CN110982466A - Bi-component flexible epoxy pouring sealant and preparation method and application thereof - Google Patents
Bi-component flexible epoxy pouring sealant and preparation method and application thereof Download PDFInfo
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- CN110982466A CN110982466A CN201911295464.9A CN201911295464A CN110982466A CN 110982466 A CN110982466 A CN 110982466A CN 201911295464 A CN201911295464 A CN 201911295464A CN 110982466 A CN110982466 A CN 110982466A
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- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/83—Chemically modified polymers
- C08G18/831—Chemically modified polymers by oxygen-containing compounds inclusive of carbonic acid halogenides, carboxylic acid halogenides and epoxy halides
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08L2203/00—Applications
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- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention discloses a double-component flexible epoxy pouring sealant and a preparation method and application thereof, wherein the double-component flexible epoxy pouring sealant comprises the following components in percentage by weight of 100: 22-27 of a flexible epoxy pouring sealant A component and a flexible epoxy pouring sealant B component, wherein the flexible epoxy pouring sealant A component is prepared from 10-20% of hydroxyl-terminated polyurethane prepolymer, 30-50% of epoxy resin, 5-15% of grease, 10-40% of flame-retardant filler, 5-10% of heat-conducting filler and 0.1-1% of defoaming agent, and the flexible epoxy pouring sealant B component is prepared from 30-70% of carboxyl-terminated polyurethane prepolymer, 30-70% of methylnadic anhydride and 0.1-1% of DMP-30 accelerator. The bi-component flexible epoxy potting adhesive prepared by the invention has good thermal shock resistance after being cured, avoids cracking caused by thermal shock, and has excellent bonding property, waterproof property and moisture resistance.
Description
Technical Field
The invention relates to the technical field of pouring sealant materials, in particular to a two-component flexible epoxy pouring sealant and a preparation method and application thereof.
Background
The pouring sealant is mainly used for bonding, sealing, encapsulating, coating protection and the like of electronic components, can play the roles of moisture prevention, corrosion prevention, shock prevention and dust prevention, can improve the service performance, and is beneficial to the miniaturization and integrity of devices.
At present, the commonly used pouring sealant mainly comprises organic silicon pouring sealant, polyurethane pouring sealant and epoxy pouring sealant. The organosilicon pouring sealant has excellent repair capability due to low viscosity, and can be used for quickly and conveniently taking out, repairing and replacing sealed components; however, they are expensive, have a slightly poor adhesion, and are likely to cause problems such as non-curing due to catalyst poisoning, and thus their use is limited. The polyurethane pouring sealant has excellent low-temperature resistance, and according to the principle that the structure determines the performance, the polyurethane pouring sealant with different performances can be obtained by regulating and controlling the structure of polyurethane. The epoxy pouring sealant has excellent high temperature resistance and electrical insulation capacity, is simple to operate, has stable performance before and after curing, and has excellent adhesive force to various metal substrates and porous substrates. However, the epoxy potting adhesive has poor thermal shock resistance, and is easy to crack after being subjected to thermal shock, so that water vapor permeates into electronic components from the cracks, and the moisture resistance is poor; meanwhile, the cured colloid has high hardness and is brittle, and electronic components are easy to be scratched.
Therefore, how to prepare the flexible epoxy pouring sealant needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a double-component flexible epoxy pouring sealant and a preparation method and application thereof, wherein the double-component flexible epoxy pouring sealant is an epoxy sealant in which a component A and a component B are both modified by polyurethane, and during preparation, a hydroxyl-terminated polyurethane prepolymer is synthesized firstly, and 2,2, 4-trimethyl-1, 3-pentanediol is introduced into the hydroxyl-terminated polyurethane prepolymer to improve the waterproof performance of a system, and then the hydroxyl-terminated polyurethane prepolymer is compounded with epoxy resin to be used as the component A of the epoxy sealant; the carboxyl-terminated polyurethane prepolymer is synthesized by esterification reaction of hydroxyl-terminated polyurethane prepolymer and methyl nadic anhydride, and then the carboxyl-terminated polyurethane prepolymer is compounded with the methyl nadic anhydride to be used as a component B of the epoxy adhesive. The bi-component flexible epoxy pouring sealant is odorless, small in viscosity, good in fluidity, good in waterproof performance, good in flexibility and bonding performance, good in cold and heat shock resistance after the product is cured, and capable of solving the problem of the performance defects of epoxy pouring sealants in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a two-component flexible epoxy pouring sealant, which comprises the following components in percentage by weight of 100: 22-27 of a flexible epoxy pouring sealant A component and a flexible epoxy pouring sealant B component, wherein the flexible epoxy pouring sealant A component is composed of the following raw materials in percentage by weight:
the component B of the flexible epoxy pouring sealant consists of the following raw materials:
30 to 70 percent of carboxyl-terminated polyurethane prepolymer,
30 to 70 percent of methyl nadic anhydride,
0.1 to 1 percent of DMP-30 accelerant.
The introduction of the flexible groups in the hydroxyl-terminated polyurethane prepolymer and the carboxyl-terminated polyurethane prepolymer can well solve the problems of cracking, water seepage and poor moisture resistance of a workpiece in the use process after glue pouring, and the bi-component flexible epoxy pouring sealant integrates the excellent low temperature resistance of polyurethane and the high temperature resistance of epoxy glue, so that the high and low temperature resistance of the bi-component flexible epoxy pouring sealant is realized, and the cold and hot shock resistance of a system is improved. In addition, in the curing process, the polyurethane participates in the curing of the epoxy glue, the epoxy pouring glue is structurally modified, the alkyl flexible group in the polyurethane structure improves the low-temperature resistance of the system, and the carbamate polar group in the polyurethane structure improves the bonding property of the system.
Further, the hydroxyl-terminated polyurethane prepolymer is prepared by synthesizing 68.3% of polyethylene glycol 400, 10% of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7% of isophorone diisocyanate according to weight percentage. The synthetic route of the hydroxyl-terminated polyurethane prepolymer is as follows:
2,2, 4-trimethyl-1, 3-pentanediol is introduced into the hydroxyl-terminated polyurethane prepolymer, and hydroxyl is protected by methyl groups in spatial positions, so that the waterproof performance of the system is improved, and the system has excellent high-temperature and high-humidity resistance.
Further, the carboxyl-terminated polyurethane prepolymer is prepared by synthesizing 41.1% of polyethylene glycol 400, 5% of 2,2, 4-trimethyl-1, 3-pentanediol, 12.8% of isophorone diisocyanate and 41.1% of methyl nadic anhydride according to weight percentage. The synthetic route of the carboxyl-terminated polyurethane prepolymer is as follows:
preferably, the epoxy resin is one or any combination of epoxy resin E51, epoxy resin E44 and vinylcyclohexene dioxide.
Preferably, the grease is one or any combination of castor oil, epoxidized soybean oil and tung oil.
Preferably, the flame-retardant filler is one or any combination of aluminum hydroxide, magnesium hydroxide and melamine pyrophosphate. Preferably, the aluminum hydroxide is powder with 600 meshes to 800 meshes; the magnesium hydroxide is powder with the grain diameter of 1.5-2 mu m, and the whiteness is more than or equal to 95; the melamine pyrophosphate is white fine powder with the particle size of less than 10 mu m.
Preferably, the heat conducting filler is one or any combination of alumina, silica micropowder and calcium carbonate. Preferably, the grain diameter of the alumina is less than or equal to 10 μm; the grain diameter of the silicon micro powder is 2000 meshes; the particle size of the calcium carbonate is 20-500 mu m.
Preferably, the defoaming agent is a 6800 defoaming agent or a BYK A555 defoaming agent.
In a second aspect, the invention provides a preparation method of the bi-component flexible epoxy pouring sealant, which comprises the following steps:
(1) synthesizing a hydroxyl-terminated polyurethane prepolymer: adding polyethylene glycol 400, 2, 4-trimethyl-1, 3-pentanediol and isophorone diisocyanate into a four-neck flask with nitrogen introduced in sequence, stirring and heating at a rotating speed of 50 r/min-200 r/min to 60 ℃, and when the content of NCO is less than 5%, reacting to reach the end point, thus synthesizing the hydroxyl-terminated polyurethane prepolymer for later use;
(2) synthesizing a carboxyl-terminated polyurethane prepolymer: sequentially adding polyethylene glycol 400, 2, 4-trimethyl-1, 3-pentanediol and isophorone diisocyanate into a four-neck flask into which nitrogen is introduced, reacting for 2 hours at 60 ℃, adding methyl nadic anhydride into a system when the content of NCO is less than 5%, stirring and heating to 60 ℃ at the rotating speed of 50 r/min-200 r/min, and synthesizing to obtain carboxyl-terminated polyurethane when the acid value is less than 400mgKOH/g and the reaction is finished for later use;
(3) preparing a component A of the flexible epoxy pouring sealant: uniformly stirring and mixing the hydroxyl-terminated polyurethane prepolymer prepared in the step (1) with epoxy resin, grease, flame-retardant filler, heat-conducting filler and defoamer at a rotating speed of 600 r/min-1000 r/min to obtain a component A of the flexible epoxy pouring sealant;
(4) preparing a component B of the flexible epoxy pouring sealant: uniformly stirring and mixing the carboxyl-terminated polyurethane prepolymer prepared in the step (2) with methyl nadic anhydride and DMP-30 accelerator at the rotating speed of 30 r/min-600 r/min to obtain a component B of the flexible epoxy pouring sealant;
(5) preparing a double-component flexible epoxy pouring sealant: and (4) stirring and uniformly mixing the component A of the flexible epoxy pouring sealant obtained in the step (3) and the component B of the flexible epoxy pouring sealant obtained in the step (4) at the rotating speed of 30-600 r/min to obtain the double-component flexible epoxy pouring sealant.
In the step (1), the stirring speed is preferably 100 r/min; in the step (2), the stirring speed is preferably 150 r/min; in the step (3), the stirring speed is preferably 800 r/min; in the step (4), the stirring speed is preferably 400 r/min; in step (5), the stirring speed is preferably 400 r/min. The polyurethane prepolymer is synthesized by a simple process, the process is simple, and industrialization is convenient to realize.
In a third aspect, the invention also provides an application of the two-component flexible epoxy pouring sealant in preparation of electronic component sealing.
The bi-component flexible epoxy pouring sealant disclosed by the invention has good thermal shock resistance after being cured, and is suitable for common or vacuum pressure impregnation treatment of H, C-grade motors and electrical appliances. Specifically, the prepared two-component flexible epoxy pouring sealant can be applied to a feedthrough capacitor device, such as a feedthrough capacitor of a microwave oven. During storage, the component A of the flexible epoxy pouring sealant and the component B of the flexible epoxy pouring sealant are separately stored; when the flexible epoxy pouring sealant is required to be used, the component A of the flexible epoxy pouring sealant and the component B of the flexible epoxy pouring sealant are stirred, mixed uniformly and cured.
Compared with the prior art, the invention provides a bi-component flexible epoxy pouring sealant and a preparation method and application thereof, and the bi-component flexible epoxy pouring sealant has the following beneficial effects:
(1) compared with the common epoxy pouring sealant, the epoxy pouring sealant has the advantages of long storage period, quick curing, no odor, no toxicity, convenient operation, less volatilization during curing, environmental protection and the like, overcomes the problem that water vapor is easy to crack after being subjected to cold and heat shock and permeates into electronic components from the cracks, and has excellent bonding performance, waterproof performance and moisture resistance.
(2) The environment is protected, and the system has no other small molecules except water vapor, so that the environment is really protected.
Detailed Description
The technical solutions of the present invention will be described clearly and completely by the detailed embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following examples are in weight percent unless otherwise indicated.
Example 1
The embodiment 1 provides a two-component flexible epoxy pouring sealant, which comprises the following components in percentage by weight of 100: 25 and a flexible epoxy pouring sealant B, wherein the flexible epoxy pouring sealant A consists of the following raw materials:
the component B of the flexible epoxy pouring sealant consists of the following raw materials:
40 percent of carboxyl-terminated polyurethane prepolymer,
59.5 percent of methyl nadic anhydride,
0.5 percent of DMP-30 accelerant;
wherein the hydroxyl-terminated polyurethane prepolymer is prepared by synthesizing 68.3 percent of polyethylene glycol 400, 10 percent of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7 percent of isophorone diisocyanate. The carboxyl-terminated polyurethane prepolymer is prepared by synthesizing 41.1 percent of polyethylene glycol 400, 5 percent of 2,2, 4-trimethyl-1, 3-pentanediol, 12.8 percent of isophorone diisocyanate and 41.1 percent of methyl nadic anhydride. The aluminum hydroxide is 600-800 meshes of powder; the grain size of the silicon micropowder is 2000 meshes.
The preparation method of the double-component flexible epoxy pouring sealant comprises the following steps:
(1) synthesizing a hydroxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 68.3% of polyethylene glycol 400, 10% of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7% of isophorone diisocyanate, stirring and heating to 60 ℃ at a rotating speed of 100r/min, finally judging the reaction process by testing the content of NCO, when the content of NCO is less than 5%, the reaction reaches the end point, namely synthesizing to obtain a hydroxyl-terminated polyurethane prepolymer, and discharging for later use;
(2) synthesizing a carboxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 41.1% of polyethylene glycol 400, 5% of 2,2, 4-trimethyl-1, 3-pentanediol and 12.8% of isophorone diisocyanate, reacting for 2 hours at 60 ℃, adding 41.1% of methyl nadic anhydride into the system when the content of NCO is less than 5%, stirring and heating to 60 ℃ at the rotating speed of 150r/min, finally judging the reaction process through the change of acid value, when the acid value is less than 400mgKOH/g, reaching the end point of the reaction, synthesizing to obtain a carboxyl-terminated polyurethane prepolymer, and discharging for later use;
(3) preparing a component A of the flexible epoxy pouring sealant: stirring and mixing 10% of the hydroxyl-terminated polyurethane prepolymer prepared in the step (1) with 39.5% of epoxy resin E44, 10% of vinylcyclohexene dioxide, 10% of castor oil, 25% of aluminum hydroxide, 5% of silicon micropowder and 0.5% of moderate 6800 defoamer uniformly at a rotating speed of 800r/min to prepare a component A of the flexible epoxy pouring sealant, and discharging for later use;
(4) preparing a component B of the flexible epoxy pouring sealant: uniformly stirring and mixing 40% of the carboxyl-terminated polyurethane prepolymer prepared in the step (2), 59.5% of methyl nadic anhydride and 0.5% of DMP-30 accelerator at a rotating speed of 400r/min to obtain a component B of the flexible epoxy pouring sealant, and discharging for later use;
(5) preparing a double-component flexible epoxy pouring sealant: according to the weight ratio of 100: and 25, stirring and uniformly mixing the component A of the flexible epoxy pouring sealant obtained in the step (3) and the component B of the flexible epoxy pouring sealant obtained in the step (4) at the rotating speed of 400r/min to obtain the double-component flexible epoxy pouring sealant.
During encapsulation, the prepared two-component flexible epoxy pouring sealant is heated and cured.
Example 2
The embodiment 2 provides a two-component flexible epoxy pouring sealant, which comprises the following components in percentage by weight of 100: 25 and a flexible epoxy pouring sealant B, wherein the flexible epoxy pouring sealant A consists of the following raw materials:
the component B of the flexible epoxy pouring sealant consists of the following raw materials:
30 percent of carboxyl-terminated polyurethane prepolymer,
69.5 percent of methyl nadic anhydride,
0.5 percent of DMP-30 accelerant;
wherein the hydroxyl-terminated polyurethane prepolymer is prepared by synthesizing 68.3 percent of polyethylene glycol 400, 10 percent of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7 percent of isophorone diisocyanate. The carboxyl-terminated polyurethane prepolymer is prepared by synthesizing 41.1 percent of polyethylene glycol 400, 5 percent of 2,2, 4-trimethyl-1, 3-pentanediol, 12.8 percent of isophorone diisocyanate and 41.1 percent of methyl nadic anhydride. The magnesium hydroxide is powder with the grain diameter of 1.5-2 mu m, and the whiteness is more than or equal to 95; the particle size of the calcium carbonate is 20-500 mu m.
The preparation method of the double-component flexible epoxy pouring sealant comprises the following steps:
(1) synthesizing a hydroxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 68.3% of polyethylene glycol 400, 10% of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7% of isophorone diisocyanate, stirring and heating to 60 ℃ at a rotating speed of 100r/min, finally judging the reaction process by testing the content of NCO, when the content of NCO is less than 5%, the reaction reaches the end point, namely synthesizing to obtain a hydroxyl-terminated polyurethane prepolymer, and discharging for later use;
(2) synthesizing a carboxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 41.1% of polyethylene glycol 400, 5% of 2,2, 4-trimethyl-1, 3-pentanediol and 12.8% of isophorone diisocyanate, reacting for 2 hours at 60 ℃, adding 41.1% of methyl nadic anhydride into the system when the content of NCO is less than 5%, stirring and heating to 60 ℃ at the rotating speed of 150r/min, finally judging the reaction process through the change of acid value, when the acid value is less than 400mgKOH/g, reaching the end point of the reaction, synthesizing to obtain a carboxyl-terminated polyurethane prepolymer, and discharging for later use;
(3) preparing a component A of the flexible epoxy pouring sealant: stirring and mixing 20% of the hydroxyl-terminated polyurethane prepolymer prepared in the step (1) with 30% of epoxy resin E51, 10% of epoxidized soybean oil, 34.5% of magnesium hydroxide, 5% of calcium carbonate and 0.5% of BYKA555 defoamer uniformly at a rotating speed of 800r/min to obtain a component A of the flexible epoxy pouring sealant, and discharging for later use;
(4) preparing a component B of the flexible epoxy pouring sealant: uniformly stirring and mixing 30% of the carboxyl-terminated polyurethane prepolymer prepared in the step (2), 69.5% of methyl nadic anhydride and 0.5% of DMP-30 accelerator at a rotating speed of 400r/min to obtain a component B of the flexible epoxy pouring sealant, and discharging for later use;
(5) preparing a double-component flexible epoxy pouring sealant: according to the weight ratio of 100: and 25, stirring and uniformly mixing the component A of the flexible epoxy pouring sealant obtained in the step (3) and the component B of the flexible epoxy pouring sealant obtained in the step (4) at the rotating speed of 400r/min to obtain the double-component flexible epoxy pouring sealant.
During encapsulation, the prepared two-component flexible epoxy pouring sealant is heated and cured.
Example 3
The embodiment 3 provides a two-component flexible epoxy pouring sealant, which comprises the following components in percentage by weight of 100: 25 and a flexible epoxy pouring sealant B, wherein the flexible epoxy pouring sealant A consists of the following raw materials:
the component B of the flexible epoxy pouring sealant consists of the following raw materials:
50 percent of carboxyl-terminated polyurethane prepolymer,
49.5 percent of methyl nadic anhydride,
0.5 percent of DMP-30 accelerant;
wherein the hydroxyl-terminated polyurethane prepolymer is prepared by synthesizing 68.3 percent of polyethylene glycol 400, 10 percent of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7 percent of isophorone diisocyanate. The carboxyl-terminated polyurethane prepolymer is prepared by synthesizing 41.1 percent of polyethylene glycol 400, 5 percent of 2,2, 4-trimethyl-1, 3-pentanediol, 12.8 percent of isophorone diisocyanate and 41.1 percent of methyl nadic anhydride. The melamine pyrophosphate is white fine powder with the particle size of less than 10 mu m; the grain diameter of the alumina is less than or equal to 10 mu m.
The preparation method of the double-component flexible epoxy pouring sealant comprises the following steps:
(1) synthesizing a hydroxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 68.3% of polyethylene glycol 400, 10% of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7% of isophorone diisocyanate, stirring and heating to 60 ℃ at a rotating speed of 100r/min, finally judging the reaction process by testing the content of NCO, when the content of NCO is less than 5%, the reaction reaches the end point, namely synthesizing to obtain a hydroxyl-terminated polyurethane prepolymer, and discharging for later use;
(2) synthesizing a carboxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 41.1% of polyethylene glycol 400, 5% of 2,2, 4-trimethyl-1, 3-pentanediol and 12.8% of isophorone diisocyanate, reacting for 2 hours at 60 ℃, adding 41.1% of methyl nadic anhydride into the system when the content of NCO is less than 5%, stirring and heating to 60 ℃ at the rotating speed of 150r/min, finally judging the reaction process through the change of acid value, when the acid value is less than 400mgKOH/g, reaching the end point of the reaction, synthesizing to obtain a carboxyl-terminated polyurethane prepolymer, and discharging for later use;
(3) preparing a component A of the flexible epoxy pouring sealant: stirring and mixing 15% of the hydroxyl-terminated polyurethane prepolymer prepared in the step (1) with 50% of vinylcyclohexene dioxide, 10% of tung oil, 15% of melamine pyrophosphate, 9.5% of aluminum oxide and 0.5% of moderate 6800 defoamer uniformly at a rotating speed of 800r/min to prepare a component A of the flexible epoxy pouring sealant, and discharging for later use;
(4) preparing a component B of the flexible epoxy pouring sealant: stirring and mixing 50% of the carboxyl-terminated polyurethane prepolymer prepared in the step (2), 49.5% of methyl nadic anhydride and 0.5% of DMP-30 accelerator uniformly at the rotating speed of 400r/min to obtain a flexible epoxy pouring sealant B component, and discharging for later use;
(5) preparing a double-component flexible epoxy pouring sealant: according to the weight ratio of 100: and 25, stirring and uniformly mixing the component A of the flexible epoxy pouring sealant obtained in the step (3) and the component B of the flexible epoxy pouring sealant obtained in the step (4) at the rotating speed of 400r/min to obtain the double-component flexible epoxy pouring sealant.
During encapsulation, the prepared two-component flexible epoxy pouring sealant is heated and cured.
Example 4
The embodiment 4 provides a two-component flexible epoxy pouring sealant, which comprises the following components in percentage by weight of 100: 22 and a flexible epoxy pouring sealant B, wherein the flexible epoxy pouring sealant A consists of the following raw materials:
the component B of the flexible epoxy pouring sealant consists of the following raw materials:
70 percent of carboxyl-terminated polyurethane prepolymer,
29.9 percent of methyl nadic anhydride,
0.1% of DMP-30 accelerator;
wherein the hydroxyl-terminated polyurethane prepolymer is prepared by synthesizing 68.3 percent of polyethylene glycol 400, 10 percent of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7 percent of isophorone diisocyanate. The carboxyl-terminated polyurethane prepolymer is prepared by synthesizing 41.1 percent of polyethylene glycol 400, 5 percent of 2,2, 4-trimethyl-1, 3-pentanediol, 12.8 percent of isophorone diisocyanate and 41.1 percent of methyl nadic anhydride. The aluminum hydroxide is 600-800 meshes of powder; the grain diameter of the alumina is less than or equal to 10 mu m; the grain size of the silicon micropowder is 2000 meshes.
The preparation method of the double-component flexible epoxy pouring sealant comprises the following steps:
(1) synthesizing a hydroxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 68.3% of polyethylene glycol 400, 10% of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7% of isophorone diisocyanate, stirring and heating to 60 ℃ at a rotating speed of 50r/min, finally judging the reaction process by testing the content of NCO, when the content of NCO is less than 5%, the reaction reaches the end point, namely synthesizing to obtain a hydroxyl-terminated polyurethane prepolymer, and discharging for later use;
(2) synthesizing a carboxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 41.1% of polyethylene glycol 400, 5% of 2,2, 4-trimethyl-1, 3-pentanediol and 12.8% of isophorone diisocyanate, reacting for 2 hours at 60 ℃, adding 41.1% of methyl nadic anhydride into the system when the content of NCO is less than 5%, stirring and heating to 60 ℃ at a rotating speed of 50r/min, finally judging the reaction process through the change of acid value, when the acid value is less than 400mgKOH/g, reaching the end point of the reaction, synthesizing to obtain a carboxyl-terminated polyurethane prepolymer, and discharging for later use;
(3) preparing a component A of the flexible epoxy pouring sealant: stirring and mixing 20% of the hydroxyl-terminated polyurethane prepolymer prepared in the step (1), 40% of epoxy resin E44, 5% of epoxidized soybean oil, 24.9% of aluminum hydroxide, 5% of aluminum oxide, 5% of silicon micropowder and 0.1% of moderate 6800 defoamer uniformly at a rotating speed of 600r/min to prepare a component A of the flexible epoxy pouring sealant, and discharging for later use;
(4) preparing a component B of the flexible epoxy pouring sealant: stirring and mixing 70% of the carboxyl-terminated polyurethane prepolymer prepared in the step (2), 29.9% of methyl nadic anhydride and 0.1% of DMP-30 accelerator uniformly at a rotating speed of 30r/min to obtain a flexible epoxy pouring sealant B component, and discharging for later use;
(5) preparing a double-component flexible epoxy pouring sealant: according to the weight ratio of 100: and 22, uniformly stirring and mixing the component A of the flexible epoxy pouring sealant obtained in the step 3 and the component B of the flexible epoxy pouring sealant obtained in the step 4 at the rotating speed of 30r/min to obtain the double-component flexible epoxy pouring sealant.
During encapsulation, the prepared two-component flexible epoxy pouring sealant is heated and cured.
Example 5
This embodiment 5 provides a two-component flexible epoxy pouring sealant, which includes, by weight, 100: 27 and a flexible epoxy pouring sealant A component and a flexible epoxy pouring sealant B component, wherein the flexible epoxy pouring sealant A component is composed of the following raw materials:
the component B of the flexible epoxy pouring sealant consists of the following raw materials:
30 percent of carboxyl-terminated polyurethane prepolymer,
69 percent of methyl nadic anhydride,
1% of DMP-30 accelerator;
wherein the hydroxyl-terminated polyurethane prepolymer is prepared by synthesizing 68.3 percent of polyethylene glycol 400, 10 percent of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7 percent of isophorone diisocyanate. The carboxyl-terminated polyurethane prepolymer is prepared by synthesizing 41.1 percent of polyethylene glycol 400, 5 percent of 2,2, 4-trimethyl-1, 3-pentanediol, 12.8 percent of isophorone diisocyanate and 41.1 percent of methyl nadic anhydride. The aluminum hydroxide is 600-800 meshes of powder; the magnesium hydroxide is powder with the grain diameter of 1.5-2 mu m, and the whiteness is more than or equal to 95; the grain diameter of the alumina is less than or equal to 10 mu m.
The preparation method of the double-component flexible epoxy pouring sealant comprises the following steps:
(1) synthesizing a hydroxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 68.3% of polyethylene glycol 400, 10% of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7% of isophorone diisocyanate, stirring and heating to 60 ℃ at a rotating speed of 200r/min, finally judging the reaction process by testing the content of NCO, when the content of NCO is less than 5%, the reaction reaches the end point, namely synthesizing to obtain a hydroxyl-terminated polyurethane prepolymer, and discharging for later use;
(2) synthesizing a carboxyl-terminated polyurethane prepolymer: introducing nitrogen into a four-neck flask provided with a thermometer, a condenser, a stirring paddle and an air guide tube, then sequentially adding 41.1% of polyethylene glycol 400, 5% of 2,2, 4-trimethyl-1, 3-pentanediol and 12.8% of isophorone diisocyanate, reacting for 2 hours at 60 ℃, adding 41.1% of methyl nadic anhydride into the system when the content of NCO is less than 5%, stirring and heating to 60 ℃ at the rotating speed of 200r/min, finally judging the reaction process through the change of acid value, when the acid value is less than 400mgKOH/g, reaching the end point of the reaction, synthesizing to obtain a carboxyl-terminated polyurethane prepolymer, and discharging for later use;
(3) preparing a component A of the flexible epoxy pouring sealant: stirring and mixing the 10% of hydroxyl-terminated polyurethane prepolymer prepared in the step (1), 30% of epoxy resin E44, 5% of castor oil, 10% of epoxy soybean oil, 10% of aluminum hydroxide, 27% of magnesium hydroxide, 7% of aluminum oxide and 1% of moderate 6800 defoamer uniformly at the rotating speed of 1000r/min to prepare a component A of the flexible epoxy pouring sealant, and discharging for later use;
(4) preparing a component B of the flexible epoxy pouring sealant: uniformly stirring and mixing 30% of the carboxyl-terminated polyurethane prepolymer prepared in the step (2), 69% of methyl nadic anhydride and 1% of DMP-30 accelerator at a rotating speed of 600r/min to obtain a component B of the flexible epoxy pouring sealant, and discharging for later use;
(5) preparing a double-component flexible epoxy pouring sealant: according to the weight ratio of 100: and 27, stirring and uniformly mixing the component A of the flexible epoxy pouring sealant obtained in the step (3) and the component B of the flexible epoxy pouring sealant obtained in the step (4) at the rotating speed of 600r/min to obtain the double-component flexible epoxy pouring sealant.
During encapsulation, the prepared two-component flexible epoxy pouring sealant is heated and cured.
Comparative example
The comparative example provides a pouring sealant, which comprises the following components in percentage by weight of 100: 25 and a pouring sealant B, wherein the pouring sealant A consists of the following raw materials:
the component B of the pouring sealant consists of the following raw materials:
99 percent of methyl nadic anhydride,
1% of DMP-30 accelerator;
wherein, the aluminum hydroxide is powder of 600 meshes to 800 meshes; the grain diameter of the alumina is less than or equal to 10 mu m.
The preparation method of the pouring sealant comprises the following steps:
(1) preparing a pouring sealant A component: stirring and mixing 59.9% of epoxy resin E44, 10% of epoxidized soybean oil, 20% of aluminum hydroxide, 10% of aluminum oxide and 0.1% of a moderate board 6800 defoaming agent uniformly at the rotating speed of 800r/min to prepare a pouring sealant A component, and discharging for later use;
(2) preparing a pouring sealant B component: stirring and mixing 99% of methyl nadic anhydride and 1% of DMP-30 accelerator uniformly at the rotating speed of 400r/min to obtain a pouring sealant B component, and discharging for later use;
(3) preparing a pouring sealant: according to the weight ratio of 100: and 25, stirring and uniformly mixing the component A of the pouring sealant obtained in the step (1) and the component B of the pouring sealant obtained in the step (2) at the rotating speed of 400r/min to obtain the pouring sealant.
During encapsulation, the prepared pouring sealant is heated and cured.
In order to further verify the performance of the two-component flexible epoxy potting adhesive, the potting adhesives prepared in the above examples 1-5 and comparative examples were used for sealing electronic components, and the potting adhesive and the cured products were tested during the curing process. The tests of each index are carried out according to the terms of GB/T15023-1994 test method for electric insulation solvent-free polymerizable resin compounds. The medium for the electrical strength test is transformer oil, and a continuous boosting mode is adopted. The results are shown in table 1:
TABLE 1 Properties of the potting Compounds from the examples and comparative examples
The data analysis in table 1 shows that the temperature resistance of the capacitor sealed by the two-component flexible epoxy pouring sealant is 2.5-3.75 times of that of the comparative example, and the water absorption after curing is far lower than that of the comparative example, which shows that the product system of the invention has excellent high temperature and high humidity resistance; meanwhile, after being subjected to a cold and hot impact test, the examples 1-5 have no cracking, and the comparative example has a cracking phenomenon, so that the cold and hot impact resistant paint has better cold and hot impact resistance, can avoid cracking and water seepage of a workpiece after being used after glue pouring, and has better moisture resistance; in addition, compared with the comparative example, the hardness of the two-component flexible epoxy pouring sealant in the embodiments 1 to 5 after curing is relatively low, so that the electronic component is not easy to be scratched.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The double-component flexible epoxy pouring sealant is characterized by comprising the following components in percentage by weight of 100: 22-27 of a flexible epoxy pouring sealant A component and a flexible epoxy pouring sealant B component, wherein the flexible epoxy pouring sealant A component is composed of the following raw materials in percentage by weight:
the component B of the flexible epoxy pouring sealant consists of the following raw materials:
30 to 70 percent of carboxyl-terminated polyurethane prepolymer,
30 to 70 percent of methyl nadic anhydride,
0.1 to 1 percent of DMP-30 accelerant.
2. The two-component flexible epoxy pouring sealant as claimed in claim 1, wherein the hydroxyl-terminated polyurethane prepolymer is prepared by synthesizing 68.3% of polyethylene glycol 400, 10% of 2,2, 4-trimethyl-1, 3-pentanediol and 21.7% of isophorone diisocyanate in percentage by weight.
3. The two-component flexible epoxy pouring sealant as claimed in claim 1, wherein the carboxyl-terminated polyurethane prepolymer is prepared by synthesizing 41.1% of polyethylene glycol 400, 5% of 2,2, 4-trimethyl-1, 3-pentanediol, 12.8% of isophorone diisocyanate, and 41.1% of methylnadic anhydride.
4. The two-component flexible epoxy potting adhesive of claim 1, wherein the epoxy resin is one or any combination of epoxy resin E51, epoxy resin E44, vinylcyclohexene dioxide.
5. The two-component flexible epoxy pouring sealant as claimed in claim 1, wherein the grease is one or any combination of castor oil, epoxidized soybean oil and tung oil.
6. The two-component flexible epoxy pouring sealant as claimed in claim 1, wherein the flame retardant filler is one or any combination of aluminum hydroxide, magnesium hydroxide and melamine pyrophosphate.
7. The two-component flexible epoxy potting adhesive of claim 1, wherein the heat conductive filler is one or any combination of alumina, silica micropowder and calcium carbonate.
8. The two-component flexible epoxy pouring sealant according to claim 1, wherein the defoamer is a 6800 defoamer or a BYK A555 defoamer.
9. The preparation method of the two-component flexible epoxy pouring sealant as claimed in any one of claims 1 to 8, comprising the following steps:
(1) synthesizing a hydroxyl-terminated polyurethane prepolymer: adding polyethylene glycol 400, 2, 4-trimethyl-1, 3-pentanediol and isophorone diisocyanate into a four-neck flask with nitrogen introduced in sequence, stirring and heating at a rotating speed of 50 r/min-200 r/min to 60 ℃, and when the content of NCO is less than 5%, reacting to reach the end point, thus synthesizing the hydroxyl-terminated polyurethane prepolymer for later use;
(2) synthesizing a carboxyl-terminated polyurethane prepolymer: sequentially adding polyethylene glycol 400, 2, 4-trimethyl-1, 3-pentanediol and isophorone diisocyanate into a four-neck flask into which nitrogen is introduced, reacting for 2 hours at 60 ℃, adding methyl nadic anhydride into a system when the content of NCO is less than 5%, stirring and heating to 60 ℃ at the rotating speed of 50 r/min-200 r/min, and synthesizing to obtain carboxyl-terminated polyurethane when the acid value is less than 400mgKOH/g and the reaction is finished for later use;
(3) preparing a component A of the flexible epoxy pouring sealant: uniformly stirring and mixing the hydroxyl-terminated polyurethane prepolymer prepared in the step (1) with epoxy resin, grease, flame-retardant filler, heat-conducting filler and defoamer at a rotating speed of 600 r/min-1000 r/min to obtain a component A of the flexible epoxy pouring sealant;
(4) preparing a component B of the flexible epoxy pouring sealant: uniformly stirring and mixing the carboxyl-terminated polyurethane prepolymer prepared in the step (2) with methyl nadic anhydride and DMP-30 accelerator at the rotating speed of 30 r/min-600 r/min to obtain a component B of the flexible epoxy pouring sealant;
(5) preparing a double-component flexible epoxy pouring sealant: and (4) stirring and uniformly mixing the component A of the flexible epoxy pouring sealant obtained in the step (3) and the component B of the flexible epoxy pouring sealant obtained in the step (4) at the rotating speed of 30-600 r/min to obtain the double-component flexible epoxy pouring sealant.
10. Use of the two-component flexible epoxy potting adhesive according to any of claims 1 to 8 in the preparation of electronic component seals.
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| CN111826105A (en) * | 2020-06-11 | 2020-10-27 | 北京康美特科技股份有限公司 | Packaging adhesive for LED and use method and application thereof |
| CN112778949A (en) * | 2020-12-31 | 2021-05-11 | 山西省交通科技研发有限公司 | Environment-friendly adhesive capable of being mixed for construction and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111826105A (en) * | 2020-06-11 | 2020-10-27 | 北京康美特科技股份有限公司 | Packaging adhesive for LED and use method and application thereof |
| CN111826105B (en) * | 2020-06-11 | 2022-04-15 | 北京康美特科技股份有限公司 | Packaging adhesive for LED and use method and application thereof |
| CN112778949A (en) * | 2020-12-31 | 2021-05-11 | 山西省交通科技研发有限公司 | Environment-friendly adhesive capable of being mixed for construction and preparation method thereof |
| CN112831301A (en) * | 2020-12-31 | 2021-05-25 | 山西省交通科技研发有限公司 | High-light-reflection environment-friendly colorful anti-skid pavement and preparation method thereof |
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