CN116003812A - Cyclic silicon-containing hydrogen bond crosslinking agent, sealant composition containing cyclic silicon-containing hydrogen bond crosslinking agent and preparation method of sealant composition - Google Patents
Cyclic silicon-containing hydrogen bond crosslinking agent, sealant composition containing cyclic silicon-containing hydrogen bond crosslinking agent and preparation method of sealant composition Download PDFInfo
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- 239000003431 cross linking reagent Substances 0.000 title claims abstract description 59
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- 239000000203 mixture Substances 0.000 title claims abstract description 48
- 125000004122 cyclic group Chemical group 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 54
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 21
- WZJUBBHODHNQPW-UHFFFAOYSA-N 2,4,6,8-tetramethyl-1,3,5,7,2$l^{3},4$l^{3},6$l^{3},8$l^{3}-tetraoxatetrasilocane Chemical compound C[Si]1O[Si](C)O[Si](C)O[Si](C)O1 WZJUBBHODHNQPW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 10
- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical compound CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 238000010438 heat treatment Methods 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
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- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical group C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a cyclic silicon-containing hydrogen bond cross-linking agent and a preparation method thereof, wherein the cyclic silicon-containing hydrogen bond cross-linking agent comprises 200 parts of gamma- (methacryloyloxy) propyl trimethoxy silane, 100-120 parts of tetramethyl cyclotetrasiloxane with hydrogen content of 1.6%, 1-5 parts of graphene oxide, 0.02-0.04 part of first platinum catalyst and 0.008-0.02 part of methylbutynol; an adhesive sealant composition for an inductor and a method of preparing the same are also disclosed. The adhesive sealant composition for the inductor provided by the invention has the advantages that the annular silicon-containing hydrogen bond crosslinking agent is utilized to endow colloid with excellent adhesive property, a sealing ring which has high strength and tight adhesive property with an aluminum shell of the inductor can be formed by curing at 120 ℃, the sealing ring has good sealing waterproof performance and shockproof performance, the complex tooling process for pasting a 3M adhesive tape on the traditional sealing ring is replaced in a simple and efficient manner, the quick construction sealing requirement is met, and the tooling problem of the sealing ring of the optical Fu Diangan device is effectively solved.
Description
Technical Field
The invention relates to the technical field of photovoltaic inductor sealing materials, in particular to an annular silicon-containing hydrogen bond cross-linking agent, a sealant composition containing the same and a preparation method of the sealant composition.
Background
Photovoltaic has been developed rapidly in recent years as a novel energy source with high efficiency. The inverter is a core component of photovoltaic equipment, the inductor is an important component in the inverter, the temperature of the high-power inductor can reach 160 ℃ in daily work, a metal radiator is often designed at the foot position of the inductor, the inductor is assembled in a flip-chip mode for better radiating heat, the inductor further meets the requirements of shock resistance and water resistance on the basis, and sealing rubber strips are required to be assembled on the inductor. The traditional sealing mode is to use an injection molded silica gel sealing ring, paste a 3M double-sided tape on the sealing ring, then paste the sealing ring on an inductor, and the construction process is complicated, if oil stains exist on the inductor, the debonding phenomenon often occurs, the reworking rate is high, and the production efficiency is seriously affected. At present, hydrogen-containing silicone oil is generally adopted as a sealant of a cross-linking agent, the hydrogen-containing silicone oil belongs to a linear body cross-linking agent, the physical and mechanical strength of the cured hydrogen-containing silicone oil is relatively poor, a large amount of tackifier is required to be additionally added, and the curing effect and the mechanical strength are poor. Therefore, development of an adhesive sealant for inductors is important.
Disclosure of Invention
In order to overcome the technical problems, the invention discloses a cyclic silicon-containing hydrogen bond cross-linking agent, a sealant composition containing the cyclic silicon-containing hydrogen bond cross-linking agent and a preparation method of the sealant composition.
The technical scheme adopted by the invention for achieving the purpose is as follows:
the cyclic silicon-containing hydrogen bond cross-linking agent comprises the following raw materials in parts by mass: 200 parts of gamma- (methacryloyloxy) propyl trimethoxysilane, 100 to 120 parts of tetramethyl cyclotetrasiloxane with hydrogen content of 1.6%, 1 to 5 parts of graphene oxide, 0.02 to 0.04 part of first platinum catalyst and 0.008 to 0.02 part of methylbutynol.
The cyclic silicon-containing hydrogen bond cross-linking agent, wherein the purity of the graphene oxide is greater than or equal to 90%, the thickness is 0.3-1 nm, and the oxygen content is greater than 45%.
A preparation method of a cyclic silicon-containing hydrogen bond cross-linking agent, which is used for preparing the cyclic silicon-containing hydrogen bond cross-linking agent;
the preparation method comprises the following steps:
step 1, taking gamma- (methacryloyloxy) propyl trimethoxysilane, tetramethyl cyclotetrasiloxane with hydrogen content of 1.6% and graphene oxide, controlling the temperature to be 25+/-2 ℃, dropwise adding a first platinum catalyst while stirring at a stirring speed of 200-220 r/min, and carrying out heat preservation and stirring for 5-10 min to obtain a first reactant;
step 2, maintaining the stirring speed of 200-220 r/min, heating the first reactant to 80+/-2 ℃, and carrying out heat preservation reaction for 120+/-10 min to obtain a second reactant;
and 3, cooling the second reactant to 25+/-2 ℃, adding methyl butynol under the condition of continuous stirring, and uniformly mixing to obtain the annular silicon-containing hydrogen bond cross-linking agent.
An adhesive sealant composition for an inductor comprises the following raw materials in parts by weight: 100 parts of vinyl-terminated polydimethylsiloxane, 10-25 parts of fumed silica, 0.01-0.05 part of inhibitor, 3-6 parts of cyclic silicon-containing hydrogen bond cross-linking agent and 0.8 part of second platinum catalyst.
The adhesive sealant composition for an inductor, wherein the viscosity of the vinyl-terminated polydimethylsiloxane is 350-5000 mPas, and the content of dimethylsiloxane ring bodies D3-D10 is less than 300ppm.
The adhesive sealant composition for the inductor, wherein the fumed silica is hydrophobic fumed silica and has a specific surface area of 180-200 m 2 /g。
The adhesive sealant composition for an inductor, wherein the viscosity of the cyclic silicon-containing hydrogen bond cross-linking agent is 5-35 mPa.s, and the hydrogen content is 0.1-0.8 wt%.
The preparation method of the adhesive sealant composition for the inductor is characterized by comprising the steps of preparing the adhesive sealant composition for the inductor;
the preparation method comprises the following steps:
step I, taking vinyl-terminated polydimethylsiloxane and fumed silica, and starting to heat under a first stirring condition to obtain a reactant A;
step II, heating the reactant A to 120-130 ℃ under a second stirring condition, and starting vacuum removal of low molecules to obtain a reactant B;
step III, cooling the reactant B to 5+/-2 ℃, adding a cyclic silicon-containing hydrogen bond cross-linking agent and an inhibitor, and carrying out vacuum reaction under a third stirring condition to obtain a reactant C;
and IV, adding a second platinum catalyst into the reactant C, and carrying out vacuum reaction under a fourth stirring condition to obtain the adhesive sealant composition for the inductor.
The preparation method of the adhesive sealant composition for the inductor comprises the following steps of: revolution is carried out at 40-50 rpm, the dispersing disc is stirred at 500-600 rpm, and stirring time is 60-70 minutes;
the second stirring condition is as follows: revolution is carried out at 40-50 rpm, the dispersing disc is stirred at 500-600 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 90-100 minutes.
The preparation method of the adhesive sealant composition for the inductor, wherein the third stirring condition is as follows: revolution is carried out at 30-35 rpm, the dispersion disc is stirred at 200-300 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 10-20 minutes;
the fourth stirring condition is as follows: revolution is carried out at 30-35 rpm, the dispersing disc is stirred at 200-300 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 10-20 minutes.
The beneficial effects of the invention include the following points:
(1) The synthesis of the cyclic silicon-containing hydrogen bond cross-linking agent is that a silicon-hydrogen addition reaction is carried out between partial silicon hydrogen bond of the tetramethyl cyclotetrasiloxane and propenyl of gamma- (methacryloyloxy) propyl trimethoxy silane and alkenyl of the graphene oxide under the action of the first platinum catalyst, so that a trimethoxy group and a graphene oxide structure containing a large number of oxygen-containing functional groups (mainly hydroxy, epoxy, carboxyl and carbonyl) are connected at the silicon-hydrogen group position of the tetramethyl cyclotetrasiloxane to form an adhesive group of the cyclic silicon-containing hydrogen bond cross-linking agent, and the adhesive group can form a tight and firm adhesive effect with an aluminum shell of an inductor, and particularly can quickly and effectively establish an adhesive effect under the medium-high temperature condition;
(2) The tetramethyl cyclotetrasiloxane is also reserved with active silicon hydrogen bonds, so that the tetramethyl cyclotetrasiloxane is used for being crosslinked with the vinyl-terminated polydimethylsiloxane under the action of the second platinum catalyst in the later process of preparing the adhesive sealant composition to be solidified into an elastomer, and the physical mechanical strength of the annular silicon-containing hydrogen bond crosslinking agent with an annular structure after being solidified is greatly improved compared with that of the traditional linear body crosslinking agent, so that the requirement of an inductor in a flip-chip technology on the high physical mechanical strength of the sealant is exactly met;
(3) The ring-shaped silicon-containing hydrogen bond cross-linking agent not only contains a large number of polar groups such as adhesive methoxy groups, hydroxyl groups, epoxy groups, completion groups and the like, has an easier adhesive effect on an aluminum shell of an inductor, but also contains a silicon hydrogen bond capable of participating in a vinyl-terminated polydimethylsiloxane reaction, has a ring-shaped structure, has a synergistic effect on the enhancement effect of the physical and mechanical properties of colloid, is different from the traditional hydrogen-containing silicone oil only containing the silicon hydrogen bond, and can form an elastomer which has high strength and is tightly connected with the aluminum shell of the inductor by medium-temperature rapid solidification without adding an adhesion promoter;
(4) The adhesive sealant composition for the inductor is a single-component sealant, is convenient to construct, can be cured into sealant with excellent performance on the inductor after being cured at medium temperature for 20 minutes after dispensing, and has high production efficiency and low cost, and is incomparable with the traditional sealing ring assembly mode;
(5) The adhesive sealant composition for the inductor utilizes the annular silicon-containing hydrogen bond crosslinking agent to endow excellent adhesion between the colloid and the aluminum shell of the inductor, and the adhesive sealant composition can be cured at 120 ℃ to form a sealing ring with high strength and tight adhesion with the aluminum shell of the inductor, has good sealing waterproof performance and shockproof performance, realizes the complex tooling process of replacing the traditional sealing ring with a 3M adhesive tape in a simple and efficient manner, is particularly suitable for the rapid construction sealing requirement of a photovoltaic inverter, has obvious effect, and effectively solves the tooling problem of the sealing ring of the optical Fu Diangan device.
Detailed Description
The present invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention.
The invention provides a cyclic silicon-containing hydrogen bond cross-linking agent, which comprises the following raw materials in parts by mass: 200 parts of gamma- (methacryloyloxy) propyl trimethoxysilane, 100 to 120 parts of tetramethyl cyclotetrasiloxane with hydrogen content of 1.6%, 1 to 5 parts of graphene oxide, 0.02 to 0.04 part of first platinum catalyst and 0.008 to 0.02 part of methylbutynol.
Preferably, the purity of the graphene oxide is greater than or equal to 90%, the thickness is 0.3-1 nm, and the oxygen content is greater than 45%; the graphene oxide has higher purity, can avoid excessive interference of other impurities on the reaction, ensures that the graphene oxide contains more oxygen active groups due to higher oxygen content, is favorable for the progress of radical reaction, and has more excellent adhesion and reinforcement synergistic effect on the cyclic silicon-containing hydrogen bond crosslinking agent due to the graphene oxide with the thickness of less than 1 nm.
The preparation method of the cyclic silicon-containing hydrogen bond cross-linking agent comprises the following steps:
step 1, taking gamma- (methacryloyloxy) propyl trimethoxysilane, tetramethyl cyclotetrasiloxane with hydrogen content of 1.6% and graphene oxide, controlling the temperature to be 25+/-2 ℃, dropwise adding a first platinum catalyst while stirring at a stirring speed of 200-220 r/min, and carrying out heat preservation and stirring for 5-10 min to obtain a first reactant; wherein the stirring speed is 200-220 rpm;
step 2, maintaining the stirring speed of 200-220 r/min, heating the first reactant to 80+/-2 ℃, and carrying out heat preservation reaction for 120+/-10 min to obtain a second reactant; wherein the stirring speed is 200-220 rpm;
and 3, cooling the second reactant to 25+/-2 ℃, adding methyl butynol under the condition of continuous stirring, and uniformly mixing to obtain the annular silicon-containing hydrogen bond cross-linking agent.
Specifically, the synthesis of the cyclic silicon-containing hydrogen bond cross-linking agent is that the silicon-hydrogen addition reaction is carried out between part of silicon hydrogen bonds of the tetramethyl cyclotetrasiloxane and propenyl of gamma- (methacryloyloxy) propyl trimethoxy silane and alkenyl of the graphene oxide under the action of the first platinum catalyst, so that a trimethoxy group and a graphene oxide structure containing a large amount of oxygen-containing functional groups (mainly hydroxy, epoxy, carboxyl and carbonyl) are connected at the silicon-hydrogen group position of the tetramethyl cyclotetrasiloxane to form an adhesive group of the cyclic silicon-containing hydrogen bond cross-linking agent, and the adhesive group can form a tight and firm adhesive effect with an aluminum shell of an inductor, and particularly can quickly and effectively establish the adhesive effect under the medium-high temperature condition.
Meanwhile, the tetramethyl cyclotetrasiloxane is also reserved with active silicon hydrogen bonds, so that the tetramethyl cyclotetrasiloxane is used for crosslinking with vinyl-terminated polydimethylsiloxane under the action of a second platinum catalyst in the later process of preparing the adhesive sealant composition, an elastomer is solidified, the physical mechanical strength of the annular silicon-containing hydrogen bond crosslinking agent with an annular structure after solidification is greatly improved compared with that of the traditional linear body crosslinking agent, and the requirement of an inductor in a flip-chip technology on the high physical mechanical strength of the sealant is just met.
In addition, the ring-shaped silicon-containing hydrogen bond cross-linking agent not only contains a large number of polar groups such as adhesive methoxy groups, hydroxyl groups, epoxy groups and completion groups, and the like, has an easier adhesive effect on the aluminum shell of the inductor, but also contains silicon hydrogen bonds capable of participating in the reaction of vinyl-terminated polydimethylsiloxane, has a ring-shaped structure, has a synergistic effect on the enhancement effect of the physical and mechanical properties of colloid, is different from the traditional hydrogen-containing silicone oil only containing the silicon hydrogen bonds, and can form an elastomer which has high strength and is tightly connected with the aluminum shell of the inductor by medium-temperature rapid solidification without adding an adhesion promoter.
The invention also discloses an adhesive sealant composition for the inductor, which comprises the following raw materials in parts by mass: 100 parts of vinyl-terminated polydimethylsiloxane, 10-25 parts of fumed silica, 0.01-0.05 part of inhibitor, 3-6 parts of cyclic silicon-containing hydrogen bond cross-linking agent and 0.8 part of second platinum catalyst.
Specifically, the first platinum catalyst and the second platinum catalyst are both cassiterite platinum catalysts.
Preferably, the viscosity of the vinyl-terminated polydimethylsiloxane is 350-5000 mPa.s, the content of the dimethylsiloxane ring bodies D3-D10 is less than 300ppm, and poor electrical performance caused by volatilization and migration of the D3-D10 to a welding contact point in a circuit when the inverter inductor operates at high temperature can be effectively avoided.
Preferably, the fumed silica is hydrophobic fumed silica and has a specific surface area of 180-200 m 2 /g。
Preferably, the viscosity of the cyclic silicon-containing hydrogen bond cross-linking agent is 5-35 mPa.s, and the hydrogen content is 0.1-0.8 wt%;
specifically, the inhibitor is 1-ethynyl 1-cyclohexanol.
The preparation method of the adhesive sealant composition for the inductor comprises the following steps:
step I, taking vinyl-terminated polydimethylsiloxane and fumed silica, and starting to heat under a first stirring condition to obtain a reactant A;
step II, heating the reactant A to 120-130 ℃ under a second stirring condition, and starting vacuum removal of low molecules to obtain a reactant B;
step III, cooling the reactant B to 5+/-2 ℃, adding a cyclic silicon-containing hydrogen bond cross-linking agent and an inhibitor, and carrying out vacuum reaction under a third stirring condition to obtain a reactant C;
and IV, adding a catalyst into the reactant C, and carrying out vacuum reaction under a fourth stirring condition to obtain the adhesive sealant composition for the inductor.
Preferably, the first stirring condition is: revolution is carried out at 40-50 rpm, the dispersing disc is stirred at 500-600 rpm, and stirring time is 60-70 minutes;
the second stirring condition is as follows: revolution is carried out at 40-50 rpm, the dispersing disc is stirred at 500-600 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 90-100 minutes;
the third stirring condition is as follows: revolution is carried out at 30-35 rpm, the dispersion disc is stirred at 200-300 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 10-20 minutes;
the fourth stirring condition is as follows: revolution is carried out at 30-35 rpm, the dispersing disc is stirred at 200-300 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 10-20 minutes.
Specifically, when the adhesive sealant composition for the inductor is directly extruded and constructed at the groove of the aluminum shell of the inductor by using adhesive sealant equipment in use, the adhesive sealant composition for the inductor passes through a tunnel furnace at 120 ℃ for 10 minutes on a conveyor belt, so that a sealing ring with high strength and tight adhesion with the aluminum shell of the inductor can be formed by curing, the adhesive sealant composition has good sealing waterproof performance and shockproof performance, the complex tooling process for sticking a 3M adhesive tape to a traditional sealing ring is replaced in a simple and efficient mode, the effect is obvious, and the tooling difficulty of the sealing ring of the optical Fu Diangan device is effectively solved.
The following examples are now described in detail for the preparation process according to the invention:
example 1: the embodiment discloses a cyclic silicon-containing hydrogen bond cross-linking agent, and the preparation method comprises the following steps:
step 1, 200 parts by mass of gamma- (methacryloyloxy) propyl trimethoxysilane, 100 parts by mass of tetramethyl cyclotetrasiloxane with hydrogen content of 1.6% and 1 part by mass of graphene oxide are taken and added into a reactor with a constant temperature function, the temperature is controlled to be 25 ℃, 0.02 part by mass of a Karster platinum catalyst is dropwise added while stirring at a stirring speed of 220 revolutions per minute, and the temperature is kept for 8 minutes to obtain a first reactant;
step 2, maintaining the stirring speed of 220 r/min, heating the first reactant to 80 ℃, and carrying out heat preservation reaction for 120 minutes to obtain a second reactant;
and 3, cooling the second reactant to 25 ℃, and adding 0.008 parts by mass of methylbutinol under the condition of continuous stirring, and uniformly mixing to obtain the annular silicon-containing hydrogen bond cross-linking agent.
Also disclosed is an adhesive sealant composition for an inductor, the preparation method thereof comprising the steps of:
step I, in a dynamic mixer, taking 100 parts by mass of vinyl-terminated polydimethylsiloxane and 10 parts by mass of surface-treated fumed silica with the viscosity of 350 mPa.s, keeping revolution at 40 rpm, stirring a dispersion disc at 500 rpm, and starting heating reaction for 60 minutes to obtain a reactant A;
step II, maintaining revolution at 40 rpm, stirring a dispersing disc at 500 rpm, heating the reactant A to 120 ℃, and vacuum removing low molecules for 90 minutes at the vacuum degree of-0.09 MPa to obtain a reactant B;
step III, cooling the reactant B to 5 ℃, adding 3 parts by mass of a cyclic silicon-containing hydrogen bond cross-linking agent with the viscosity of 30 mPas and the hydrogen content of 0.5wt% and 0.01 part by mass of a 1-ethynyl 1-cyclohexyl alcohol inhibitor, keeping revolution at 30 rpm, stirring a dispersion disc at 200 rpm for 2 minutes, and carrying out vacuum reaction at a vacuum degree of-0.09 MPa for 10 minutes to obtain a reactant C;
and IV, adding 0.8 part by mass of a Karst platinum catalyst into the reactant C, keeping revolution at 30 revolutions per minute, stirring a dispersion disc at 200 revolutions per minute, and carrying out vacuum reaction for 10 minutes at a vacuum degree of-0.09 MPa to prepare the adhesive sealant composition for the inductor.
Example 2: the embodiment discloses a cyclic silicon-containing hydrogen bond cross-linking agent, and the preparation method comprises the following steps:
step 1, 200 parts by mass of gamma- (methacryloyloxy) propyl trimethoxysilane, 105 parts by mass of tetramethyl cyclotetrasiloxane with hydrogen content of 1.6% and 2 parts by mass of graphene oxide are taken and added into a reactor with a constant temperature function, the temperature is controlled to be 25 ℃, 0.025 parts by mass of a Karster platinum catalyst is dropwise added while stirring at a stirring speed of 220 revolutions per minute, and the temperature is kept for 8 minutes to obtain a first reactant;
step 2, maintaining the stirring speed of 220 r/min, heating the first reactant to 80 ℃, and carrying out heat preservation reaction for 120 minutes to obtain a second reactant;
and 3, cooling the second reactant to 25 ℃, and adding 0.011 parts by mass of methylbutinol under the condition of continuous stirring, and uniformly mixing to obtain the annular silicon-containing hydrogen bond cross-linking agent.
Also disclosed is an adhesive sealant composition for an inductor, the preparation method thereof comprising the steps of:
step I, in a dynamic mixer, taking 100 parts by mass of vinyl-terminated polydimethylsiloxane and 15 parts by mass of surface-treated fumed silica with the viscosity of 500 mPa.s, keeping revolution at 40 rpm, stirring a dispersion disc at 500 rpm, and starting heating reaction for 60 minutes to obtain a reactant A;
step II, maintaining revolution at 40 rpm, stirring a dispersing disc at 500 rpm, heating the reactant A to 120 ℃, and vacuum removing low molecules for 90 minutes at the vacuum degree of-0.09 MPa to obtain a reactant B;
step III, cooling the reactant B to 5 ℃, adding 4 parts by mass of a cyclic silicon-containing hydrogen bond cross-linking agent with the viscosity of 30 mPas and the hydrogen content of 0.4wt% and 0.03 part by mass of a 1-ethynyl 1-cyclohexyl alcohol inhibitor, keeping revolution at 30 rpm, stirring a dispersion disc at 200 rpm for 2 minutes, and carrying out vacuum reaction at a vacuum degree of-0.09 MPa for 10 minutes to obtain a reactant C;
and IV, adding 0.8 part by mass of a Karst platinum catalyst into the reactant C, keeping revolution at 30 revolutions per minute, stirring a dispersion disc at 200 revolutions per minute, and carrying out vacuum reaction for 10 minutes at a vacuum degree of-0.09 MPa to prepare the adhesive sealant composition for the inductor.
Example 3: the embodiment discloses a cyclic silicon-containing hydrogen bond cross-linking agent, and the preparation method comprises the following steps:
step 1, 200 parts by mass of gamma- (methacryloyloxy) propyl trimethoxysilane, 110 parts by mass of tetramethyl cyclotetrasiloxane with hydrogen content of 1.6% and 3 parts by mass of graphene oxide are taken and added into a reactor with a constant temperature function, the temperature is controlled to be 27 ℃, 0.03 parts by mass of a Karster platinum catalyst is dropwise added while stirring at a stirring speed of 220 revolutions per minute, and the temperature is kept for 5 minutes to obtain a first reactant;
step 2, maintaining the stirring speed of 220 revolutions per minute, heating the first reactant to 82 ℃, and reacting for 110 minutes with heat preservation to obtain a second reactant;
and 3, cooling the second reactant to 23 ℃, and adding 0.017 parts by mass of methylbutinol under the condition of continuous stirring, and uniformly mixing to obtain the annular silicon-containing hydrogen bond cross-linking agent.
Also disclosed is an adhesive sealant composition for an inductor, the preparation method thereof comprising the steps of:
step I, in a dynamic mixer, taking 100 parts by mass of vinyl-terminated polydimethylsiloxane and 20 parts by mass of surface-treated fumed silica with the viscosity of 1000 mPa.s, keeping revolution at 40 rpm, stirring a dispersion disc at 500 rpm, and starting heating reaction for 60 minutes to obtain a reactant A;
step II, maintaining revolution at 40 rpm, stirring a dispersing disc at 500 rpm, heating the reactant A to 120 ℃, and vacuum removing low molecules for 90 minutes at the vacuum degree of-0.09 MPa to obtain a reactant B;
step III, cooling the reactant B to 5 ℃, adding 5 parts by mass of a cyclic silicon-containing hydrogen bond cross-linking agent with the viscosity of 25 mPas and the hydrogen content of 0.5wt% and 0.04 part by mass of a 1-ethynyl 1-cyclohexyl alcohol inhibitor, keeping revolution at 30 rpm, stirring a dispersion disc at 200 rpm for 2 minutes, and carrying out vacuum reaction at a vacuum degree of-0.09 MPa for 10 minutes to obtain a reactant C;
and IV, adding 0.8 part by mass of a Karst platinum catalyst into the reactant C, keeping revolution at 30 revolutions per minute, stirring a dispersion disc at 200 revolutions per minute, and carrying out vacuum reaction for 10 minutes at a vacuum degree of-0.09 MPa to prepare the adhesive sealant composition for the inductor.
Example 4: the embodiment discloses a cyclic silicon-containing hydrogen bond cross-linking agent, and the preparation method comprises the following steps:
step 1, 200 parts by mass of gamma- (methacryloyloxy) propyl trimethoxysilane, 120 parts by mass of tetramethyl cyclotetrasiloxane with hydrogen content of 1.6% and 5 parts by mass of graphene oxide are taken and added into a reactor with a constant temperature function, the temperature is controlled to be 27 ℃, 0.05 part by mass of a Karster platinum catalyst is dropwise added while stirring at a stirring speed of 220 revolutions per minute, and the temperature is kept for 5 minutes to obtain a first reactant;
step 2, maintaining the stirring speed of 220 revolutions per minute, heating the first reactant to 82 ℃, and reacting for 110 minutes with heat preservation to obtain a second reactant;
and 3, cooling the second reactant to 23 ℃, and adding 0.02 part by mass of methylbutinol under the condition of continuous stirring, and uniformly mixing to obtain the annular silicon-containing hydrogen bond cross-linking agent.
Also disclosed is an adhesive sealant composition for an inductor, the preparation method thereof comprising the steps of:
step I, in a dynamic mixer, taking 100 parts by mass of vinyl-terminated polydimethylsiloxane and 25 parts by mass of surface-treated fumed silica with the viscosity of 2000 mPa.s, keeping revolution at 50 rpm, stirring a dispersion disc at 600 rpm, and starting heating reaction for 70 minutes to obtain a reactant A;
step II, maintaining revolution at 50 rpm, stirring a dispersion disc at 600 rpm, heating the reactant A to 130 ℃, and vacuum removing low molecules for 90 minutes at the vacuum degree of-0.1 MPa to obtain a reactant B;
step III, cooling the reactant B to 3 ℃, adding 6 parts by mass of a cyclic silicon-containing hydrogen bond cross-linking agent with the viscosity of 15 mPas and the hydrogen content of 0.3wt% and 0.05 part by mass of a 1-ethynyl 1-cyclohexyl alcohol inhibitor, keeping revolution at 35 rpm, stirring a dispersion disc at 300 rpm for 2 minutes, and carrying out vacuum reaction for 20 minutes at a vacuum degree of-0.1 MPa to obtain a reactant C;
and IV, adding 0.8 part by mass of a Karst platinum catalyst into the reactant C, keeping revolution at 35 revolutions per minute, stirring a dispersion disc at 300 revolutions per minute, and carrying out vacuum reaction for 20 minutes at a vacuum degree of-0.1 MPa to prepare the adhesive sealant composition for the inductor.
The following performance tests were conducted on the adhesive sealant compositions for inductors prepared in examples 1 to 4:
(1) Injecting the glue into the aluminum shell groove of the inductor, curing for 10 minutes at 120 ℃, and prying the glue to observe the bonding characteristic between the glue and the aluminum shell;
(2) Coating a sizing material on an aluminum sheet with the specification of length-width-thickness=100 (+ -0.25) mm (+ -25.25) mm (+ -1.6 (+ -0.1) mm, coating the aluminum sheet with the length of 12.5 mm+/-0.25 mm, overlapping another aluminum sheet with the same specification on the sizing material-coated sheet, clamping the aluminum sheet by a clamp, baking the aluminum sheet at 120 ℃ for 10 minutes to prepare a shear sample, and testing the shear strength according to GB/T7124-2008 adhesive tensile shear strength (rigid materials vs rigid materials);
(3) Injecting the sizing material into a mold with the thickness of 2mm, and testing the tensile strength and the elongation at break of the prepared sample according to GB/T528-1998;
(4) Injecting the sizing material into a mold with the thickness of 6mm, and testing the Shore A hardness of the prepared sample according to GB/T531.2-2009. The detailed test results are shown in table 1.
TABLE 1 Performance test results
The above description is merely of the preferred embodiments of the invention, and is not intended to limit the invention in any way
And (5) limiting. Any person skilled in the art can make many possible variations and modifications to the technical solution of the present invention or modifications to equivalent embodiments using the technical means and technical contents disclosed above without departing from the scope of the technical solution of the present invention. Therefore, all equivalent changes according to the shape, structure and principle of the present invention should be covered in the protection scope of the present invention.
Claims (10)
1. The cyclic silicon-containing hydrogen bond cross-linking agent is characterized by comprising the following raw materials in parts by mass: 200 parts of gamma- (methacryloyloxy) propyl trimethoxysilane, 100 to 120 parts of tetramethyl cyclotetrasiloxane with hydrogen content of 1.6%, 1 to 5 parts of graphene oxide, 0.02 to 0.04 part of first platinum catalyst and 0.008 to 0.02 part of methylbutynol.
2. The cyclic silicon-containing hydrogen bond cross-linking agent according to claim 1, wherein the graphene oxide has a purity of 90% or more, a thickness of 0.3-1 nm, and an oxygen content of 45% or more.
3. A method for preparing a cyclic silicon-containing hydrogen bond cross-linking agent, which is characterized in that the cyclic silicon-containing hydrogen bond cross-linking agent is used for preparing the cyclic silicon-containing hydrogen bond cross-linking agent according to claim 1 or 2;
the preparation method comprises the following steps:
step 1, taking gamma- (methacryloyloxy) propyl trimethoxysilane, tetramethyl cyclotetrasiloxane with hydrogen content of 1.6% and graphene oxide, controlling the temperature to be 25+/-2 ℃, dropwise adding a first platinum catalyst while stirring at a stirring speed of 200-220 r/min, and carrying out heat preservation and stirring for 5-10 min to obtain a first reactant;
step 2, maintaining the stirring speed of 200-220 r/min, heating the first reactant to 80+/-2 ℃, and carrying out heat preservation reaction for 120+/-10 min to obtain a second reactant;
and 3, cooling the second reactant to 25+/-2 ℃, adding methyl butynol under the condition of continuous stirring, and uniformly mixing to obtain the annular silicon-containing hydrogen bond cross-linking agent.
4. The adhesive sealant composition for the inductor is characterized by comprising the following raw materials in parts by weight: 100 parts of vinyl-terminated polydimethylsiloxane, 10-25 parts of fumed silica, 0.01-0.05 part of inhibitor, 3-6 parts of cyclic silicon-containing hydrogen bond cross-linking agent as defined in claim 1 and 0.8 part of second platinum catalyst.
5. The adhesive sealant composition for an inductor according to claim 4, wherein the viscosity of the vinyl-terminated polydimethylsiloxane is 350 to 5000 mPa-s and the content of dimethylsiloxane ring D3 to D10 is less than 300ppm.
6. The adhesive sealant composition for inductors as set forth in claim 5, wherein said fumed silica is hydrophobic fumed silica and has a specific surface area of 180 to 200m 2 /g。
7. The adhesive sealant composition for an inductor according to claim 6, wherein the viscosity of the cyclic silicon-containing hydrogen bond crosslinking agent is 5 to 35 mPa-s and the hydrogen content is 0.1 to 0.8wt%.
8. A method for producing an adhesive sealant composition for an inductor, characterized in that the method is used for producing the adhesive sealant composition for an inductor according to any one of claims 4 to 7;
the preparation method comprises the following steps:
step I, taking vinyl-terminated polydimethylsiloxane and fumed silica, and starting to heat under a first stirring condition to obtain a reactant A;
step II, heating the reactant A to 120-130 ℃ under a second stirring condition, and starting vacuum removal of low molecules to obtain a reactant B;
step III, cooling the reactant B to 5+/-2 ℃, adding a cyclic silicon-containing hydrogen bond cross-linking agent and an inhibitor, and carrying out vacuum reaction under a third stirring condition to obtain a reactant C;
and IV, adding a second platinum catalyst into the reactant C, and carrying out vacuum reaction under a fourth stirring condition to obtain the adhesive sealant composition for the inductor.
9. The method of producing an adhesive sealant composition for inductors according to claim 8, wherein the first stirring condition is: revolution is carried out at 40-50 rpm, the dispersing disc is stirred at 500-600 rpm, and stirring time is 60-70 minutes;
the second stirring condition is as follows: revolution is carried out at 40-50 rpm, the dispersing disc is stirred at 500-600 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 90-100 minutes.
10. The method for producing an adhesive sealant composition for inductors according to claim 9, wherein the third stirring condition is: revolution is carried out at 30-35 rpm, the dispersion disc is stirred at 200-300 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 10-20 minutes;
the fourth stirring condition is as follows: revolution is carried out at 30-35 rpm, the dispersing disc is stirred at 200-300 rpm, the vacuum degree is minus 0.09MPa to minus 0.1MPa, and the stirring time is 10-20 minutes.
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| CN102775786A (en) * | 2012-08-09 | 2012-11-14 | 西北工业大学 | Graphene oxide/cyanate ester composite material and preparation method thereof |
| CN109401669A (en) * | 2018-10-15 | 2019-03-01 | 广州机械科学研究院有限公司 | Middle low-temperature setting bonding dual composition addition type liquid silastic and preparation method thereof |
| CN114350311A (en) * | 2022-01-10 | 2022-04-15 | 东莞市佳迪新材料有限公司 | Organic silicon heat-conducting pouring sealant composition for photovoltaic inverter and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775786A (en) * | 2012-08-09 | 2012-11-14 | 西北工业大学 | Graphene oxide/cyanate ester composite material and preparation method thereof |
| CN109401669A (en) * | 2018-10-15 | 2019-03-01 | 广州机械科学研究院有限公司 | Middle low-temperature setting bonding dual composition addition type liquid silastic and preparation method thereof |
| CN114350311A (en) * | 2022-01-10 | 2022-04-15 | 东莞市佳迪新材料有限公司 | Organic silicon heat-conducting pouring sealant composition for photovoltaic inverter and preparation method thereof |
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