosslinker to the base mixture.
The invention also provides another preparation method of the transparent pouring sealant composition, which comprises the following steps:
dividing the self-made cross-linking agent into two parts, uniformly mixing the coupling agent and one part of the self-made cross-linking agent under the protection of dry nitrogen or argon to obtain a first mixture, and sealing and storing the first mixture for later use; preferably, the self-made cross-linking agent is divided into two parts on average;
uniformly mixing the first catalyst and another part of self-made cross-linking agent under the protection of dry nitrogen or argon to obtain a second mixture, and sealing and storing the second mixture for later use;
adding the first mixture into the basic polymer under the protection of dry nitrogen or argon, and then stirring and mixing uniformly under vacuum pumping to obtain a third mixture;
and adding the second mixture into the third mixture under the protection of dry nitrogen or argon, and then stirring and mixing uniformly under vacuum pumping to prepare the transparent pouring sealant composition.
In one particular example, the toughening polymer and/or the modified MQ silicone resin is pre-added to the base polymer and mixed to homogeneity prior to adding the first mixture to the base mixture.
The invention also provides an electronic component which comprises the cured transparent pouring sealant composition.
The present invention will be described in further detail with reference to specific examples and comparative examples. It is understood that the following examples are more specific to the apparatus and materials used, and in other embodiments, are not limited thereto.
Example 1
Preparing a self-made crosslinking agent: under the protection of nitrogen, 100 parts of micromolecular hydroxyl silicone oil with the viscosity of 50 mPas is heated to 80 ℃, and then 0.5 part of (CH) is added3)4NOH and 20 parts of ethyl orthosilicate, and continuously stirring for 5 hours; heating to 160 deg.C and holding for 8 hr to decompose the catalyst; heating to 180 ℃, setting the vacuum degree to be 0.01MPa and keeping for 5 hours to remove the micromolecular low-boiling-point substances.
Preparation of toughened polymer: 1000 parts of octamethylcyclotetrasiloxane and 10 parts of methyltriethoxysilane are heated to 120 ℃ and then 0.2 part of (CH)3)4And (3) carrying out a polymerization reaction for 6 hours, adding 30 parts of micromolecule hydroxyl silicone oil with the viscosity of 20 mPa.s after the reaction is finished, carrying out end capping reaction for 2 hours, heating to 160 ℃ after the reaction is finished, keeping for 4 hours to decompose the catalyst, heating to 180 ℃, setting the vacuum degree to be 0.01MPa, and keeping for 2 hours to remove micromolecule low-boiling-point substances.
Preparation of modified MQ silicone resin: under the protection of nitrogen, 100 parts of MQ methyl silicone resin with MQ value of 0.7 and 100 parts of toluene are stirred and refluxed at 100 ℃ until the MQ silicone resin is completely dissolved, then 100 parts of toughening polymer is added, the temperature is set to be 120 ℃, the vacuum degree is 0.01MPa, and the mixture is kept for 5 hours to remove the toluene.
Preparing a transparent pouring sealant:
uniformly mixing 2 parts of coupling agent gamma-aminoethyl aminopropyltrimethoxysilane and 20 parts of self-made crosslinking agent under the protection of nitrogen to obtain a first mixture, and sealing and storing for later use;
uniformly mixing 1 part of diisopropoxybis (ethyl acetoacetate) titanium catalyst and 20 parts of self-made crosslinking agent under the protection of nitrogen to obtain a second mixture, and sealing and storing for later use;
uniformly stirring 100 parts of trimethoxy terminated alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 1500 mPas, 50 parts of toughening polymer and 80 parts of modified MQ resin under vacuum pumping to obtain a third mixture,
adding the first mixture into the third mixture under the protection of nitrogen, and then stirring and mixing uniformly under the condition of vacuumizing to obtain a fourth mixture;
and adding the second mixture into the fourth mixture under the protection of nitrogen, and then stirring and uniformly mixing under vacuum pumping to prepare the transparent pouring sealant composition.
Example 2
Preparing a self-made crosslinking agent: under the protection of nitrogen, 100 parts of micromolecular hydroxyl silicone oil with the viscosity of 10 mPas is heated to 60 ℃, and then 0.1 part of (CH) is added3)4NOH and 10 parts of vinyltrimethoxysilane, and stirring is continued for 4 hours; heating to 160 deg.C and holding for 6 hr to decompose the catalyst; then the vacuum degree is set at 0.01MPa and kept for 4 hours at 160 ℃ to remove the micromolecular low-boiling-point substances.
Preparation of toughened polymer: 1000 parts of octamethylcyclotetrasiloxane and 10 parts of methyltriethoxysilane are heated to 120 ℃ and then 0.2 part of (CH)3)4And (3) carrying out a polymerization reaction for 6 hours, adding 50 parts of micromolecule hydroxyl silicone oil with the viscosity of 20 mPa.s after the reaction is finished, carrying out end capping reaction for 2 hours, heating to 160 ℃ after the reaction is finished, keeping for 4 hours to decompose the catalyst, heating to 180 ℃, setting the vacuum degree to be 0.01MPa, and keeping for 2 hours to remove micromolecule low-boiling-point substances.
Preparation of modified MQ silicone resin: under the protection of nitrogen, 100 parts of MQ methyl silicone resin with MQ value of 0.9 and 100 parts of toluene are stirred and refluxed at 100 ℃ until the MQ silicone resin is completely dissolved, then 60 parts of toughening polymer is added, the temperature is set to be 120 ℃, the vacuum degree is 0.01MPa and the mixture is kept for 5 hours, so that the toluene is removed.
Preparing a transparent pouring sealant:
uniformly mixing 1 part of coupling agent gamma-aminopropyltrimethoxysilane and 10 parts of self-made crosslinking agent under the protection of nitrogen to obtain a first mixture, and sealing and storing the first mixture for later use;
uniformly mixing 1 part of diisopropoxybis (ethyl acetoacetate) titanium catalyst and 10 parts of self-made crosslinking agent under the protection of nitrogen to obtain a second mixture, and sealing and storing for later use;
uniformly stirring 100 parts of trimethoxy terminated alpha, omega-dihydroxy polydimethylsiloxane with the viscosity of 50000 mPas, 80 parts of toughening polymer and 100 parts of modified MQ resin under the condition of vacuumizing to obtain a third mixture,
adding the first mixture into the third mixture under the protection of nitrogen, and then stirring and mixing uniformly under the condition of vacuumizing to obtain a fourth mixture;
and adding the second mixture into the fourth mixture under the protection of nitrogen, and then stirring and uniformly mixing under vacuum pumping to prepare the transparent pouring sealant composition.
Example 3
Preparing a self-made crosslinking agent: under the protection of nitrogen, 100 parts of micromolecular hydroxyl silicone oil with the viscosity of 50 mPas is heated to 100 ℃, and then 0.4 part of (C) is added4H9)4POH and 30 parts of vinyl trimethoxy silane are stirred for 6 hours; heating to 160 deg.C and holding for 6 hr to decompose the catalyst; at 180 ℃, the vacuum degree is set to be 0.01MPa and kept for 6 hours to remove the micromolecular low-boiling-point substances.
Preparation of toughened polymer: 1000 parts of octamethylcyclotetrasiloxane and 10 parts of methyltriethoxysilane are heated to 120 ℃ and then 0.8 part of (CH)3)4NOH is subjected to polymerization reaction for 8 hours, 80 parts of micromolecular hydroxyl silicone oil with the viscosity of 50mPa & s is added after the reaction is finished to carry out end capping reaction for 2 hours, the temperature is raised to 160 ℃ after the reaction is finished and is kept for 4 hours to decompose the catalyst, and thenThen the temperature is raised to 180 ℃, the vacuum degree is set to be 0.01MPa and kept for 2 hours, so as to remove the micromolecular low-boiling-point substances.
Preparation of modified MQ silicone resin: under the protection of nitrogen, 100 parts of MQ methyl silicone resin with MQ value of 0.9 and 100 parts of toluene are stirred and refluxed at 100 ℃ until the MQ silicone resin is completely dissolved, then 120 parts of toughening polymer is added, the temperature is set to be 120 ℃, the vacuum degree is 0.01MPa and the mixture is kept for 5 hours, so that the toluene is removed.
Preparing a transparent pouring sealant:
uniformly mixing 1 part of coupling agent gamma-aminopropyltrimethoxysilane and 15 parts of self-made crosslinking agent under the protection of nitrogen to obtain a first mixture, and sealing and storing the first mixture for later use;
uniformly mixing 1 part of catalyst dibutyltin dilaurate and 15 parts of self-made crosslinking agent under the protection of nitrogen to obtain a second mixture, and sealing and storing for later use;
uniformly stirring 100 parts of trimethoxy terminated alpha, omega-dihydroxy polydimethylsiloxane with viscosity of 20000 mPas, 60 parts of toughening polymer and 50 parts of modified MQ resin under vacuum pumping to obtain a third mixture,
adding the first mixture into the third mixture under the protection of nitrogen, and then stirring and mixing uniformly under the condition of vacuumizing to obtain a fourth mixture;
and adding the second mixture into the fourth mixture under the protection of nitrogen, and then stirring and uniformly mixing under vacuum pumping to prepare the transparent pouring sealant composition.
Example 4
Example 4 all the amounts and steps of the self-made cross-linking agent were kept the same as in example 1 except that the total amount of the self-made cross-linking agent was 60 parts (divided into two parts to be mixed with the coupling agent and the catalyst, respectively), the toughening polymer was 40 parts, and the modified MQ silicone resin was 40 parts when preparing the transparent potting adhesive.
Comparative example 1
Comparative example 1 corresponds essentially to example 1, but in the preparation of the clear casting compound, uncapped α, ω -dihydroxypolydimethylsiloxane was used.
Comparative example 2
Comparative example 2 was essentially identical to example 2, but the preparation of the modified MQ silicone resin and the transparent potting compound was carried out using the customary toughener polydimethylsiloxane instead of the self-made toughener, in addition to which the MQ value of the MQ silicone resin was 1.2.
Comparative example 3
Comparative example 3 is substantially the same as example 2, but in the preparation of the transparent potting compound, the crosslinking agent is not prepared by self, and the dealcoholization type crosslinking agent methyl trimethoxy silane is adopted.
Comparative example 4
Comparative example 4 is substantially the same as example 3, but when preparing the transparent potting adhesive, the coupling agent or catalyst and the self-made crosslinking agent are not mixed uniformly in advance and then added in portions, but all the components are directly mixed according to the traditional preparation method.
Comparative example 5
Comparative example 5 is substantially the same as example 1, but the amount of the self-made crosslinking agent is 70 parts (divided into two parts to be mixed with the coupling agent and the catalyst respectively) when the transparent pouring sealant is prepared.
Comparative example 6
Comparative example 6 is substantially the same as example 1, but when the transparent pouring sealant is prepared, the amount of the self-made crosslinking agent is 6 parts (the self-made crosslinking agent is evenly divided into two parts to be respectively mixed with the coupling agent and the catalyst).
Comparative example 7
Comparative example 7 is substantially the same as example 1, except that 100 parts of the toughening polymer is used in preparing the transparent potting adhesive.
Comparative example 8
Comparative example 8 is essentially identical to example 1, except that 120 parts of modified MQ silicone resin are used in the preparation of the transparent potting compound.
The samples prepared in the above examples and comparative examples were subjected to two sets of tests, one immediately after preparation and one after 6 months of storage, according to the test items of open time, tensile strength, elongation at break, hardness and light transmittance, in GB/T13477.5-2002.
TABLE 1
Figure BDA0002872666250000151
TABLE 2
Figure BDA0002872666250000152
Figure BDA0002872666250000161
As can be seen from Table 1, the potting adhesive prepared by the scheme of the invention has balanced performance, can have the elongation at break of more than 510% when having certain hardness, and has the advantages of short surface drying time, low modulus, convenience in use, high light transmittance and wide application scenes. In addition, after being stored for six months, the performance is not obviously reduced, which shows that the product of the invention has good stability and is convenient to store.
As can be seen from table 2, in comparative example 1, when the non-blocked α, ω -dihydroxypolydimethylsiloxane was used as the base polymer, the elongation at break of the product was reduced to some extent first, and in addition, the product was deteriorated to some extent after being left for six months, an intermediate affecting the curing reaction was generated, resulting in a great increase in the open time, and the properties of elongation at break, hardness, light transmittance, and the like were also significantly affected; in the comparative example 2, no toughening agent is prepared, which affects the strength and toughness of the product; in the comparative example 3, the common dealcoholization type cross-linking agent is adopted to replace a self-made cross-linking agent, so that the surface drying time is greatly improved, the elongation at break is greatly reduced, the hardness is too high, and the transparency is obviously reduced; in comparative example 4, all the components were directly mixed according to a conventional method, resulting in poor compatibility among the components, and thus various properties were affected, wherein the decrease in transparency was particularly significant, only thirty-one percent; in comparative example 5, too much self-made crosslinker was used, and elongation at break, hardness, and transmittance were affected; in comparative example 6, too little self-made cross-linking agent is used, which results in incomplete reaction and too low hardness of the pouring sealant; in comparative example 7, too much toughening polymer was used, resulting in too low hardness; in comparative example 8, the modified MQ silicone resin was used in an excessive amount, the open time was too long, the hardness was too high, and the elongation at break was reduced.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The transparent pouring sealant composition is characterized by comprising a base polymer, a self-made cross-linking agent and a first catalyst;
the base polymer is alkoxy-terminated alpha, omega-dihydroxy polydimethylsiloxane, the self-made cross-linking agent is prepared by modifying a dealcoholization cross-linking agent by first micromolecule hydroxyl silicone oil, and the dealcoholization cross-linking agent accounts for 5-40 parts by mass, and the first micromolecule hydroxyl silicone oil accounts for 90-110 parts by mass.
2. The transparent pouring sealant composition as claimed in claim 1, wherein the amount of the base polymer is 90-110 parts by mass, and the amount of the self-made cross-linking agent is 10-60 parts by mass.
3. The transparent potting adhesive composition of claim 1, wherein the viscosity of the base polymer is 1000 to 100000 mPa-s at 25 ± 0.5 ℃ and the viscosity of the first small molecule hydroxy silicone oil is 5 to 60 mPa-s at 25 ± 0.5 ℃.
4. The transparent pouring sealant composition as claimed in claim 1, wherein the dealcoholization type cross-linking agent is at least one of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane and vinyltriethoxysilane;
the first catalyst is at least one of dibutyltin dilaurate, dibutyltin diacetate, diisopropoxy bis (ethyl acetoacetate) titanium, di-tert-butoxy-bis (ethyl acetoacetate) titanium, 1, 3-propyldioxy-bis (ethyl acetoacetate) titanium, 1, 2-propyldioxy-bis (ethyl acetoacetate) titanium and dialkoxy bis (acetylacetone) titanium, and the amount of the first catalyst is 0.1-5 parts by mass.
5. The transparent pouring sealant composition according to claim 2, further comprising 5-80 parts by mass of a toughening polymer, wherein the toughening polymer comprises the following raw material components:
Figure FDA0002872666240000011
the tri-functionality alkoxy silane is at least one of trimethoxy silane, methyl triethoxy silane, vinyl trimethoxy silane, vinyl triethoxy silane, ethyl trimethoxy silane and ethyl triethoxy silane; the viscosity of the second micromolecular hydroxyl silicone oil is 10mPa & s-60 mPa & s at 25 +/-0.5 ℃; the second catalyst is organic amine and/or organic phosphine.
6. The transparent pouring sealant composition according to claim 2, further comprising 10-100 parts by mass of modified MQ silicone resin, wherein the modified MQ silicone resin comprises the following raw material components:
80-160 parts of MQ silicon resin;
50-160 parts of a toughening polymer; and
80-160 parts of an organic solvent;
the MQ value of the MQ silicon resin is 0.6-1, and the MQ silicon resin is selected from methyl MQ silicon resin, phenyl MQ silicon resin and vinyl MQ silicon resin; the toughening polymer is defined by the toughening polymer of claim 5.
7. The transparent pouring sealant composition according to any one of claims 1 to 6, further comprising 1 to 10 parts by mass of a coupling agent, wherein the coupling agent is at least one of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-aminoethylaminopropyltrimethoxysilane, and gamma-aminoethylaminopropyltriethoxysilane.
8. The method for preparing the transparent pouring sealant composition according to any one of claims 1 to 6, wherein the first catalyst and the self-made cross-linking agent are uniformly mixed in advance under the protection of dry nitrogen or argon, and then the mixture is uniformly mixed with the rest of the components under the condition of vacuum pumping.
9. The method for preparing the transparent pouring sealant composition according to claim 7, wherein the self-made cross-linking agent is divided into two parts,
uniformly mixing the coupling agent and one part of self-made crosslinking agent under the protection of dry nitrogen or argon to obtain a first mixture;
uniformly mixing the first catalyst and another part of self-made cross-linking agent under the protection of dry nitrogen or argon to obtain a second mixture;
under the protection of dry nitrogen or argon, uniformly stirring and mixing the first mixture and the other components except the first mixture and the second mixture under the condition of vacuumizing to obtain a third mixture;
and under the protection of dry nitrogen or argon, stirring and uniformly mixing the third mixture and the second mixture under the condition of vacuumizing.
10. An electronic component, characterized by comprising the cured transparent potting adhesive composition as claimed in any one of claims 1 to 7.
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