CN111592852A - Low-viscosity high-mechanical-property polyurethane pouring sealant and preparation method and application thereof - Google Patents
Low-viscosity high-mechanical-property polyurethane pouring sealant and preparation method and application thereof Download PDFInfo
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08G18/28—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
- C08G18/36—Hydroxylated esters of higher fatty acids
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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
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
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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
- 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
- C08G18/6696—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/36 or hydroxylated esters of higher fatty acids of C08G18/38
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention provides a polyurethane pouring sealant with low viscosity and high mechanical property, and a preparation method and application thereof. The polyurethane pouring sealant with low viscosity and high mechanical property comprises raw materials of a component A and a component B, wherein the component A comprises MDI-50 and PAPI, and the component B comprises castor oil and an auxiliary agent. The polyisocyanate of the polyurethane pouring sealant with low viscosity and high mechanical property adopts the combination of MDI-50 and PAPI, the dosage of the MDI-50 and the PAPI is optimized, and the polyurethane formed can simultaneously have low viscosity and high mechanical property under the action of other castor oil, additives and the like. The lower viscosity brings better flow property, and simultaneously, the excellent mechanical property of the high-viscosity high-fluidity high-viscosity liquid is also suitable for the daily environmental.
Description
Technical Field
The invention relates to the technical field of polyurethane, in particular to a polyurethane pouring sealant with low viscosity and high mechanical property, and a preparation method and application thereof.
Background
The pouring sealant is widely applied to the manufacturing of electronic components, can strengthen the overall performance of the electronic components, improve the resistance to external impact and vibration, improve the insulativity between internal elements and circuits, avoid the direct exposure of the elements and the circuits, and improve the waterproof and damp-proof performances of the components. The existing pouring sealant products mainly comprise three types of epoxy pouring sealants, polyurethane pouring sealants and organic silicon pouring sealants, wherein the epoxy pouring sealants are brittle and do not resist cold and heat shock, and the organic silicon pouring sealants are low in strength, poor in adhesive force and higher in cost. The polyurethane potting adhesive has wide hardness adjustment range, not only has the elasticity of rubber but also has the hardness of plastics, has excellent performance, overcomes the defects of easy brittle fracture of epoxy resin and low strength and poor adhesion of organic silicon, and is widely applied to the fields of telecommunication cables, electronics, aerospace, ships, automobiles and the like.
The preparation of polyurethane pouring sealant can be generally divided into three methods, including a one-step method and a prepolymerization method. The prepolymerization method is to react polyester or polyether polyol with isocyanate to generate prepolymer, and then chain-extend the prepolymer with diol or diamine to generate polyurethane. The polyurethane pouring sealant prepared by the prepolymerization method has a certain block structure, and the arrangement of molecular chain segments is complete, so that the polyurethane pouring sealant has good mechanical properties, but the viscosity of a prepolymer is too high, the operating performance is poor, the complicated electronic components are difficult to naturally fill, and gaps are easy to remain. Compared with the prior art, the polyurethane pouring sealant prepared by the one-step method has disordered molecular chains, and the mechanical property after curing is poor although the viscosity is low. Therefore, there is a need to provide a polyurethane potting adhesive having both low viscosity and good mechanical properties.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a polyurethane pouring sealant with low viscosity and high mechanical property, and a preparation method and application thereof.
In a first aspect, an embodiment of the present invention provides a low-viscosity high-mechanical-property polyurethane pouring sealant, which includes, by weight ratio (15-25): 100 of a component A and a component B, wherein the component A comprises the following raw materials in a weight ratio of 1: (5-10) MDI-50 and PAPI, and the component B comprises castor oil and an auxiliary agent.
Diphenylmethane diisocyanate (MDI) includes isomers of 4,4'-MDI, 2' -MDI, etc., and MDI-50 used in the examples of the present invention is an MDI product having 4,4'-MDI and 2,4' -MDI contents each of which accounts for about 50%. Polymethylene polyphenyl polyisocyanate (PAPI, also known as PMDI, crude MDI) is a mixture of polyisocyanates of different functionalities, including diisocyanates and isocyanates of low degree of polymerization.
The polyurethane pouring sealant with low viscosity and high mechanical property provided by the embodiment of the invention has at least the following beneficial effects:
the polyisocyanate of the polyurethane pouring sealant with low viscosity and high mechanical property adopts the combination of MDI-50 and PAPI, the dosage of the MDI-50 and the PAPI is optimized, and the polyurethane formed can simultaneously have low viscosity and high mechanical property under the action of other castor oil and other auxiliary agents. The lower viscosity brings better flow property, and simultaneously, the excellent mechanical property of the high-viscosity high-fluidity high-viscosity liquid is also suitable for the daily environmental requirement.
According to the polyurethane pouring sealant with low viscosity and high mechanical property of some embodiments of the invention, the component B also comprises polyether polyol. The hydrolysis resistance of the pouring sealant is improved by adding polyether polyol.
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the polyether polyol is selected from at least one of polyoxypropylene diol and polyoxypropylene triol. The polyurethane produced by using the polyoxypropylene diol or the polyoxypropylene triol as the source of the polyether polyol to react with the polyisocyanate, and reacting two or three hydroxyl groups on the polyoxypropylene diol or the polyoxypropylene triol with MDI-50 or PAPI has better mechanical property.
According to the polyurethane pouring sealant with low viscosity and high mechanical property, disclosed by the invention, the weight average molecular weight of the polyether polyol is 500-1000. The polyether polyol with the weight average molecular weight in the range has the molecular weight close to that of castor oil, the reaction activity is also close, the intersolubility is good, the prepared product has regular molecules and good mechanical property.
According to the polyurethane pouring sealant with low viscosity and high mechanical property of some embodiments of the invention, the polyether polyol is polyoxypropylene triol. The polyurethane obtained by the reaction of the polyoxypropylene triol with the functionality of 3, MDI-50 and PAPI keeps lower elongation at break while the viscosity of the polyurethane is reduced.
According to some embodiments of the present invention, the polyurethane pouring sealant has low viscosity and high mechanical properties, and the castor oil is refined first-grade castor oil. The polyurethane obtained by the reaction of the castor oil and the polyisocyanate can obtain higher crosslinking degree and better heat resistance.
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the auxiliary agent comprises color paste, an anti-settling agent, a coupling agent, a catalyst, a defoaming agent, a flame retardant, a water removing agent and a filler.
According to some embodiments of the invention, the component B comprises, by weight, 0-20 parts of polyether polyol, 25-45 parts of castor oil, 0.2-0.5 part of color paste, 0.1-0.5 part of anti-settling agent, 0.2-0.5 part of coupling agent, 0-0.2 part of catalyst, 0.1-0.5 part of defoaming agent, 20-45 parts of flame retardant, 1-3 parts of water removing agent, and 10-30 parts of filler
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the anti-settling agent is selected from at least one of YRFC-01 (Guangzhou Youyun synthetic materials Co., Ltd.), YRFC-03 (Guangzhou Youyun synthetic materials Co., Ltd.) and RSA (Shanghai Gehrig chemical industry Co., Ltd.).
According to the polyurethane pouring sealant with low viscosity and high mechanical property of some embodiments of the present invention, the flame retardant is selected from at least two of ammonium polyphosphate (APP), aluminum hydroxide, Aluminum Hypophosphite (AHP), diethyl aluminum hypophosphite (ADP), Melamine (MC), Melamine Cyanurate (MCA).
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the flame retardant is ammonium polyphosphate, aluminum hydroxide and aluminum hypophosphite. The flame retardant combination of ammonium polyphosphate, aluminum hydroxide and aluminum hypophosphite is adopted, so that a sufficient flame retardant effect can be obtained on the basis of ensuring the performance of polyurethane.
According to the polyurethane pouring sealant with low viscosity and high mechanical property of some embodiments of the invention, the catalyst is an organic metal catalyst, such as an organic lead catalyst, an organic tin catalyst, an organic titanium catalyst, an organic zinc catalyst and an organic mercury catalyst.
According to the polyurethane pouring sealant with low viscosity and high mechanical property of some embodiments of the invention, the catalyst is selected from at least one of CUCTA-H (Guangzhou Youyun synthetic materials Co., Ltd.), DY-5350 (Shanghai Desheng chemical Co., Ltd.), DY-5508 (Shanghai Desheng chemical Co., Ltd.).
According to the polyurethane pouring sealant with low viscosity and high mechanical property of some embodiments of the invention, the coupling agent is at least one selected from gamma-aminopropyl ethoxy siloxane (KH550), gamma-glycidoxypropyl trimethoxy silane (KH560) and gamma-aminoethylaminopropyl trimethoxy silane (KH 792).
According to the polyurethane pouring sealant with low viscosity and high mechanical property, disclosed by the invention, the coupling agent is gamma-glycidyl ether oxypropyltrimethoxysilane.
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the defoaming agent is at least one of an organic silicon defoaming agent and a polymer defoaming agent.
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the water removal agent is at least one OF Additive OF water removal agent, p-Toluenesulfonyl Isocyanate (TI), calcium oxide, molecular sieve drying agent, oxazolidine water removal agent and carbodiimide water removal agent.
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the water removal agent is an Additive OF water removal agent and p-toluenesulfonyl isocyanate.
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the filler is selected from at least one of crystalline silica micropowder, spherical alumina, magnesium oxide, aluminum nitride, boron nitride and silicon carbide.
According to the polyurethane pouring sealant with low viscosity and high mechanical property, the filler is spherical alumina.
In a second aspect, an embodiment of the present invention provides a method for preparing the polyurethane pouring sealant with low viscosity and high mechanical properties, including the following steps:
preparation of component A:
mixing MDI-50 and PAPI, sealing and packaging;
preparation of component B:
mixing castor oil, polyether polyol, a flame retardant, a filler, an anti-settling agent, a coupling agent and color paste, dispersing at 120-130 ℃, dehydrating, degassing, cooling to 50-60 ℃, adding a catalyst, a defoaming agent and a water removing agent, mixing uniformly, sealing and packaging.
According to the preparation method of the polyurethane pouring sealant with low viscosity and high mechanical property, MDI-50 and PAPI are mixed uniformly, vacuumized at normal temperature and then packaged in a sealing mode.
According to the preparation method of the polyurethane pouring sealant with low viscosity and high mechanical property, the dehydration and degassing method is to dehydrate and degas for 3-4h under the vacuum condition.
In a third aspect, an embodiment of the present invention provides a method of potting an electronic device, the method comprising the steps of:
taking the component A and the component B of the polyurethane pouring sealant with low viscosity and high mechanical property according to the ratio of (15-25): 100 weight percent, and then pouring the mixture into an electronic device.
According to the encapsulating method of the electronic device, after pouring, the gel can be formed at room temperature for 4-6 hours, the gel can be solidified apparently after about 6 hours, the hardness (70A-80A) reaches 90% after 48 hours, and the final performance is reached after 7 days; heating and baking at 60-70 deg.C for 1 hr to solidify, reaching 90% hardness (70-80A) after 48 hr, and reaching final performance after 7 days.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and other embodiments obtained by those skilled in the art without inventive efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
Example 1
The embodiment provides a polyurethane pouring sealant with low viscosity and high mechanical property, which comprises raw materials of a component A and a component B.
Component A comprises 10 parts by weight of MDI-50 and 90 parts by weight of PAPI (the total parts by weight of component A is 100 parts).
The component B comprises the following components in parts by weight (the total parts by weight of the component B is 100 parts):
15 portions of polyether polyol (MN-1000),
25 parts of refined first-grade castor oil,
0.5 portion of carbon black color paste,
0.4 part of anti-settling agent (YRFC-03),
0.2 portion of coupling agent (KH550),
0.1 portion of catalyst (CUCTA-H),
0.5 part of defoaming agent (BYK-17940.2 parts, BYK-066N 0.3 part),
35 parts of flame retardant (15 parts of ammonium polyphosphate, 10 parts of aluminum hydroxide and 10 parts of aluminum hypophosphite),
1.3 parts OF water-removing agent (Additive OF 0.5 parts, TI 0.8 parts),
22 parts of filler (spherical alumina).
The preparation method of the polyurethane pouring sealant with low viscosity and high mechanical property comprises the following steps:
(1) mixing and stirring PAPI and MDI-50 uniformly, vacuumizing for 1h at normal temperature, and barreling and sealing for packaging;
(2) adding refined first-grade castor oil, polyether polyol, a flame retardant, a filler, an anti-settling agent, a coupling agent and carbon black color paste into a reaction kettle, dispersing at a high speed at 120-130 ℃, vacuumizing, dehydrating, degassing for 3-4h, cooling to 50-60 ℃, adding a catalyst, a defoaming agent and a water removing agent, stirring uniformly, sealing and packaging.
The method for encapsulating the electronic device by using the polyurethane encapsulating adhesive with low viscosity and high mechanical property comprises the following steps of mixing the component A and the component B according to the weight ratio of 16.6: 100 (the component A and the component B in the component distribution ratio respectively represent the measurement standard only inside the component A and the component B in 100 parts, but do not represent the relative measurement of the component A and the component B) are uniformly mixed, and the mixture is poured on an electronic device to be cured for 7d at room temperature, so that the encapsulation of the electronic device is completed.
Example 2
The embodiment provides a polyurethane pouring sealant with low viscosity and high mechanical property, which comprises raw materials of a component A and a component B.
Component A comprises 10 parts by weight of MDI-50 and 90 parts by weight of PAPI.
The component B comprises the following components in parts by weight:
10 portions of polyether polyol (MN-1000),
35 parts of refined first-grade castor oil,
0.5 portion of carbon black color paste,
0.4 part of anti-settling agent (YRFC-03),
0.2 portion of coupling agent (KH550),
0.1 portion of catalyst (CUCTA-H),
0.5 part of defoaming agent (BYK-17940.2 parts, BYK-066N 0.3 part),
35 parts of flame retardant (15 parts of ammonium polyphosphate, 10 parts of aluminum hydroxide and 10 parts of aluminum hypophosphite),
1.3 parts OF water-removing agent (Additive OF 0.5 parts, TI 0.8 parts),
17 parts of filler (spherical alumina).
The preparation method of the polyurethane pouring sealant with low viscosity and high mechanical property comprises the following steps:
(1) mixing and stirring PAPI and MDI-50 uniformly, vacuumizing for 1h at normal temperature, and barreling and sealing for packaging;
(2) adding refined first-grade castor oil, polyether polyol, a flame retardant, a filler, an anti-settling agent, a coupling agent and carbon black color paste into a reaction kettle, dispersing at a high speed at 120-130 ℃, vacuumizing, dehydrating, degassing for 3-4h, cooling to 50-60 ℃, adding a catalyst, a defoaming agent and a water removing agent, stirring uniformly, sealing and packaging.
The method for encapsulating the electronic device by using the polyurethane encapsulating adhesive with low viscosity and high mechanical property comprises the following steps of mixing the component A and the component B according to the ratio of 20: 100, and pouring the mixture on the electronic device for curing at room temperature for 7 days to complete the encapsulation of the electronic device.
Example 3
The embodiment provides a polyurethane pouring sealant with low viscosity and high mechanical property, which comprises raw materials of a component A and a component B.
Component A comprises 15 parts by weight of MDI-50 and 85 parts by weight of PAPI.
The component B comprises the following components in parts by weight:
10 portions of polyether polyol (MN-700),
35 parts of refined first-grade castor oil,
0.5 portion of carbon black color paste,
0.4 part of anti-settling agent (YRFC-03),
0.2 portion of coupling agent (KH550),
0.1 portion of catalyst (CUCTA-H),
0.5 part of defoaming agent (BYK-17940.2 parts, BYK-066N 0.3 part),
35 parts of flame retardant (15 parts of ammonium polyphosphate, 10 parts of aluminum hydroxide and 10 parts of aluminum hypophosphite),
1.3 parts OF water-removing agent (Additive OF 0.5 parts, TI 0.8 parts),
17 parts of filler (spherical alumina).
The preparation method of the polyurethane pouring sealant with low viscosity and high mechanical property comprises the following steps:
(1) mixing and stirring PAPI and MDI-50 uniformly, vacuumizing for 1h at normal temperature, and barreling and sealing for packaging;
(2) adding refined first-grade castor oil, polyether polyol, a flame retardant, a filler, an anti-settling agent, a coupling agent and carbon black color paste into a reaction kettle, dispersing at a high speed at 120-130 ℃, vacuumizing, dehydrating, degassing for 3-4h, cooling to 50-60 ℃, adding a catalyst, a defoaming agent and a water removing agent, stirring uniformly, sealing and packaging.
The method for encapsulating the electronic device by using the polyurethane encapsulating adhesive with low viscosity and high mechanical property comprises the following steps of mixing the component A and the component B according to the ratio of 20: 100, and pouring the mixture on the electronic device for curing at room temperature for 7 days to complete the encapsulation of the electronic device.
Example 4
The embodiment provides a polyurethane pouring sealant with low viscosity and high mechanical property, which comprises raw materials of a component A and a component B.
Component A comprises 10 parts by weight of MDI-50 and 90 parts by weight of PAPI.
The component B comprises the following components in parts by weight:
45 parts of refined first-grade castor oil,
0.5 portion of carbon black color paste,
0.4 part of anti-settling agent (YRFC-03),
0.2 portion of coupling agent (KH550),
0 portion of catalyst,
0.5 part of defoaming agent (BYK-17940.2 parts, BYK-066N 0.3 part),
35 parts of flame retardant (15 parts of ammonium polyphosphate, 10 parts of aluminum hydroxide and 10 parts of aluminum hypophosphite),
1.4 parts OF water-removing agent (Additive OF 0.6 parts, TI 0.8 parts),
17 parts of filler (spherical alumina).
The preparation method of the polyurethane pouring sealant with low viscosity and high mechanical property comprises the following steps:
(1) mixing and stirring PAPI and MDI-50 uniformly, vacuumizing for 1h at normal temperature, and barreling and sealing for packaging;
(2) adding the refined first-grade castor oil, the flame retardant, the filler, the anti-settling agent, the coupling agent and the carbon black color paste into a reaction kettle, dispersing at a high speed at 120-130 ℃, vacuumizing, dehydrating and degassing for 3-4h, cooling to 50-60 ℃, adding the defoaming agent and the water removing agent, stirring uniformly, and sealing and packaging.
The method for encapsulating the electronic device by using the polyurethane encapsulating adhesive with low viscosity and high mechanical property comprises the following steps of mixing the component A and the component B according to the ratio of 20: 100, and pouring the mixture on the electronic device for curing at room temperature for 7 days to complete the encapsulation of the electronic device.
Example 5
Comparative experiment
Comparative example 1: a polyurethane pouring sealant with low viscosity and high mechanical property comprises raw materials of a component A and a component B. The weight ratio of the component A to the component B is 20: 100. wherein the content of the first and second substances,
the component A is 100 parts of PAPI by weight.
The component B comprises the following components in parts by weight:
45 parts of refined first-grade castor oil,
0.5 portion of carbon black color paste,
0.4 part of anti-settling agent (YRFC-03),
0.2 portion of coupling agent (KH550),
0.1 portion of catalyst (CUCTA-H),
0.5 part of defoaming agent (BYK-17940.2 parts, BYK-066N 0.3 part),
35 parts of flame retardant (15 parts of ammonium polyphosphate, 10 parts of aluminum hydroxide and 10 parts of aluminum hypophosphite),
1.3 parts OF water-removing agent (Additive OF 0.5 parts, TI 0.8 parts),
17 parts of filler (spherical alumina).
The preparation method of the polyurethane pouring sealant with low viscosity and high mechanical property refers to the above examples.
Comparative example 2 is a polyurethane pouring sealant product of market-imported brand Huntsman (Huntsman), which is mainly prepared from raw materials including isocyanate as component A, and polyol, flame retardant, filler, pigment, auxiliary agent and the like as component B, and has a composition similar to that of the raw materials of the invention. The AB component was as follows: 100, and curing for 7d at room temperature.
The polyurethane pouring sealants with low viscosity and high mechanical property of examples 1-4 and comparative examples 1 and 2 are respectively selected, mixed according to respective proportions and tested for viscosity, and other items are tested after being cured for 7 days.
Wherein the viscosity is measured by a rotational viscometer method in GB/T10247-2008 viscosity measuring method.
The bubble testing method comprises the steps of encapsulating the same electronic components in the same glue filling mode, baking or curing at normal temperature, and carrying out visual inspection.
The Shore A hardness is measured by a Shore A durometer according to the standard of GB/T531.1-2008 vulcanized rubber or thermoplastic rubber indentation hardness test method.
The tensile strength and the elongation at break are measured by an electronic universal tester according to the GB/T528-2009 determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber.
The dielectric strength was measured according to GB/T1408.1-2016 insulating Material electric Strength test method, part 1, Power frequency test.
The volume resistivity is measured according to GB/T1410-2006 solid insulating material volume resistivity and surface resistivity test method.
The thermal conductivity was measured according to the thermal wire method for measuring thermal conductivity of non-metallic solid materials GB 10297-2015.
Flame retardancy the horizontal and vertical flammability were determined according to UL 94.
The storage stability determination criteria were: after the powder is stored for a certain time at room temperature, the precipitated starch material is less than or equal to 20 percent of the total powder, the powder is judged to be not precipitated and stable to store, otherwise, the powder is judged to be precipitated and deteriorated.
The cold and hot impact test conditions are as follows: and (3) respectively keeping high and low temperatures in an environment box circulating at the temperature of minus 40 ℃ and 85 ℃ for 1 hour, 500 times of circulation and 1000 hours, then observing appearance conditions, and testing mechanical properties and electrical properties after standing at room temperature for 7 days.
The results are shown in table 1 below.
TABLE 1 comparative experimental results
From the measurement results, the pouring sealant prepared in the examples 1 to 4 has good mechanical property, electrical property and flame retardant property, is stable in storage and is not prone to precipitation. And the pouring sealant has low viscosity, good fluidity and good operation performance. By adjusting the types and the proportion of isocyanate, polyether glycol and the like, the product with low viscosity and high mechanical property is obtained, and the method is suitable for encapsulating the micro-control board with a fine structure. In the scheme of the comparative example 1, due to the difference of the raw material proportion, the product has high viscosity, and is difficult to defoam and easy to have bubbles. Compared with the comparative example 2, the performance of the polyurethane pouring sealant with low viscosity and high mechanical property provided by the embodiment of the invention reaches the same level of foreign products, has higher mechanical property while keeping lower viscosity, has better operation performance when in use, has higher cost performance and better economic applicability, and can replace similar imported products.
The polyurethane pouring sealant with low viscosity and high mechanical property provided by the embodiment of the invention has high flowing property, is suitable for pouring the fine structure of the micro-control board, can be cured by baking or normal temperature curing, is simple and convenient to operate, and has strong applicability. Meanwhile, the defoaming effect is good, natural defoaming can be realized, vacuum defoaming is not needed, and the operation equipment is simple; because no plasticizer is added, the pouring sealant has excellent electrical performance, strong bonding force with the micro control board, water resistance, moisture resistance and good anti-vibration effect, and can effectively prolong the service life of electronic equipment. In addition, the stability test and the cold and heat shock resistant test result show that the polyurethane pouring sealant with low viscosity and high mechanical property provided by the embodiment of the invention has good stability, does not precipitate, is not easy to deteriorate, and can be stored for more than 6 months at normal temperature. But also can resist cold and heat shock for more than 1000 hours at the temperature of minus 40 ℃ to 85 ℃ without cracking, and has better cold and heat shock resistance.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. The polyurethane pouring sealant with low viscosity and high mechanical property is characterized by comprising the following components in parts by weight (15-25): 100 of a component A and a component B, wherein the component A comprises the following raw materials in a weight ratio of 1: (5-10) MDI-50 and PAPI, wherein the component B comprises castor oil and an auxiliary agent.
2. The low-viscosity high-mechanical-property polyurethane pouring sealant as claimed in claim 1, wherein the component B further comprises polyether polyol.
3. The polyurethane pouring sealant with low viscosity and high mechanical property as claimed in claim 2, wherein the polyether polyol is at least one selected from polyoxypropylene diol and polyoxypropylene triol.
4. The polyurethane pouring sealant with low viscosity and high mechanical property as claimed in claim 2, wherein the polyether polyol has a weight average molecular weight of 500-1000.
5. The polyurethane pouring sealant with low viscosity and high mechanical property as claimed in any one of claims 1 to 4, wherein the component B comprises, by weight, 0 to 20 parts of polyether polyol, 25 to 45 parts of castor oil, 0.2 to 0.5 part of color paste, 0.1 to 0.5 part of anti-settling agent, 0.2 to 0.5 part of coupling agent, 0 to 0.2 part of catalyst, 0.1 to 0.5 part of defoaming agent, 20 to 45 parts of flame retardant, 1 to 3 parts of water scavenger, and 10 to 30 parts of filler.
6. The low-viscosity high-mechanical-property polyurethane pouring sealant as claimed in claim 5, wherein the flame retardant is selected from at least two of ammonium polyphosphate, aluminum hydroxide, aluminum hypophosphite, diethyl aluminum hypophosphite, melamine and melamine uronate.
7. The polyurethane pouring sealant with low viscosity and high mechanical property as claimed in claim 5, wherein the coupling agent is at least one selected from γ -aminopropyl ethoxysiloxane, γ -glycidoxypropyl trimethoxysilane and γ -aminoethyl aminopropyltrimethoxysilane.
8. The polyurethane pouring sealant with low viscosity and high mechanical property as claimed in claim 7, wherein the coupling agent is gamma-glycidoxypropyltrimethoxysilane.
9. The method for preparing the polyurethane pouring sealant with low viscosity and high mechanical property as claimed in any one of claims 1 to 8, comprising the following steps:
preparation of component A:
mixing MDI-50 and PAPI, sealing and packaging;
preparation of component B:
mixing castor oil, polyether polyol, a flame retardant, a filler, an anti-settling agent, a coupling agent and color paste, dispersing at 120-130 ℃, dehydrating, degassing, cooling to 50-60 ℃, adding a catalyst, a defoaming agent and a water removing agent, mixing uniformly, sealing and packaging.
10. A method for encapsulating an electronic device, comprising the steps of:
taking the component A and the component B of the polyurethane pouring sealant with low viscosity and high mechanical property as defined in any one of claims 1 to 8, according to the ratio of (15-25): and after being uniformly mixed according to the weight ratio of 100, the mixture is poured into the electronic device.
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