CN118308062A - Double-component polyurethane pouring sealant and preparation method and application thereof - Google Patents

Double-component polyurethane pouring sealant and preparation method and application thereof Download PDF

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Publication number
CN118308062A
CN118308062A CN202410469351.0A CN202410469351A CN118308062A CN 118308062 A CN118308062 A CN 118308062A CN 202410469351 A CN202410469351 A CN 202410469351A CN 118308062 A CN118308062 A CN 118308062A
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China
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component
parts
polyol
bentonite
component polyurethane
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Inventor
李云龙
应天祥
陶小乐
何丹薇
尤羽中
何永富
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Hangzhou Zhijiang Silicone Chemicals Co Ltd
Hangzhou Zhijiang New Material Co Ltd
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Hangzhou Zhijiang Silicone Chemicals Co Ltd
Hangzhou Zhijiang New Material Co Ltd
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Priority to CN202410469351.0A priority Critical patent/CN118308062A/en
Publication of CN118308062A publication Critical patent/CN118308062A/en
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Abstract

The invention provides a bi-component polyurethane pouring sealant, a preparation method and application thereof, wherein the bi-component polyurethane pouring sealant comprises a component A and a component B; the component A is isocyanate-terminated polymer; the component B comprises the following components in parts by weight: 10-50 parts of grease polyol; 10-50 parts of polyether polyol; 35-60 parts of a heat conducting filler; 5-15 parts of modified bentonite; 1-5 parts of an adhesion promoter; 0.001 to 0.1 part of catalyst; 5-15 parts of flame retardant; the isocyanate-terminated polymer is prepared from isocyanate and a second polyether polyol. The bi-component polyurethane pouring sealant provided by the invention has high flowing property and excellent anti-sedimentation property.

Description

Double-component polyurethane pouring sealant and preparation method and application thereof
Technical Field
The invention belongs to the technical field of binders, and particularly relates to a bi-component polyurethane pouring sealant, a preparation method and application thereof.
Background
Along with the continuous enhancement of environmental awareness, the attention to new energy automobiles is gradually raised. The overall performance of new energy automobiles depends largely on the performance of their motors, batteries and electrical controls, with thermal management being a major issue. At present, most of the power batteries of the new energy automobiles are lithium ion batteries, and the lithium ion batteries in the automobile battery packs can generate heat in the charging and discharging processes. In order to transfer the heat generated by the battery to the cooling system of the battery pack, a heat conductive material is required. The battery pack has a compact battery assembly structure, small gaps between the batteries, and excellent fluidity of the heat conducting material before solidification is required, so that the gaps of the batteries are filled. In addition, the battery pack is inevitably subjected to vibration during the running of the automobile, and thus the heat conductive material is required to have excellent adhesion property and shock absorption.
The heat conduction pouring sealant is a heat management material which is widely applied to new energy electric automobiles at present. The heat-conducting pouring sealant mainly comprises three categories of epoxy heat-conducting pouring sealant, polyurethane heat-conducting pouring sealant and organic silicon heat-conducting pouring sealant; the epoxy heat conduction pouring sealant has the characteristics of poor toughness, easiness in cracking, cold and hot shock resistance, low hardness and low bonding strength, and the polyurethane pouring sealant has the characteristics of adjustable hardness, moderate bonding strength, high elasticity, high impact resistance, high wear resistance, excellent low temperature resistance and the like, so that the polyurethane heat conduction pouring sealant is more and more widely used in new energy batteries. At present, a 55 gallon vat or even a ton package type bi-component polyurethane pouring sealant is used on site of a customer, and due to the high liquid level, sedimentation of the heat conducting filler becomes a main technical problem which puzzles the polyurethane pouring sealant.
Many technicians solve the problem of settlement of the bi-component polyurethane pouring sealant by adding rheological additives such as gas-phase white carbon black, but the addition of the rheological additives leads to remarkable change of the flowing performance of the polyurethane pouring sealant, so that the small gap position cannot be filled, and even the flow cannot be leveled.
Therefore, the polyurethane pouring sealant with high flowing property and excellent anti-sedimentation performance is provided, and the polyurethane pouring sealant becomes a problem to be solved in the application field of the double-component polyurethane heat-conducting pouring sealant.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a bi-component polyurethane pouring sealant, and a preparation method and application thereof. The bi-component polyurethane pouring sealant provided by the invention has the advantages of high flowing property, excellent anti-sedimentation property, good flame retardant effect and long operable time, and can be used for pouring and sealing related components of new energy automobiles.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a two-component polyurethane potting adhesive comprising a component a and a component B;
the component A is isocyanate-terminated polymer;
the component B comprises the following components in parts by weight:
The isocyanate-terminated polymer is prepared from isocyanate and a second polyether polyol.
The double-component polyurethane pouring sealant provided by the invention comprises a component A and a component B, wherein the component A is isocyanate-terminated polymer; the component B comprises a combination of grease polyol, polyether polyol, heat conducting filler, modified bentonite, an adhesion promoter, a catalyst and a flame retardant in a specific part; by adopting the component A and the component B for matching, and adding the specific component A and the specific modified bentonite into the component B, the obtained double-component polyurethane pouring sealant has high flowing property and excellent anti-sedimentation property.
In the invention, the amount of the grease polyol used in the component B may be 10 parts, 13 parts, 15 parts, 18 parts, 20 parts, 23 parts, 25 parts, 28 parts, 30 parts, 33 parts, 35 parts, 38 parts, 40 parts, 43 parts, 45 parts, 48 parts, 50 parts, etc. in parts by weight.
In the present invention, the polyether polyol may be used in an amount of 10 parts, 13 parts, 15 parts, 18 parts, 20 parts, 23 parts, 25 parts, 28 parts, 30 parts, 33 parts, 35 parts, 38 parts, 40 parts, 43 parts, 45 parts, 48 parts, 50 parts, etc. in terms of parts by weight of the B component.
In the present invention, the B component may be used in an amount of 35 parts, 38 parts, 40 parts, 43 parts, 45 parts, 48 parts, 50 parts, 53 parts, 55 parts, 58 parts, 60 parts, etc. by weight.
In the invention, the component B can be used in an amount of 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts and the like by weight.
In the invention, the component B can be used in an amount of 1 part, 2 parts, 3 parts, 4 parts, 5 parts, etc. by weight.
In the present invention, the B component may be used in an amount of 0.001 parts, 0.003 parts, 0.005 parts, 0.008 parts, 0.01 parts, 0.03 parts, 0.05 parts, 0.08 parts, 0.1 parts, etc. in terms of parts by weight.
In the invention, the B component can be used in an amount of 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, etc. by weight.
Preferably, the isocyanate comprises any one or a combination of at least two of toluene diisocyanate, isophorone diisocyanate or diphenylmethane diisocyanate.
Preferably, the second polyether polyol comprises a polyether diol and/or a polyether triol.
Preferably, the second polyether polyol has a hydroxyl value of 20 to 300mgKOH/g, such as 20mgKOH/g、50mgKOH/g、80mgKOH/g、100mgKOH/g、130mgKOH/g、150mgKOH/g、180mgKOH/g、200mgKOH/g、230mgKOH/g、250mgKOH/g、280mgKOH/g、300mgKOH/g or the like.
Preferably, the isocyanate-terminated polymer has an R value of greater than 2.5.
Preferably, the isocyanate-terminated polymer is prepared by a process comprising: and reacting the second polyether polyol with isocyanate to obtain the isocyanate-terminated polymer.
Preferably, the temperature of the reaction is 60 to 80 ℃, for example 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and the like.
Preferably, the reaction time is 1 to 3 hours, for example 1 hour, 2 hours, 3 hours, etc.
Preferably, the reaction is carried out under vacuum.
Preferably, the isocyanate-terminated polymer is prepared from a raw material further comprising any one or a combination of at least two of a diluent, a plasticizer or a flame retardant.
Preferably, the modified bentonite is an organoaluminum modified bentonite.
Preferably, the modification process comprises at least two heat treatments; the temperature of the first heat treatment is 50-150 ℃ (such as 50 ℃, 60 ℃, 70 ℃, 80 ℃,90 ℃, 100 ℃, 110 ℃,120 ℃, 130 ℃, 140 ℃, 150 ℃ and the like), and the time of the first heat treatment is at least 2h (such as 2h, 2.5h, 3h, 3.5h, 4h and the like); the temperature of the second heat treatment is 100-200deg.C (e.g. 100deg.C, 110deg.C, 120deg.C, 130deg.C, 140deg.C, 150deg.C, 160deg.C, 180deg.C, 190 deg.C, 200deg.C, etc.), and the time of the second heat treatment is at least 2h (e.g. 2h, 2.5h, 3h, 3.5h, 4h, etc.).
Preferably, the first heat treatment is carried out with a solution of an organoaluminum compound and a nonpolar solvent.
Preferably, the organoaluminum compound is selected from any one or a combination of at least two of diisopropyl (acetoacetate) aluminate, diisopropyl (acetylacetonate) aluminate, isopropyl distearoyl oxy aluminate.
Preferably, the nonpolar solvent is selected from at least one of toluene, benzene, carbon tetrachloride, methylene chloride, and ethyl chloride.
Preferably, the mass concentration of the organoaluminum compound in the solution composed of the nonpolar solvent is 1 to 10%, for example, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, etc.
Preferably, the second stage heat treatment is performed under an air atmosphere.
Preferably, the bentonite comprises any one or a combination of at least two of sodium bentonite, calcium bentonite and active bentonite.
Preferably, the bentonite has a mesh number greater than 300 mesh, such as 400 mesh, 600 mesh, 800 mesh, 1000 mesh, 1200 mesh, 1600 mesh, etc.
Preferably, the fat polyol comprises any one or a combination of at least two of cashew nut shell oil modified polyol, castor oil modified polyol, soybean oil modified polyol or palm oil modified polyol.
Preferably, the functionality of the fat polyol is from 2 to 3, such as 2, 2.2, 2.4, 2.6, 2.8, 3, etc.
Preferably, the hydroxyl value of the fat polyol is 100 to 300mgKOH/g, for example, 100mgKOH/g, 130mgKOH/g, 150mgKOH/g, 180mgKOH/g, 200mgKOH/g, 230mgKOH/g, 250mgKOH/g, 280mgKOH/g, 300mgKOH/g, etc.
Preferably, the polyether polyol comprises polypropylene oxide ether diol and/or polypropylene oxide ether triol.
Preferably, the polyether polyol has a hydroxyl value of 20 to 120mgKOH/g, for example, 20mgKOH/g, 40mgKOH/g, 60mgKOH/g, 80mgKOH/g, 100mgKOH/g, 120mgKOH/g, etc.
Preferably, the heat conductive filler includes any one or a combination of at least two of aluminum hydroxide, magnesium hydroxide, aluminum oxide, magnesium oxide, or silicon nitride.
Preferably, the D90 particle size of the thermally conductive filler is < 20 μm, e.g., 18 μm, 16 μm, 14 μm, 12 μm, etc.
Preferably, the raw materials for preparing the adhesion promoter comprise aminophenylsilane and a silane modifier.
Preferably, the aminophenylsilane comprises any one or a combination of at least two of N-phenyl-gamma-aminopropyl trimethoxysilane, N-phenyl-gamma-aminopropyl triethoxysilane, N-phenylaminomethyl trimethoxysilane or N-phenylaminomethyl triethoxysilane.
Preferably, the silane modifier comprises any one or a combination of at least two of o-tolylglycidyl ether, p-tolylglycidyl ether, phenyl glycidyl ether, trityl- (S) -glycidyl ether or resorcinol diglycidyl ether.
Preferably, the molar ratio of secondary amino groups in the aminophenylsilane to glycidyl ether groups in the silane modifier is 1 (0.5 to 1.5), such as 1:0.5, 1:0.8, 1:1, 1:1.2, 1:1.3, 1:1.5, etc.
Preferably, the adhesion promoter is prepared by a process comprising: reacting the aminophenylsilane with a silane modifier to obtain the adhesion promoter.
Preferably, the temperature of the reaction is 30 to 70 ℃, for example 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, etc.
Preferably, the reaction time is 1 to 3 hours, for example 1 hour, 2 hours, 3 hours, etc.
Preferably, the catalyst comprises any one or a combination of at least two of bismuth neodecanoate, bismuth laurate, bismuth isooctanoate or bismuth naphthenate.
Preferably, the flame retardant comprises any one or a combination of at least two of triisopropylphenyl phosphate, tricresyl phosphate and toluenediphenyl phosphate.
Preferably, the mass ratio of the A component to the B component is (10-50): 100, such as 12:100、14:100、16:100、18:100、20:100、22:100、24:100、26:100、28:100、30:100、32:100、34:100、36:100、38:100、40:100、42:100、44:100、46:100、48:100、50:100, etc.
Preferably, the viscosity of the a-component is 200 to 2000 mPa-s, for example 250 mPa-s, 400 mPa-s, 600 mPa-s, 800 mPa-s, 1000 mPa-s, 1200 mPa-s, 1400 mPa-s, 1600 mPa-s, 1800 mPa-s, 1900 mPa-s, etc.
Preferably, the viscosity of the B component is 2000 to 6000 mPa-s, for example 2500 mPa-s, 3000 mPa-s, 3500 mPa-s, 4000 mPa-s, 4500 mPa-s, 5000 mPa-s or 5500 mPa-s, etc.
In a second aspect, the present invention provides a method for preparing the two-component polyurethane pouring sealant according to the first aspect, the method comprising the following steps:
1) And (3) preparation of the component A: dehydrating the second polyether polyol and an optional flame retardant, adding isocyanate for polymerization, and cooling to obtain a component A;
2) Preparation of modified bentonite: dispersing bentonite in a solution composed of an organic aluminum compound and a nonpolar solvent, performing first-stage heat treatment, filtering, and performing second-stage heat treatment to obtain the modified bentonite;
3) Preparation of the adhesion promoter: reacting the aminophenylsilane with a silane modifier to obtain the adhesion promoter;
4) And (3) preparation of a component B: mixing grease polyol, polyether polyol, heat conducting filler, modified bentonite and flame retardant according to the formula amount, vacuum dehydrating, adding a catalyst and an adhesion promoter, and stirring to obtain a component B;
5) And mixing the component A and the component B to obtain the bi-component polyurethane pouring sealant.
In a third aspect, the invention provides an application of the two-component polyurethane pouring sealant in the pouring of related components of a new energy automobile.
Compared with the prior art, the invention has at least the following beneficial effects:
The double-component polyurethane pouring sealant provided by the invention comprises a component A and a component B, wherein the component A is isocyanate-terminated polymer; the component B comprises a combination of grease polyol, polyether polyol, heat conducting filler, modified bentonite, an adhesion promoter, a catalyst and a flame retardant in a specific part; by adopting the component A and the component B for matching, and adding the specific component A and the specific modified bentonite into the component B, the obtained double-component polyurethane pouring sealant has high flowing property and excellent anti-sedimentation property.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Preparation example 1
A preparation method of the modified bentonite comprises the following steps:
Mixing 500g of 1000-mesh sodium bentonite and 2000g of toluene uniformly, heating to 120 ℃, adding 40g of diisopropyl (acetylacetonate) aluminate, and stirring for 2.5h; and then filtering and drying for 4 hours in a 150-DEG C oven to obtain the modified bentonite.
Preparation example 2
A preparation method of the modified bentonite comprises the following steps:
600g of 1400-mesh calcium bentonite and 3000g of toluene are uniformly mixed, then the mixture is heated to 110 ℃, 50g of isopropyl distearyl acyloxy aluminate is added, and the mixture is stirred for 5 hours; and then filtering and drying for 3 hours in a 160-DEG C oven to obtain the modified bentonite.
Preparation example 3
A preparation method of the modified bentonite comprises the following steps:
Uniformly mixing 600g of 1600-mesh active bentonite with 2500g of carbon tetrachloride, heating to 140 ℃, adding 100g of diisopropyl (acetoacetate) aluminate, and stirring for 3h; and then filtering and drying for 3 hours in a 120-DEG C oven to obtain the modified bentonite.
Preparation example 4
A preparation method of the modified bentonite comprises the following steps:
Uniformly mixing 600g of 1600-mesh active bentonite with 2500g of carbon tetrachloride, heating to 140 ℃, adding 100g of mercaptopropyl trimethoxysilane, and stirring for 3h; and then filtering and drying for 3 hours in a 120-DEG C oven to obtain the modified bentonite.
Preparation example 5
An isocyanate-terminated polymer, prepared by a process comprising:
200g of a difunctional polyether polyol DL400, 600g of a trifunctional polyether polyol PPG3000 and 400g of triisopropylphenyl phosphate are dehydrated in vacuum at 100 ℃ for 3 hours, then cooled to 70 ℃, 600g of toluene diisocyanate is added and stirred for 2 hours to obtain an isocyanate-terminated polymer.
Preparation example 6
An isocyanate-terminated polymer, prepared by a process comprising:
600g of trifunctional polyether polyol PPG3000 and 400g of triisopropylphenyl phosphate are dehydrated in vacuum at 100 ℃ for 3 hours, then cooled to 70 ℃, 400g of toluene diisocyanate is added and stirred for 2 hours to obtain the isocyanate-terminated polymer.
Preparation example 7
An isocyanate-terminated polymer, prepared by a process comprising:
200g of difunctional polyether polyol DL400, 1000g of trifunctional polyether polyol PPG5000 and 400g of diisononyl phthalate are dehydrated in vacuum at 130 ℃ for 1.5h, then cooled to 65 ℃, 900g of diphenylmethane diisocyanate is added and stirred for 2.5h, and an isocyanate-terminated polymer is obtained.
Preparation example 8
An adhesion promoter, the preparation method of which comprises:
heating 250g N-phenyl-gamma-aminopropyl trimethoxysilane to 40 ℃, slowly adding 164g of o-tolyl glycidyl ether while stirring, and continuing stirring for 30min after the addition to obtain the adhesion promoter.
Preparation example 9
An adhesion promoter, the preparation method of which comprises:
269-g N-phenylaminomethyl triethoxysilane is taken, heated to 50 ℃, 120g of resorcinol diglycidyl ether is slowly added while stirring, and stirring is continued for 20min after the addition is completed, so that the adhesion promoter is obtained.
Preparation example 10
An adhesion promoter, the preparation method of which comprises:
342g of bis- (gamma-trimethoxysilylpropyl) amine is taken and heated to 50 ℃, 70g of diglycidyl ether is slowly added while stirring, and stirring is continued for 20min after the addition is completed, so that the adhesion promoter is obtained.
Example 1
In the embodiment, a two-component polyurethane pouring sealant is provided, which consists of a component A and a component B;
Wherein, the A component is isocyanate-terminated polymer (preparation 5);
the preparation method of the component B comprises the following steps: 220g of castor oil modified polyol A32 (Shanghai smart day), 100g of polyether polyol DL2000, 470g of aluminum hydroxide heat conduction filler HVF3, 100g of modified bentonite (preparation example 1) and 80g of triisopropylphosphate are stirred for 2 hours at 120 ℃ in vacuum, then cooled to 60 ℃, 30g of adhesion promoter (preparation example 8) and 0.1g of bismuth laurate catalyst are added, stirred for 30 minutes, cooled and discharged to obtain a component B.
The preparation method of the bi-component polyurethane pouring sealant provided by the embodiment comprises the following steps: the mass ratio is 25:100 and the component A and the component B are mixed to obtain the bi-component polyurethane pouring sealant.
Example 2
In the embodiment, a two-component polyurethane pouring sealant is provided, which consists of a component A and a component B;
Wherein, the A component is isocyanate-terminated polymer (preparation 6);
The preparation method of the component B comprises the following steps: 220g of refined castor oil polyol C010 (Shanghai smart day), 100g of polyether polyol DL2000, 500g of aluminum hydroxide heat conduction filler HVF3, 80g of modified bentonite (preparation example 2) and 70g of triisopropylphosphate are stirred for 2.5 hours at 120 ℃ in vacuum, then cooled to 60 ℃, 30g of adhesion promoter (preparation example 9) and 0.1g of bismuth isooctanoate catalyst are added, stirred for 40 minutes, cooled and discharged to obtain the component B.
The preparation method of the bi-component polyurethane pouring sealant provided by the embodiment comprises the following steps: the mass ratio is 25:100 and the component A and the component B are mixed to obtain the bi-component polyurethane pouring sealant.
Example 3
In the embodiment, a two-component polyurethane pouring sealant is provided, which consists of a component A and a component B;
Wherein, the A component is isocyanate-terminated polymer (preparation 7);
the preparation method of the component B comprises the following steps: 240g of castor oil modified polyol A32 (Shanghai smart day), 150g of polyether polyol 330N, 400g of aluminum hydroxide heat conduction filler HVF3, 120g of modified bentonite (preparation example 3) and 70g of tricresyl phosphate are stirred for 2 hours at 120 ℃ in vacuum, then cooled to 60 ℃,20 g of a promoter adhesive (preparation example 9) and 0.1g of bismuth naphthenate catalyst are added, stirred for 30 minutes, cooled and discharged to obtain a component B.
The preparation method of the bi-component polyurethane pouring sealant provided by the embodiment comprises the following steps: the mass ratio is 35:100 and the component A and the component B are mixed to obtain the bi-component polyurethane pouring sealant.
Example 4
In the embodiment, a two-component polyurethane pouring sealant is provided, which consists of a component A and a component B;
Wherein, the A component is isocyanate-terminated polymer (preparation 7);
The preparation method of the component B comprises the following steps: 240g of soybean oil modified polyol HM13150 (sea-modified polyethylene), 150g of polyether polyol 330N, 400g of aluminum hydroxide heat-conducting filler HVF3, 120g of modified bentonite (preparation example 3) and 70g of tricresyl phosphate are stirred for 2 hours at 120 ℃ in vacuum, then cooled to 60 ℃,20 g of a promoter binder (preparation example 9) and 0.1g of bismuth naphthenate catalyst are added, stirred for 30 minutes, cooled and discharged to obtain a component B.
The preparation method of the bi-component polyurethane pouring sealant provided by the embodiment comprises the following steps: the mass ratio is 35:100 and the component A and the component B are mixed to obtain the bi-component polyurethane pouring sealant.
Example 5
In the embodiment, a two-component polyurethane pouring sealant is provided, which consists of a component A and a component B;
Wherein, the A component is isocyanate-terminated polymer (preparation 7);
The preparation method of the component B comprises the following steps: 180g of cashew nut shell oil modified polyol NX-5825 (Cardley), 250g of polyether polyol 330N, 380g of aluminum hydroxide heat conduction filler HVF3, 120g of modified bentonite (preparation example 3) and 70g of tricresyl phosphate are stirred for 2.5 hours at 110 ℃, then cooled to 60 ℃,20 g of adhesion promoter (preparation example 9) and 0.1g of bismuth naphthenate catalyst are added, stirred for 30 minutes, cooled and discharged to obtain the component B.
The preparation method of the bi-component polyurethane pouring sealant provided by the embodiment comprises the following steps: the mass ratio is 35:100 and the component A and the component B are mixed to obtain the bi-component polyurethane pouring sealant.
Example 6
In the embodiment, a two-component polyurethane pouring sealant is provided, which consists of a component A and a component B;
Wherein, the A component is isocyanate-terminated polymer (preparation 5);
The preparation method of the component B comprises the following steps: 220g of castor oil modified polyol A32 (Shanghai smart day), 100g of polyether polyol DL1000, 470g of aluminum hydroxide heat conduction filler HVF3, 100g of modified bentonite (preparation example 2) and 80g of triisopropylphosphate are stirred for 2 hours at 120 ℃ in vacuum, then cooled to 60 ℃, 30g of adhesion promoter (preparation example 9) and 0.1g of bismuth laurate catalyst are added, stirred for 30 minutes, cooled and discharged to obtain a component B.
The preparation method of the bi-component polyurethane pouring sealant provided by the embodiment comprises the following steps: the mass ratio is 25:100 and the component A and the component B are mixed to obtain the bi-component polyurethane pouring sealant.
Comparative example 1
This comparative example differs from example 1 only in that the amount of modified bentonite used was 25g.
Comparative example 2
This comparative example differs from example 1 only in that the amount of modified bentonite used was 250g.
Comparative example 3
This comparative example differs from example 1 only in that the modified bentonite was replaced with an equal weight of sodium bentonite.
Comparative example 4
This comparative example differs from example 1 only in that the modified bentonite was replaced with the modified bentonite provided in preparation example 4.
Comparative example 5
This comparative example differs from example 1 only in that the isocyanate-terminated polymer was replaced with polyphenyl polymethylene isocyanate PM200.
Comparative example 6
This comparative example differs from example 1 only in that the adhesion promoter is replaced with the adhesion promoter in preparation 10.
The performance test is carried out on the two-component polyurethane pouring sealant provided in the examples and the comparative examples, and the test method is as follows:
Viscosity: the test is carried out according to the GB/T2794-2013 rule and the test is carried out under the condition of 25-75% torque range.
Mixing viscosity: mixing A, B components (total amount 100 g) according to a certain proportion, repeatedly stirring for 5min in different directions, and then testing viscosity according to GB/T2794-2013, namely the viscosity after mixing.
Settleability (upper layer viscosity after 90 days): the component B after 90 days of storage is taken and the upper layer is tested according to the GB/T2794-2013 rule.
The results of the performance test are shown in Table 1.
TABLE 1
As can be seen from Table 1, the two-component polyurethane pouring sealant provided by the invention has high flowing property (mixed viscosity: 2100-2600 mPa.s) and excellent anti-sedimentation property (viscosity after storage: 4500-5250 mPa.s), and the viscosity of the two-component polyurethane pouring sealant is not greatly different from that of the component B before storage.
Compared with the example 1, the two-component polyurethane pouring sealant provided in the comparative example 1 has high flowing property, but the anti-sedimentation property is obviously reduced, and the viscosity of the component B is obviously reduced after storage; the drooling property of the two-component polyurethane pouring sealant provided in comparative example 2 is obviously deteriorated; the two-component polyurethane pouring sealant provided in comparative example 3 and comparative example 4 has reduced drooling and anti-settling properties.
Compared with example 1, the mixing viscosity of the two-component polyurethane pouring sealant provided in comparative example 5 is obviously increased, and the sagging property is reduced.
The two-component polyurethane potting adhesive of comparative example 6 was reduced in both of the drooling property and the anti-settling property as compared with example 1.
The applicant states that the present invention is illustrated by the above examples as well as the preparation method and application thereof, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be practiced by relying on the above examples. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.

Claims (10)

1. The double-component polyurethane pouring sealant is characterized by comprising a component A and a component B;
the component A is isocyanate-terminated polymer;
the component B comprises the following components in parts by weight:
The isocyanate-terminated polymer is prepared from isocyanate and a second polyether polyol.
2. The two-component polyurethane potting adhesive of claim 1, wherein the isocyanate comprises any one or a combination of at least two of toluene diisocyanate, isophorone diisocyanate, or diphenylmethane diisocyanate;
Preferably, the second polyether polyol comprises a polyether diol and/or a polyether triol;
Preferably, the second polyether polyol has a hydroxyl value of 20 to 300mgKOH/g;
preferably, the isocyanate-terminated polymer has an R value of greater than 2.5;
preferably, the isocyanate-terminated polymer is prepared from a raw material further comprising any one or a combination of at least two of a diluent, a plasticizer or a flame retardant.
3. The two-component polyurethane potting adhesive of claim 1 or 2, wherein the modified bentonite is an organoaluminum modified bentonite;
Preferably, the modification process comprises at least two heat treatments; the temperature of the first heat treatment is 50-150 ℃, and the time of the first heat treatment is at least 2h; the temperature of the second heat treatment is 100-200 ℃, and the time of the second heat treatment is at least 2h;
Preferably, the first heat treatment is performed by using a solution composed of an organic aluminum compound and a nonpolar solvent;
preferably, the organoaluminum compound is selected from any one or a combination of at least two of diisopropyl (acetoacetate) aluminate, diisopropyl (acetylacetonate) aluminate, isopropyl distearoyloxy aluminate;
preferably, the nonpolar solvent is selected from at least one of toluene, benzene, carbon tetrachloride, methylene chloride and chloroethane;
Preferably, the mass concentration of the organic aluminum compound in the solution composed of the organic aluminum compound and the nonpolar solvent is 1-10%;
Preferably, the second stage heat treatment is performed under an air atmosphere;
Preferably, the bentonite comprises any one or a combination of at least two of sodium bentonite, calcium bentonite and active bentonite;
Preferably, the bentonite has a mesh number greater than 300 mesh.
4. The two-component polyurethane potting adhesive of any one of claims 1-3, wherein the grease polyol comprises any one or a combination of at least two of cashew nut shell oil modified polyol, castor oil modified polyol, soybean oil modified polyol, or palm oil modified polyol;
Preferably, the functionality of the grease polyol is 2-3;
Preferably, the hydroxyl value of the fat polyol is 100 to 300mgKOH/g;
preferably, the polyether polyol comprises polypropylene oxide ether diol and/or polypropylene oxide ether triol;
preferably, the polyether polyol has a hydroxyl value of 20 to 120mgKOH/g.
5. The two-component polyurethane potting adhesive of any one of claims 1 to 4, wherein the thermally conductive filler comprises any one or a combination of at least two of aluminum hydroxide, magnesium hydroxide, aluminum oxide, magnesium oxide, or silicon nitride;
preferably, the D90 particle size of the thermally conductive filler is < 20 μm.
6. The two-component polyurethane potting adhesive of any one of claims 1 to 5, wherein the raw materials for preparing the adhesion promoter comprise aminophenylsilane and a silane modifier;
Preferably, the aminophenylsilane comprises any one or a combination of at least two of N-phenyl-gamma-aminopropyl trimethoxysilane, N-phenyl-gamma-aminopropyl triethoxysilane, N-phenylaminomethyl trimethoxysilane or N-phenylaminomethyl triethoxysilane;
preferably, the silane modifier comprises any one or a combination of at least two of o-tolylglycidyl ether, p-tolylglycidyl ether, phenyl glycidyl ether, trityl- (S) -glycidyl ether or resorcinol diglycidyl ether;
Preferably, the molar ratio of secondary amino groups in the aminophenylsilane to glycidyl ether groups in the silane modifier is 1 (0.5 to 1.5).
7. The two-component polyurethane potting adhesive of any one of claims 1-6, wherein the catalyst comprises any one or a combination of at least two of bismuth neodecanoate, bismuth laurate, bismuth isooctanoate, or bismuth naphthenate;
Preferably, the flame retardant comprises any one or a combination of at least two of triisopropylphenyl phosphate, tricresyl phosphate and toluenediphenyl phosphate.
8. The two-component polyurethane potting adhesive according to any one of claims 1 to 7, wherein the mass ratio of the a component and the B component is (10 to 50): 100;
preferably, the viscosity of the A component is 200-2000 mPa.s;
Preferably, the viscosity of the B component is 2000-6000 mPas.
9. A method for preparing the two-component polyurethane pouring sealant according to any one of claims 1 to 8, wherein the method comprises the following steps:
1) And (3) preparation of the component A: dehydrating the second polyether polyol and an optional flame retardant, adding isocyanate for polymerization, and cooling to obtain a component A;
2) Preparation of modified bentonite: dispersing bentonite in a solution composed of an organic aluminum compound and a nonpolar solvent, performing first-stage heat treatment, filtering, and performing second-stage heat treatment to obtain the modified bentonite;
3) Preparation of the adhesion promoter: reacting the aminophenylsilane with a silane modifier to obtain the adhesion promoter;
4) Mixing grease polyol, polyether polyol, heat conducting filler, modified bentonite and flame retardant according to the formula amount, vacuum dehydrating, adding a catalyst and an adhesion promoter, and stirring to obtain a component B;
5) And mixing the component A and the component B to obtain the bi-component polyurethane pouring sealant.
10. Use of the two-component polyurethane potting adhesive according to any one of claims 1 to 8 for potting related components of new energy automobiles.
CN202410469351.0A 2024-04-18 2024-04-18 Double-component polyurethane pouring sealant and preparation method and application thereof Pending CN118308062A (en)

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