CN109504338B - Polyurethane foaming heat-conducting electronic pouring sealant and preparation method thereof - Google Patents
Polyurethane foaming heat-conducting electronic pouring sealant and preparation method thereof Download PDFInfo
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- CN109504338B CN109504338B CN201811492953.9A CN201811492953A CN109504338B CN 109504338 B CN109504338 B CN 109504338B CN 201811492953 A CN201811492953 A CN 201811492953A CN 109504338 B CN109504338 B CN 109504338B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J191/00—Adhesives based on oils, fats or waxes; Adhesives based on derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention relates to a polyurethane foaming heat-conducting electronic pouring sealant and a preparation method thereof.
Description
Technical Field
The invention belongs to the technical field of sealants, and particularly relates to a polyurethane foaming heat-conducting electronic pouring sealant and a preparation method thereof.
Background
In recent years, new energy automobiles such as electric automobiles and the like become a new trend of the future automobile industry due to the advantages of no pollution, low noise, high energy efficiency, diversification, simple structure, convenience in maintenance and the like. Particularly, electric automobiles in China have been in the industrialization stage from the research and development stage initially through the process of one decade and one sword. Among them, it is generally pursued in the industry to improve the driving mileage, increase the number of battery packs, and reduce the weight of automobile body and spare part. As is well known, the reduction of the weight of the automobile can effectively reduce the emission of the automobile and realize the improvement of the combustion efficiency of the automobile. The self weight of the automobile is reduced by 10 percent, and the fuel consumption can be reduced by 6 to 8 percent. Therefore, the weight reduction of the automobile can reduce energy consumption, increase the speed of the automobile, improve safety and reduce pollution.
The most common and widely-used electronic pouring sealant at present is a polyurethane pouring sealant, which can effectively reduce the weight of parts such as a vehicle-mounted charger, a battery module management system, an air conditioner management system, a transmission controller and the like. The traditional polyurethane pouring sealant has the advantages of water resistance, acid resistance, good toughness, good sealing property and the like. However, the stability of single polyurethane is poor, the heat conductivity is poor, and the phenomena of air bubbles, glue shortage and the like are easy to occur during encapsulation.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the polyurethane foaming heat-conducting electronic pouring sealant with good stability and heat-conducting property and the preparation method thereof.
The technical scheme adopted by the invention is as follows:
a polyurethane foaming heat-conducting electronic pouring sealant comprises the following raw material components:
4-10 parts of polyurethane, 4-10 parts of acrylic resin emulsion, 0.5-2 parts of surfactant, 80-100 parts of polyol A, 3-6 parts of polyol B, 80-110 parts of castor oil, 0.01-0.05 part of catalyst, 20-30 parts of heat conducting agent and 5-30 parts of curing agent.
The surfactant is OP-10.
The polyalcohol A is one or a mixture of more of polypropylene glycol, 1, 2-propylene glycol and 1, 2-propylene glycol cage polysilsesquioxane;
the polyalcohol B is one or a mixture of more of polypropylene glycol, 1, 2-propylene glycol and 1, 2-propylene glycol cage polysilsesquioxane.
The structural formula of the 1, 2-propylene glycol cage polysilsesquioxane is as follows:
the catalyst is a dipropylene glycol solution of triethylene diamine with the mass concentration of 33%;
the heat conducting agent is graphene;
the curing agent is modified polyphenyl polymethylene polyisocyanate.
The preparation method of the polyurethane foaming heat-conducting electronic pouring sealant comprises the following steps:
(1) preparation of polyurethane-acrylate composite emulsion
Respectively taking the polyurethane and the acrylic resin emulsion, fully mixing under stirring, adding the surfactant in the stirring process, and fully and uniformly mixing to obtain polyurethane-acrylic ester composite emulsion;
(2) preparation of acrylic acid modified polyurethane prepolymer
Taking the polyhydric alcohol A, and carrying out vacuum-pumping dehydration to obtain dehydrated polyhydric alcohol A; under the protection of nitrogen, cooling the dehydrated polyol A, adding the polyurethane-acrylate composite emulsion in the step (1), controlling the addition amount of the polyurethane-acrylate composite emulsion to be 5-20% of the mass fraction of the dehydrated polyol A, stirring to uniformly mix, heating to 80-90 ℃ and reacting for 2-3h to obtain an acrylic modified polyurethane prepolymer;
(3) preparation of chain extender component
Respectively taking the polyol B and the castor oil, uniformly mixing, vacuumizing, dehydrating, cooling, adding the catalyst, and fully stirring to obtain a chain extender component;
(4) preparation of pouring sealant
Respectively preheating the acrylic acid modified polyurethane prepolymer in the step (2) and the chain extender in the step (3), mixing, adding the heat-conducting agent, stirring, adding the curing agent, stirring and simultaneously performing vacuum defoaming to obtain the polyurethane foaming heat-conducting electronic potting adhesive.
In the step (1), the stirring speed is 800-;
in the step (2), the temperature for vacuum dehydration is 80-110 ℃, the pressure for vacuum dehydration is-0.095 MPa, the time for vacuum dehydration is 1.5-2.0h, and the water content of the dehydrated polyalcohol A is less than 0.1%; and cooling the dehydrated polyol A to 30-50 ℃, wherein the stirring speed is 800-1000r/min, and the stirring time is 5-10 min.
In the step (3), the temperature for vacuum dehydration is 80-110 ℃, the pressure for vacuum dehydration is-0.095 MPa, the time for vacuum dehydration is 1.0-1.5h, and the water content after dehydration is less than 0.1%; cooling to room temperature; the stirring speed is 800-;
in the step (4), the preheating is carried out for 30min at the temperature of 50-60 ℃;
the mass ratio of the acrylic acid modified polyurethane prepolymer to the chain extender component is 40-90: 100; the stirring speed of the two times is 800-1000r/min, and the stirring time is 5-10 min.
The invention has the beneficial effects that:
1. according to the preparation method of the polyurethane foaming heat-conducting electronic pouring sealant, polyurethane is modified by using acrylic resin to obtain the acrylic modified polyurethane prepolymer, and then the chain extender, the heat conducting agent and the curing agent are added into the acrylic modified polyurethane prepolymer under specific conditions to carry out stirring reaction, so that the finally prepared polyurethane foaming heat-conducting electronic pouring sealant is good in stability and heat conducting performance, and can effectively avoid the problems of bubbles, glue shortage and the like during pouring. The reason is that the inventor finds that single polyurethane is unsatisfactory in stability and the like in long-term research, and the acrylic resin has the advantages of high mechanical strength, aging resistance, yellowing resistance, good water resistance and the like, but has the defects of poor organic solvent resistance, poor heat resistance, poor wear resistance and the like.
2. According to the polyurethane foaming heat-conducting electronic pouring sealant disclosed by the invention, graphene is used as a heat-conducting agent, so that the heat conductivity of the pouring sealant can be effectively improved, and the special requirement on the heat conductivity in the actual use process is met.
3. According to the polyurethane foaming heat-conducting electronic pouring sealant, 1, 2-propylene glycol cage type polysilsesquioxane is used as a chain extender, and a special cage type frame structure is utilized, so that the finally prepared pouring sealant has good performance, and the strength and the toughness can be effectively improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
In the following examples 1g is represented by 1 part by weight.
Example 1
The embodiment provides a polyurethane foaming heat conduction electronic pouring sealant, and the raw material components include:
4 parts of polyurethane, 4 parts of acrylic resin emulsion, 0.5 part of surfactant OP-10, 80 parts of 1, 2-propylene glycol cage polysilsesquioxane polyol A, 3 parts of 1, 2-propylene glycol cage polysilsesquioxane polyol B, 80 parts of castor oil, 0.01 part of dipropylene glycol solution of 33% of triethylene diamine as a catalyst, 20 parts of graphene as a heat conducting agent and 5 parts of modified polyphenyl polymethylene polyisocyanate as a curing agent.
The preparation method of the polyurethane foaming heat-conducting electronic pouring sealant comprises the following steps:
(1) preparation of polyurethane-acrylate composite emulsion
Respectively taking the polyurethane and the acrylic resin emulsion, stirring for 5min under the stirring condition of 800r/min to fully mix, adding the surfactant in the stirring process, and fully and uniformly mixing to obtain polyurethane-acrylate composite emulsion;
(2) preparation of acrylic acid modified polyurethane prepolymer
Adding the polyol A into a vacuumizing stirring kettle, vacuumizing and dehydrating for 1.5h under the conditions of 80 ℃ and-0.095 MPa, and stopping vacuumizing when the moisture content is measured to be less than 0.1% to obtain dehydrated polyol A; under the protection of nitrogen, cooling the dehydrated polyol A to 45 ℃, adding the polyurethane-acrylate composite emulsion in the step (1), controlling the addition amount of the polyurethane-acrylate composite emulsion to be 5% of the mass fraction of the dehydrated polyol A, stirring at the speed of 800r/min for 5min to uniformly mix, and heating to 80 ℃ for reaction for 2h to obtain an acrylic modified polyurethane prepolymer;
(3) preparation of chain extender component
Adding the polyol B and the castor oil into a stirring kettle, vacuumizing and dehydrating for 1.0-1.5h under the conditions of 80 ℃ and-0.095 MPa, stopping vacuumizing when the water content is measured to be less than 0.1%, cooling to room temperature, adding the catalyst, and stirring at the speed of 1000r/min for 2-3min to obtain a chain extender component;
(4) preparation of pouring sealant
Respectively preheating the acrylic acid modified polyurethane prepolymer in the step (2) and the chain extender component in the step (3) at 50 ℃ for 30min, and then mixing, wherein the mass ratio of the acrylic acid modified polyurethane prepolymer to the chain extender component is controlled to be 40: 100; and then adding the heat-conducting agent, stirring for 5min at the speed of 800r/min, finally adding the curing agent, stirring at the speed of 800r/min and defoaming in vacuum for 5min at the same time, thus obtaining the polyurethane foaming heat-conducting electronic pouring sealant.
Example 2
The embodiment provides a polyurethane foaming heat conduction electronic pouring sealant, and the raw material components include:
5 parts of polyurethane, 5 parts of acrylic resin emulsion, 1 part of surfactant OP-10, 85 parts of 1, 2-propylene glycol cage polysilsesquioxane as polyol A, 4 parts of 1, 2-propylene glycol cage polysilsesquioxane as polyol B, 90 parts of castor oil, 0.03 part of dipropylene glycol solution of 33% of triethylene diamine as a catalyst, 25 parts of graphene as a heat conducting agent and 15 parts of modified polyphenyl polymethylene polyisocyanate as a curing agent.
The preparation method of the polyurethane foaming heat-conducting electronic pouring sealant comprises the following steps:
(1) preparation of polyurethane-acrylate composite emulsion
Respectively taking the polyurethane and the acrylic resin emulsion, stirring for 7min under the stirring condition of 850r/min to fully mix, adding the surfactant in the stirring process, and fully and uniformly mixing to obtain polyurethane-acrylate composite emulsion;
(2) preparation of acrylic acid modified polyurethane prepolymer
Adding the polyol A into a vacuumizing stirring kettle, vacuumizing and dehydrating for 1.5h under the conditions of 90 ℃ and-0.095 MPa, and stopping vacuumizing when the moisture content is measured to be less than 0.1% to obtain dehydrated polyol A; under the protection of nitrogen, cooling the dehydrated polyol A to 45 ℃, adding the polyurethane-acrylate composite emulsion in the step (1), controlling the addition amount of the polyurethane-acrylate composite emulsion to be 10% of the mass fraction of the dehydrated polyol A, stirring at the speed of 850r/min for 7min to uniformly mix, and heating to 85 ℃ for reaction for 2h to obtain an acrylic modified polyurethane prepolymer;
(3) preparation of chain extender component
Adding the polyol B and the castor oil into a stirring kettle, vacuumizing and dehydrating for 1.0h under the conditions of 90 ℃ and-0.095 MPa, stopping vacuumizing when the moisture content is measured to be less than 0.1%, cooling to room temperature, adding the catalyst, and stirring at the speed of 850r/min for 2.5min to obtain a chain extender component;
(4) preparation of pouring sealant
Respectively preheating the acrylic acid modified polyurethane prepolymer in the step (2) and the chain extender component in the step (3) at 55 ℃ for 30min, and then mixing, wherein the mass ratio of the acrylic acid modified polyurethane prepolymer to the chain extender component is controlled to be 50: 100; and then adding the heat-conducting agent, stirring for 7min at the speed of 850r/min, finally adding the curing agent, stirring at the speed of 850r/min, and simultaneously carrying out vacuum defoaming for 7min to obtain the polyurethane foaming heat-conducting electronic pouring sealant.
Example 3
The embodiment provides a polyurethane foaming heat conduction electronic pouring sealant, and the raw material components include:
9 parts of polyurethane, 9 parts of acrylic resin emulsion, 1.5 parts of surfactant OP-10, 90 parts of polypropylene glycol as polyol A, 5 parts of polypropylene glycol as polyol B, 100 parts of castor oil, 0.04 part of 33% triethylene diamine dipropylene glycol solution as catalyst, 30 parts of graphene as heat conducting agent and 20 parts of modified polyphenyl polymethylene polyisocyanate as curing agent.
The preparation method of the polyurethane foaming heat-conducting electronic pouring sealant comprises the following steps:
(1) preparation of polyurethane-acrylate composite emulsion
Respectively taking the polyurethane and the acrylic resin emulsion, stirring for 10min under the stirring condition of 900r/min to fully mix, adding the surfactant in the stirring process, and fully and uniformly mixing to obtain polyurethane-acrylate composite emulsion;
(2) preparation of acrylic acid modified polyurethane prepolymer
Adding the polyol A into a vacuumizing stirring kettle, vacuumizing and dehydrating for 1.5h under the conditions of 100 ℃ and-0.095 MPa, and stopping vacuumizing when the moisture content is measured to be less than 0.1% to obtain dehydrated polyol A; under the protection of nitrogen, cooling the dehydrated polyol A to 35 ℃, adding the polyurethane-acrylate composite emulsion in the step (1), controlling the addition amount of the polyurethane-acrylate composite emulsion to be 15% of the mass fraction of the dehydrated polyol A, stirring at the speed of 900r/min for 10min to uniformly mix, and heating to 90 ℃ to react for 3h to obtain an acrylic modified polyurethane prepolymer;
(3) preparation of chain extender component
Adding the polyol B and the castor oil into a stirring kettle, vacuumizing and dehydrating for 1.5h under the conditions of 100 ℃ and-0.095 MPa, stopping vacuumizing when the moisture content is measured to be less than 0.1%, cooling to room temperature, adding the catalyst, and stirring at the speed of 900r/min for 3min to obtain a chain extender component;
(4) preparation of pouring sealant
Respectively preheating the acrylic acid modified polyurethane prepolymer in the step (2) and the chain extender component in the step (3) at 60 ℃ for 30min, and then mixing, wherein the mass ratio of the acrylic acid modified polyurethane prepolymer to the chain extender component is controlled to be 80: 100; and then adding the heat-conducting agent, stirring at the speed of 900r/min for 10min, finally adding the curing agent, stirring at the speed of 900r/min, and simultaneously carrying out vacuum defoaming for 10min to obtain the polyurethane foaming heat-conducting electronic pouring sealant.
Example 4
The embodiment provides a polyurethane foaming heat conduction electronic pouring sealant, and the raw material components include:
10 parts of polyurethane, 10 parts of acrylic resin emulsion, 2 parts of surfactant OP-10, 100 parts of 1, 2-propylene glycol as polyol A, 6 parts of 1, 2-propylene glycol as polyol B, 110 parts of castor oil, 0.05 part of dipropylene glycol solution of 33% of triethylene diamine as a catalyst, 30 parts of graphene as a heat conducting agent and 30 parts of modified polyphenyl polymethylene polyisocyanate as a curing agent.
The preparation method of the polyurethane foaming heat-conducting electronic pouring sealant comprises the following steps:
(1) preparation of polyurethane-acrylate composite emulsion
Respectively taking the polyurethane and the acrylic resin emulsion, stirring for 10min under the stirring condition of 1000r/min to fully mix, adding the surfactant in the stirring process, and fully and uniformly mixing to obtain polyurethane-acrylate composite emulsion;
(2) preparation of acrylic acid modified polyurethane prepolymer
Adding the polyol A into a vacuumizing stirring kettle, vacuumizing and dehydrating for 2.0 hours at the temperature of 110 ℃ and under the pressure of-0.095 MPa, and stopping vacuumizing when the moisture content is measured to be less than 0.1% to obtain dehydrated polyol A; under the protection of nitrogen, cooling the dehydrated polyol A to 30 ℃, adding the polyurethane-acrylate composite emulsion in the step (1), controlling the addition amount of the polyurethane-acrylate composite emulsion to be 20% of the mass fraction of the dehydrated polyol A, stirring at the speed of 1000r/min for 10min to uniformly mix, and heating to 90 ℃ to react for 3h to obtain an acrylic modified polyurethane prepolymer;
(3) preparation of chain extender component
Adding the polyol B and the castor oil into a stirring kettle, vacuumizing and dehydrating for 1.5h under the conditions of 110 ℃ and-0.095 MPa, stopping vacuumizing when the moisture content is measured to be less than 0.1%, cooling to room temperature, adding the catalyst, and stirring at the speed of 1000r/min for 3min to obtain a chain extender component;
(4) preparation of pouring sealant
Respectively preheating the acrylic acid modified polyurethane prepolymer in the step (2) and the chain extender component in the step (3) at 60 ℃ for 30min, and then mixing, wherein the mass ratio of the acrylic acid modified polyurethane prepolymer to the chain extender component is controlled to be 90: 100; and then adding the heat-conducting agent, stirring for 10min at the speed of 1000r/min, finally adding the curing agent, stirring at the speed of 1000r/min, and simultaneously carrying out vacuum defoaming for 10min to obtain the polyurethane foaming heat-conducting electronic pouring sealant.
Examples of the experiments
The polyurethane foaming heat-conducting electronic pouring sealant prepared in the examples 1 to 4 is poured into a mold to prepare a sample (the heat-conducting sample mold is a cylinder with the diameter of 4cm and the thickness of 1mm, the stretching and shearing sample is an aluminum alloy test piece hinged part, the lap joint area is 12.5mm multiplied by 25mm, and the glue layer thickness is 0.2mm), the curing conditions of all samples are 25 ℃ for curing for 7d, and the related performance is measured after the curing is finished.
1. Test method
(1) Viscosity: the measurement was carried out according to GB/T2794-1995 using a rotary viscometer.
(2) Hardness: according to the GB/531.1-2008 standard, the measurement is carried out by a Shore D durometer.
(3) Tensile shear strength: according to the GB/T7124-2008 standard, an electronic universal tester is adopted for measurement.
(4) Coefficient of thermal conductivity: the measurement was carried out by using a thermal conductivity measuring instrument in accordance with ASTM E1530-2006.
2. Test results
TABLE 1 four Performance test results
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (6)
1. The utility model provides a polyurethane foaming heat conduction electron pouring sealant which characterized in that, raw materials component includes:
4-10 parts of polyurethane, 4-10 parts of acrylic resin emulsion, 0.5-2 parts of surfactant, 80-100 parts of polyol A, 3-6 parts of polyol B, 80-110 parts of castor oil, 0.01-0.05 part of catalyst, 20-30 parts of heat conducting agent and 5-30 parts of curing agent;
the surfactant is OP-10;
the polyalcohol A is one or a mixture of more of polypropylene glycol, 1, 2-propylene glycol and 1, 2-propylene glycol cage polysilsesquioxane;
the polyalcohol B is one or a mixture of more of polypropylene glycol, 1, 2-propylene glycol and 1, 2-propylene glycol cage polysilsesquioxane;
the structural formula of the 1, 2-propylene glycol cage polysilsesquioxane is as follows:
the catalyst is a dipropylene glycol solution of triethylene diamine with the mass concentration of 33%;
the heat conducting agent is graphene;
the curing agent is modified polyphenyl polymethylene polyisocyanate;
the preparation method of the polyurethane foaming heat-conducting electronic pouring sealant comprises the following steps:
(1) preparation of polyurethane-acrylate composite emulsion
Respectively taking the polyurethane and the acrylic resin emulsion, fully mixing under stirring, adding the surfactant in the stirring process, and fully and uniformly mixing to obtain polyurethane-acrylic ester composite emulsion;
(2) preparation of acrylic acid modified polyurethane prepolymer
Taking the polyhydric alcohol A, and carrying out vacuum-pumping dehydration to obtain dehydrated polyhydric alcohol A; under the protection of nitrogen, cooling the dehydrated polyol A, adding the polyurethane-acrylate composite emulsion in the step (1), controlling the addition amount of the polyurethane-acrylate composite emulsion to be 5-20% of the mass fraction of the dehydrated polyol A, stirring to uniformly mix, heating to 80-90 ℃ and reacting for 2-3h to obtain an acrylic modified polyurethane prepolymer;
(3) preparation of chain extender component
Respectively taking the polyol B and the castor oil, uniformly mixing, vacuumizing, dehydrating, cooling, adding the catalyst, and fully stirring to obtain a chain extender component;
(4) preparation of pouring sealant
Respectively preheating the acrylic acid modified polyurethane prepolymer in the step (2) and the chain extender in the step (3), mixing, adding the heat-conducting agent, stirring, adding the curing agent, stirring and simultaneously performing vacuum defoaming to obtain the polyurethane foaming heat-conducting electronic potting adhesive.
2. The preparation method of the polyurethane foaming heat-conducting electronic pouring sealant as claimed in claim 1, characterized by comprising the following steps:
(1) preparation of polyurethane-acrylate composite emulsion
Respectively taking the polyurethane and the acrylic resin emulsion, fully mixing under stirring, adding the surfactant in the stirring process, and fully and uniformly mixing to obtain polyurethane-acrylic ester composite emulsion;
(2) preparation of acrylic acid modified polyurethane prepolymer
Taking the polyhydric alcohol A, and carrying out vacuum-pumping dehydration to obtain dehydrated polyhydric alcohol A; under the protection of nitrogen, cooling the dehydrated polyol A, adding the polyurethane-acrylate composite emulsion in the step (1), controlling the addition amount of the polyurethane-acrylate composite emulsion to be 5-20% of the mass fraction of the dehydrated polyol A, stirring to uniformly mix, heating to 80-90 ℃ and reacting for 2-3h to obtain an acrylic modified polyurethane prepolymer;
(3) preparation of chain extender component
Respectively taking the polyol B and the castor oil, uniformly mixing, vacuumizing, dehydrating, cooling, adding the catalyst, and fully stirring to obtain a chain extender component;
(4) preparation of pouring sealant
Respectively preheating the acrylic acid modified polyurethane prepolymer in the step (2) and the chain extender in the step (3), mixing, adding the heat-conducting agent, stirring, adding the curing agent, stirring and simultaneously performing vacuum defoaming to obtain the polyurethane foaming heat-conducting electronic potting adhesive.
3. The method for preparing the polyurethane foaming heat-conducting electronic pouring sealant as claimed in claim 2, wherein in the step (1), the stirring speed is 800-1000r/min, and the stirring time is 5-10 min.
4. The preparation method of the polyurethane foam heat-conducting electronic pouring sealant as claimed in claim 2, wherein in the step (2), the temperature for vacuum dehydration is 80-110 ℃, the pressure for vacuum dehydration is-0.095 MPa, the time for vacuum dehydration is 1.5-2.0h, and the water content of the dehydrated polyol A is less than 0.1%; and cooling the dehydrated polyol A to 30-50 ℃, wherein the stirring speed is 800-1000r/min, and the stirring time is 5-10 min.
5. The preparation method of the polyurethane foam heat-conducting electronic pouring sealant as claimed in claim 2, wherein in the step (3), the temperature for vacuum dehydration is 80-110 ℃, the pressure for vacuum dehydration is-0.095 MPa, the time for vacuum dehydration is 1.0-1.5h, and the water content after dehydration is less than 0.1%; cooling to room temperature; the stirring speed is 800-1000r/min, and the stirring time is 2-3 min.
6. The preparation method of the polyurethane foam heat-conducting electronic pouring sealant as claimed in claim 2, wherein in the step (4), the preheating is performed at 50-60 ℃ for 30 min;
the mass ratio of the acrylic acid modified polyurethane prepolymer to the chain extender component is 40-90: 100; the stirring speed of the two times is 800-1000r/min, and the stirring time is 5-10 min.
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| CN101974141A (en) * | 2010-09-19 | 2011-02-16 | 广州市香港科大***研究院 | Preparation method of water-based polyacrylate modified polyurethane dispersion (PUD) |
| CN106675494A (en) * | 2016-11-24 | 2017-05-17 | 俞明亮 | Water-based polyurethane adhesive for bullet-proof vest composite material and preparation method of water-based polyurethane adhesive |
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| CN102617823B (en) * | 2012-03-29 | 2013-06-12 | 合肥工业大学 | Process for preparing hydroxyl polyhedral oligomeric silsesquioxane modified polyurethane |
| CN104531033B (en) * | 2015-01-20 | 2016-08-24 | 广州市聚科聚氨酯有限公司 | A kind of preparation method of resistant to elevated temperatures water-based polyurethane adhesive |
| CN104987851B (en) * | 2015-07-31 | 2017-09-26 | 华南理工大学 | One kind electrolysis door filling polyurethane cellular glue and preparation method thereof |
| CN105238326A (en) * | 2015-09-21 | 2016-01-13 | 太仓市金锚新材料科技有限公司 | Polyurethane adhesive and preparation method thereof |
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| CN101974141A (en) * | 2010-09-19 | 2011-02-16 | 广州市香港科大***研究院 | Preparation method of water-based polyacrylate modified polyurethane dispersion (PUD) |
| CN106675494A (en) * | 2016-11-24 | 2017-05-17 | 俞明亮 | Water-based polyurethane adhesive for bullet-proof vest composite material and preparation method of water-based polyurethane adhesive |
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| Synthesis and morphology of rigid polyurethane foams with POSS as pendant groups or chemical crosslinks;Edyta Hebda等;《Polymers for advanced technologies》;20150831;第26卷(第8期);第932-940页 * |
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