CN115124963A - Metal polar plate sealant and preparation method thereof - Google Patents

Metal polar plate sealant and preparation method thereof Download PDF

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Publication number
CN115124963A
CN115124963A CN202210863987.4A CN202210863987A CN115124963A CN 115124963 A CN115124963 A CN 115124963A CN 202210863987 A CN202210863987 A CN 202210863987A CN 115124963 A CN115124963 A CN 115124963A
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parts
nco
sealant
polyurethane prepolymer
terminated polyurethane
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扶勇欢
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Shenzhen Center Power Tech Co Ltd
Shenzhen Hydrogen Fuel Cell Technology Co Ltd
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Shenzhen Center Power Tech Co Ltd
Shenzhen Hydrogen Fuel Cell Technology Co Ltd
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Priority to CN202210863987.4A priority Critical patent/CN115124963A/en
Publication of CN115124963A publication Critical patent/CN115124963A/en
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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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08G18/40—High-molecular-weight compounds
    • C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4205—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
    • C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
    • C08G18/4211—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols
    • C08G18/4213—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols from terephthalic acid and dialcohols
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4825—Polyethers containing two hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08G18/65—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
    • C08G18/6629—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/36 or hydroxylated esters of higher fatty acids of C08G18/38
    • 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
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention relates to a metal pole plate sealant which comprises the following components in parts by mass: 10-200 parts of NCO-terminated polyurethane prepolymer, 5-20 parts of zinc oxide, 20-40 parts of talcum powder, 1-10 parts of hydrogenated castor oil and 5-20 parts of titanium dioxide. The invention also provides a preparation method of the metal pole plate sealant. The method can solve the problem of shortening the single-component polyurethane by partially or completely sealing the NCO end groups of the NCO end group polyurethane prepolymerThe curing time of the sealant is short, and the sealant cannot be caused by CO 2 The single-component polyurethane sealant can not be diffused in time to cause foaming of the single-component polyurethane sealant, and the storage stability of the single-component polyurethane sealant can be ensured. The metal polar plate sealant has short curing time and good storage stability, and can not be used for CO 2 It is not too long to diffuse and cause the sealant to foam.

Description

Metal electrode plate sealant and preparation method thereof
Technical Field
The invention relates to the technical field of fuel cells, in particular to a metal polar plate sealant and a preparation method thereof.
Background
In recent years, metal electrode plates have been widely used in the field of fuel cells because of their advantages such as good mechanical strength, high electrical conductivity, and corrosion resistance. The metal polar plate is provided with a flow channel for supplying hydrogen, oxygen and water, so that if gas leakage occurs, the utilization rate of gas is easily reduced, the performance of the fuel cell is greatly influenced, even dangerous accidents occur, and the sealing property of the polar plate needs to be ensured.
In the prior art, a sealant is usually added between a metal plate and a membrane electrode frame to maintain the sealing performance of the metal plate. There are many types of sealants, and one-component sealants and two-component sealants are common. To ensure the curing speed, sealing strength and adhesive properties of the sealants, two-component sealants are generally achieved by adding catalysts to the hydroxyl component, while one-component sealants (particularly one-component moisture-curing sealants) may cause a problem of reduced storage stability if more catalysts are added, although the curing speed can be increased. The curing time of the sealant is relatively slow compared to adhesives, particularly solvent-based adhesives. Therefore, for the one-component polyurethane sealant, how to shorten the curing time and not cause CO 2 The problem that the single-component polyurethane sealant foams because the single-component polyurethane sealant cannot diffuse in time and the storage stability of the single-component polyurethane sealant can be ensured is to be solved urgently.
Disclosure of Invention
Based on the above, the embodiment of the invention provides a metal pole plate sealant and a preparation method thereof, aiming at solving the problem of how to shorten the curing time of a single-component polyurethane sealant without CO 2 The diffusion is not in time to cause the foaming of the single-component polyurethane sealant and can ensureThe storage stability of the single-component polyurethane sealant and the like. The metal polar plate sealant has short curing time and good storage stability, and can not be used for CO 2 It is not too long to diffuse and cause the sealant to foam.
In order to achieve the above object, in one aspect, an embodiment of the present invention provides a metal plate sealant, which includes the following components in parts by mass: 10-200 parts of NCO-terminated polyurethane prepolymer, 5-20 parts of zinc oxide, 20-40 parts of talcum powder, 1-10 parts of hydrogenated castor oil and 5-20 parts of titanium dioxide.
As a preferred embodiment, the metal plate sealant comprises the following components in parts by mass: 178 parts of NCO-terminated polyurethane prepolymer, 16.8 parts of zinc oxide, 25 parts of talcum powder, 5 parts of hydrogenated castor oil and 5 parts of titanium dioxide.
In a preferred embodiment, the NCO-terminated polyurethane prepolymer is prepared by the following method: carrying out condensation reflux reaction on 60-80 Parts of Polypropylene Glycol (PPG), 1-10 parts of 2, 4-toluene diisocyanate (2,4-TDI), 10-30 Parts of Polytrimethylene Terephthalate (PPT) and 1-10 parts of stannous octoate at 80-100 ℃ for 12-48 h to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
In a preferred embodiment, the NCO-terminated polyurethane prepolymer is prepared by the following method: condensing and refluxing 70 Parts of Polypropylene Glycol (PPG), 6 parts of 2, 4-toluene diisocyanate (2,4-TDI), 20 Parts of Polytrimethylene Terephthalate (PPT) and 8 parts of stannous octoate at 90 ℃ for 18h to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
As a preferable embodiment, the NCO group content of the end NCO group polyurethane prepolymer is 1% -10%, and the percentage is mass percent.
In a preferred embodiment, the NCO-terminated polyurethane prepolymer is pretreated by the following method: carrying out condensation reflux reaction on the NCO-terminated polyurethane prepolymer and N, N-bis [ (trimethoxysilyl) propyl ] amine at the temperature of 80-100 ℃ for 12-48 h to obtain an NCO-terminated prepolymer with the concentration of 5%; the percentage is mass percentage. And 5% refers to the mass percentage of the blocked NCO groups in the NCO-terminated polyurethane prepolymer.
In a preferred embodiment, the mass ratio of the NCO-group-terminated polyurethane prepolymer to the N, N-bis [ (trimethoxysilyl) propyl ] amine is (100 to 150): 0.7, preferably 112.1: 0.7.
in the embodiment of the application, the metal plate sealant still has excellent adhesion in a dry state or a soaking state (20 ℃ and 7 days), does not bubble in a high-temperature and high-humidity environment, is cured quickly (the curing time is about 10min at 120 ℃ and 65% RH), and has high strength.
On the other hand, the embodiment of the invention also provides a preparation method of the metal plate sealant, which comprises the following steps: sequentially adding 10-200 parts of NCO-terminated polyurethane prepolymer, 5-20 parts of zinc oxide, 20-40 parts of talcum powder, 1-10 parts of hydrogenated castor oil and 5-20 parts of titanium dioxide into a round-bottom flask, uniformly stirring by magnetic force, and carrying out condensation reflux reaction at 80-85 ℃ for 12-36 hours to obtain a metal pole plate sealant; the parts are parts by mass.
In a preferred embodiment, the magnetic stirring time is 2 hours. This ensures that all reactants are mixed uniformly and no solid particles are present.
The prepared metal pole plate sealant is a viscous glue sample and has an excellent bonding effect.
The method can solve the problem of shortening the curing time of the single-component polyurethane sealant and avoid CO generation by partially or completely sealing the NCO end groups of the NCO end group polyurethane prepolymer 2 The single-component polyurethane sealant can not be diffused in time to cause foaming of the single-component polyurethane sealant, and the storage stability of the single-component polyurethane sealant can be ensured. The metal polar plate sealant has short curing time and good storage stability, and can not be used for CO 2 It is not too long to diffuse and cause the sealant to foam.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a graph of 180 peel strength test data for a metal plate sealant of example 1 in accordance with the present invention;
FIG. 2 is a graph of 180 peel strength test data for a metal plate sealant of comparative example 1 in accordance with the present invention;
FIG. 3 is a schematic diagram of a peel strength testing method according to an embodiment of the invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the embodiments.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
It should be noted that, if directional indications (such as up, down, left, right, front, back, top and bottom … …) are involved in the embodiment of the present invention, the directional indications are only used to explain the relative position relationship between the components, the motion situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indications are changed accordingly.
In this application, unless expressly stated or limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can include, for example, fixed connections, removable connections, or integral parts; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
In addition, if there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
In the prior art, in order to ensure the curing speed, the sealing strength and the bonding performance of the sealant, the two-component sealant is usually realized by adding a catalyst into a hydroxyl component, while the single-component sealant (particularly the single-component wet curing sealant) can improve the curing speed but possibly cause the problem of reduced storage stability if more catalysts are added. The curing time of the sealant is relatively slow compared to adhesives, particularly solvent-based adhesives. Therefore, for the one-component polyurethane sealant, how to shorten the curing time and not cause CO 2 The problem to be solved is that the single-component polyurethane sealant can not be diffused in time to cause foaming of the single-component polyurethane sealant, and the storage stability of the single-component polyurethane sealant can be ensured. Therefore, it is necessary to provide a metal plate sealant and a preparation method thereof to solve the above technical problems.
Specifically, on the one hand, the embodiment of the invention provides a metal pole plate sealant which comprises the following components in parts by mass: 10-200 parts of NCO-terminated polyurethane prepolymer, 5-20 parts of zinc oxide, 20-40 parts of talcum powder, 1-10 parts of hydrogenated castor oil and 5-20 parts of titanium dioxide.
By controlling the dosage of each component, the curing speed and the storage stability of the metal pole plate sealant can be ensured, and the cost is lower.
As a preferred embodiment, the metal plate sealant comprises the following components in parts by mass: 178 parts of NCO-terminated polyurethane prepolymer, 16.8 parts of zinc oxide, 25 parts of talcum powder, 5 parts of hydrogenated castor oil and 5 parts of titanium dioxide.
In a preferred embodiment, the NCO-terminated polyurethane prepolymer is prepared by the following method: carrying out condensation reflux reaction on 60-80 Parts of Polypropylene Glycol (PPG), 1-10 parts of 2, 4-toluene diisocyanate (2,4-TDI), 10-30 Parts of Polytrimethylene Terephthalate (PPT) and 1-10 parts of stannous octoate at 80-100 ℃ for 12-48 h to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
By controlling the dosage of each component, the reasonable dosage of the initiator and the catalyst can be ensured, the curing speed and the storage stability of the metal polar plate sealant can be ensured, and the cost control is also reasonable. The metal polar plate sealant can be kept at the peeling strength to the maximum extent after condensation reflux reaction for 12-48 h at 80-100 ℃. When the temperature is lower than 80 ℃, the reaction of reactants is incomplete, a large amount of small molecular substances exist, and the stability of the metal plate sealant is influenced; when the temperature exceeds 100 ℃, the product can generate side reaction, so that the curing is not thorough, and the sealing performance of the metal pole plate sealant is influenced.
In a preferred embodiment, the NCO-terminated polyurethane prepolymer is prepared by the following method: condensing and refluxing 70 Parts of Polypropylene Glycol (PPG), 6 parts of 2, 4-toluene diisocyanate (2,4-TDI), 20 Parts of Polytrimethylene Terephthalate (PPT) and 8 parts of stannous octoate at 90 ℃ for 18 hours to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
As a preferred embodiment, the NCO group content in the NCO-terminated polyurethane prepolymer is 1% to 10%, and the percentage is mass percent.
In a preferred embodiment, the NCO-terminated polyurethane prepolymer is pretreated by the following method: carrying out condensation reflux reaction on the NCO-terminated polyurethane prepolymer and N, N-bis [ (trimethoxysilyl) propyl ] amine at the temperature of 80-100 ℃ for 12-48 h to obtain an NCO-terminated prepolymer with the concentration of 5%; the percentage is mass percentage. And 5 percent refers to the mass percent of blocked NCO groups in the NCO-terminated polyurethane prepolymer.
The NCO end group of the end NCO group polyurethane prepolymer is partially or completely sealed by pretreating the end NCO group polyurethane prepolymer, so that the peel strength of the metal polar plate sealant can be kept to the maximum extent, the curing time of the sealant is shortened, and CO is not generated 2 The sealant can not be diffused in time to cause the foaming of the sealant, and the storage stability of the sealant can be ensured.
In a preferred embodiment, the mass ratio of the NCO-group-terminated polyurethane prepolymer to the N, N-bis [ (trimethoxysilyl) propyl ] amine is (100 to 150): 0.7, can be 100: 0.7, 120: 0.7, 140: 0.7, 150: 0.7, etc., preferably 112.1: 0.7. therefore, the peeling strength of the metal pole plate sealant can be maintained to the maximum extent, and the adhesive force of the metal pole plate sealant can be guaranteed to the maximum extent. If the mass ratio is more than 150: 0.7, the prepared sealant has poor bonding force; if the mass ratio is less than 110: 0.7, the peel strength of the prepared sealant is poor.
In the embodiment of the application, the metal plate sealant still has excellent adhesion in a dry state or a soaking state (20 ℃ and 7 days), does not bubble in a high-temperature and high-humidity environment, is cured quickly (the curing time is about 10min at 120 ℃ and 65% RH), and has high strength.
On the other hand, the embodiment of the invention also provides a preparation method of the metal plate sealant, which comprises the following steps: sequentially adding 10-200 parts of NCO-terminated polyurethane prepolymer, 5-20 parts of zinc oxide, 20-40 parts of talcum powder, 1-10 parts of hydrogenated castor oil and 5-20 parts of titanium dioxide into a round-bottom flask, uniformly stirring by magnetic force (generally 50Hz), and carrying out condensation reflux reaction at 80-85 ℃ for 12-36 h to obtain a metal pole plate sealant; the parts are parts by mass.
By controlling the dosage of each component, the peel strength of the metal polar plate sealant can be maintained to the maximum extent, the curing time of the sealant is shortened, and CO is avoided 2 The sealant can not be diffused in time to cause the foaming of the sealant, and the storage stability of the sealant can be ensured. When the temperature is lower than 80 ℃, the reaction of reactants is incomplete, a large amount of small molecular substances exist, and the stability of the metal plate sealant is influenced; when the temperature exceeds 85 ℃, the product can generate side reaction, so that the curing is not thorough, and the sealing performance of the metal pole plate sealant is influenced.
In a preferred embodiment, the magnetic stirring time is 2 hours. This ensures that all reactants are mixed uniformly and no solid particles are present.
The prepared metal pole plate sealant is viscous and has excellent bonding effect.
The method can solve the problem of shortening the curing time of the single-component polyurethane sealant and avoid CO generation by partially or completely sealing the NCO end groups of the NCO end group polyurethane prepolymer 2 The single-component polyurethane sealant can not be diffused in time to cause foaming of the single-component polyurethane sealant, and the storage stability of the single-component polyurethane sealant can be ensured. The metal polar plate sealant has short curing time and good storage stability, and can not be caused by CO 2 It is not time to diffuse and cause the sealant to foam.
Example 1
A preparation method of a metal pole plate sealant comprises the following steps: 178 parts of NCO-terminated polyurethane prepolymer, 16.8 parts of zinc oxide, 25 parts of talcum powder, 5 parts of hydrogenated castor oil and 5 parts of titanium dioxide are sequentially added into a round-bottom flask, stirred by magnetic force (50Hz) for 2 hours until the materials are uniform, and then subjected to condensation reflux reaction at 85 ℃ for 24 hours to obtain metal pole plate sealant; the parts are parts by mass. The prepared metal pole plate sealant is viscous and has excellent bonding effect.
The NCO-terminated polyurethane prepolymer is prepared by the following method: condensing and refluxing 70 Parts of Polypropylene Glycol (PPG), 6 parts of 2, 4-toluene diisocyanate (2,4-TDI), 20 Parts of Polytrimethylene Terephthalate (PPT) and 8 parts of stannous octoate at 90 ℃ for 18h to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
The NCO-terminated polyurethane prepolymer is pretreated by the following method: condensing and refluxing the NCO-terminated polyurethane prepolymer and N, N-bis [ (trimethoxysilyl) propyl ] amine at 80 ℃ for 48 hours to obtain an NCO-terminated prepolymer with the content of about 5 percent; the percentage is mass percentage. The mass ratio of the NCO-terminated polyurethane prepolymer to the N, N-bis [ (trimethoxysilyl) propyl ] amine is 112.1: 0.7. and 5% refers to the mass percentage of the blocked NCO groups in the NCO-terminated polyurethane prepolymer.
The prepared metal pole plate sealant still has excellent bonding force in a dry state or a soaking state (20 ℃ and 7 days), does not bubble in a high-temperature and high-humidity environment, is cured quickly (the curing time is about 10min at 120 ℃ and 65% RH), and has high strength and good storage stability. The schematic diagram of the peeling strength of the metal plate sealant is shown in fig. 1, and it can be seen from fig. 1 that the prepared metal plate sealant has strong adhesive force and small fluctuation of the peeling strength.
Example 2
A preparation method of a metal pole plate sealant comprises the following steps: adding 178 parts of NCO-terminated polyurethane prepolymer, 20 parts of zinc oxide, 20 parts of talcum powder, 6 parts of hydrogenated castor oil and 7 parts of titanium dioxide into a round-bottom flask in sequence, stirring uniformly by magnetic force (50Hz) for 2 hours, and carrying out condensation reflux reaction at 90 ℃ for 24 hours to obtain a metal pole plate sealant; the parts are parts by mass. The prepared metal pole plate sealant is viscous and has excellent bonding effect.
The NCO-terminated polyurethane prepolymer is prepared by the following method: condensing 75 Parts of Polypropylene Glycol (PPG), 8 parts of 2, 4-toluene diisocyanate (2,4-TDI), 25 Parts of Polytrimethylene Terephthalate (PPT) and 10 parts of stannous octoate at 90 ℃ for reflux reaction for 20 hours to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
The NCO-terminated polyurethane prepolymer is pretreated by the following method: condensing and refluxing the NCO-terminated polyurethane prepolymer and N, N-bis [ (trimethoxysilyl) propyl ] amine at 100 ℃ for 12 hours to obtain an NCO-terminated prepolymer with the content of about 5 percent; the percentage is mass percentage. The mass ratio of the NCO-terminated polyurethane prepolymer to the N, N-bis [ (trimethoxysilyl) propyl ] amine is 112.1: 0.7. and 5% refers to the mass percentage of the blocked NCO groups in the NCO-terminated polyurethane prepolymer.
The prepared metal pole plate sealant still has excellent bonding force in a dry state or a soaking state (20 ℃ and 7 days), does not bubble in a high-temperature and high-humidity environment, is cured quickly (the curing time is about 10min at 120 ℃ and 65% RH), and has high strength and good storage stability.
Example 3
A preparation method of a metal pole plate sealant comprises the following steps: 178 parts of NCO-terminated polyurethane prepolymer, 16.8 parts of zinc oxide, 25 parts of talcum powder, 5 parts of hydrogenated castor oil and 5 parts of titanium dioxide are sequentially added into a round-bottom flask, stirred by magnetic force (50Hz) for 2 hours until the materials are uniform, and then condensed and refluxed at 85 ℃ for 24 hours to obtain the metal pole plate sealant; the parts are parts by mass. The prepared metal pole plate sealant is viscous and has excellent bonding effect.
The NCO-terminated polyurethane prepolymer is prepared by the following method: condensing and refluxing 80 Parts of Polypropylene Glycol (PPG), 6 parts of 2, 4-toluene diisocyanate (2,4-TDI), 18 Parts of Polytrimethylene Terephthalate (PPT) and 8 parts of stannous octoate at 80 ℃ for 12 hours to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
The NCO-terminated polyurethane prepolymer is pretreated by the following method: condensing and refluxing the NCO-terminated polyurethane prepolymer and N, N-bis [ (trimethoxysilyl) propyl ] amine at 90 ℃ for 24 hours to obtain an NCO-terminated prepolymer with the content of about 5%; the percentage is mass percentage. The mass ratio of the NCO-terminated polyurethane prepolymer to the N, N-bis [ (trimethoxysilyl) propyl ] amine is 112.1: 0.7. and 5% refers to the mass percentage of the blocked NCO groups in the NCO-terminated polyurethane prepolymer.
The prepared metal pole plate sealant still has excellent bonding force in a dry state or a soaking state (20 ℃ and 7 days), does not bubble in a high-temperature and high-humidity environment, is cured quickly (the curing time is about 10min at 120 ℃ and 65% RH), and has high strength and good storage stability.
Example 4
A preparation method of a metal pole plate sealant comprises the following steps: 178 parts of NCO-terminated polyurethane prepolymer, 16.8 parts of zinc oxide, 25 parts of talcum powder, 5 parts of hydrogenated castor oil and 5 parts of titanium dioxide are sequentially added into a round-bottom flask, stirred by magnetic force (50Hz) for 2 hours until the materials are uniform, and then condensed and refluxed at 90 ℃ for 12 hours to obtain the metal pole plate sealant; the parts are parts by mass. The prepared metal pole plate sealant is viscous and has excellent bonding effect.
The NCO-terminated polyurethane prepolymer is prepared by the following method: condensing and refluxing 70 Parts of Polypropylene Glycol (PPG), 3 parts of 2, 4-toluene diisocyanate (2,4-TDI), 20 Parts of Polytrimethylene Terephthalate (PPT) and 8 parts of stannous octoate at 90 ℃ for 18h to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
The NCO-terminated polyurethane prepolymer is pretreated by the following method: condensing and refluxing the NCO-terminated polyurethane prepolymer and N, N-bis [ (trimethoxysilyl) propyl ] amine at 85 ℃ for 36 hours to obtain an NCO-terminated prepolymer with the content of about 5 percent; the percentage is mass percentage. The mass ratio of the NCO-terminated polyurethane prepolymer to the N, N-bis [ (trimethoxysilyl) propyl ] amine is 112.1: 0.7. and 5% refers to the mass percentage of the blocked NCO groups in the NCO-terminated polyurethane prepolymer.
The prepared metal pole plate sealant still has excellent bonding force in a dry state or a soaking state (20 ℃ and 7 days), does not bubble in a high-temperature and high-humidity environment, is cured quickly (the curing time is about 10min at 120 ℃ and 65% RH), and has high strength and good storage stability.
Comparative example 1
A preparation method of a metal pole plate sealant comprises the following steps: 178 parts of NCO-terminated polyurethane prepolymer, 16.8 parts of zinc oxide, 25 parts of talcum powder, 5 parts of hydrogenated castor oil and 5 parts of titanium dioxide are sequentially added into a round-bottom flask, stirred by magnetic force (50Hz) for 2 hours until the materials are uniform, and then condensed and refluxed at 85 ℃ for 24 hours to obtain the metal pole plate sealant; the parts are parts by mass. The prepared metal pole plate sealant is viscous and has excellent bonding effect.
The NCO-terminated polyurethane prepolymer is prepared by the following method: condensing and refluxing 70 Parts of Polypropylene Glycol (PPG), 6 parts of 2, 4-toluene diisocyanate (2,4-TDI), 20 Parts of Polytrimethylene Terephthalate (PPT) and 8 parts of stannous octoate at 90 ℃ for 18h to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
In this example, the NCO-terminated polyurethane prepolymer was not pretreated. The prepared metal pole plate sealant has poor bonding force in a dry state or a soaking state (20 ℃ and 7 days), is easy to foam in a high-temperature and high-humidity environment, is slow to cure (the curing time is about 150min at 120 ℃ and 65% RH), has low strength and poor storage stability. The peeling strength of the metal plate sealant is schematically shown in fig. 2, and as can be seen from fig. 2, the prepared metal plate sealant has poor adhesion and large peeling strength fluctuation.
Method for testing peel strength of example of the invention as shown in fig. 3, a flexible adherend 4 is bonded to a rigid adherend 2 by holding the rigid adherend 2 with a chuck 1 and bonding the rigid adherend 2 to the flexible adherend 4 with a seal sample 3, while holding the flexible adherend 4 with a self-aligning chuck 5. The chucks 1 and 5 move up and down in opposite directions, and the moving speed is controlled to be 100mm/min, refer to GB/T2790-.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings, or any other related technical fields, which are directly or indirectly applied to the present invention, are included in the scope of the present invention.

Claims (9)

1. The metal pole plate sealant is characterized by comprising the following components in parts by mass: 10-200 parts of NCO-terminated polyurethane prepolymer, 5-20 parts of zinc oxide, 20-40 parts of talcum powder, 1-10 parts of hydrogenated castor oil and 5-20 parts of titanium dioxide.
2. The metal plate sealant according to claim 1, wherein the metal plate sealant comprises the following components in parts by mass: 178 parts of NCO-terminated polyurethane prepolymer, 16.8 parts of zinc oxide, 25 parts of talcum powder, 5 parts of hydrogenated castor oil and 5 parts of titanium dioxide.
3. The metal plate sealant as claimed in claim 1 or 2, wherein the NCO-terminated polyurethane prepolymer is prepared by the following method: condensing and refluxing 60-80 parts of polypropylene glycol, 1-10 parts of 2, 4-toluene diisocyanate, 10-30 parts of polytrimethylene terephthalate and 1-10 parts of stannous octoate at 80-100 ℃ for 12-48 h to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
4. The metal plate sealant according to claim 3, wherein the NCO-terminated polyurethane prepolymer is prepared by the following method: condensing and refluxing 70 parts of polypropylene glycol, 6 parts of 2, 4-toluene diisocyanate, 20 parts of polytrimethylene terephthalate and 8 parts of stannous octoate at 90 ℃ for 18 hours to obtain an NCO-terminated polyurethane prepolymer; the parts are parts by mass.
5. The metal plate sealant as claimed in claim 1 or 2, wherein the NCO group content of the NCO-terminated polyurethane prepolymer is 1-10% by mass.
6. The metal plate sealant as claimed in claim 1 or 2, wherein the NCO-terminated polyurethane prepolymer is pretreated by the following method: condensing and refluxing the NCO-terminated polyurethane prepolymer and N, N-bis [ (trimethoxysilyl) propyl ] amine at 80-100 ℃ for 12-48 h to obtain 5% NCO-terminated prepolymer; the percentage is mass percentage.
7. The metal plate sealant as claimed in claim 6, wherein the mass ratio of the NCO-terminated polyurethane prepolymer to the N, N-bis [ (trimethoxysilyl) propyl ] amine is (100-150): 0.7.
8. the method of preparing a metal plate sealant according to claim 1, comprising the steps of: sequentially adding 10-200 parts of NCO-terminated polyurethane prepolymer, 5-20 parts of zinc oxide, 20-40 parts of talcum powder, 1-10 parts of hydrogenated castor oil and 5-20 parts of titanium dioxide into a round-bottom flask, uniformly stirring by magnetic force, and carrying out condensation reflux reaction at 80-85 ℃ for 12-36 hours to obtain a metal pole plate sealant; the parts are parts by mass.
9. The method for preparing a metal plate sealant according to claim 8, wherein the magnetic stirring time is 2 hours.
CN202210863987.4A 2022-07-21 2022-07-21 Metal polar plate sealant and preparation method thereof Pending CN115124963A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115850642A (en) * 2022-12-05 2023-03-28 宁波聚泰新材料科技有限公司 Preparation method of high-performance polyurethane elastomer

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013095759A (en) * 2011-10-27 2013-05-20 Yokohama Rubber Co Ltd:The Polyurethane adhesive composition for resin glass
CN103897649A (en) * 2014-03-12 2014-07-02 南京艾布纳密封技术有限公司 Method for preparing single-component silane modified polyurethane sealant
CN103897650A (en) * 2014-03-17 2014-07-02 郑州大学 Hardly-foamed one-component polyurethane sealant
CN106589286A (en) * 2016-11-21 2017-04-26 万华化学集团股份有限公司 Silane modified polyurethane resin and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013095759A (en) * 2011-10-27 2013-05-20 Yokohama Rubber Co Ltd:The Polyurethane adhesive composition for resin glass
CN103897649A (en) * 2014-03-12 2014-07-02 南京艾布纳密封技术有限公司 Method for preparing single-component silane modified polyurethane sealant
CN103897650A (en) * 2014-03-17 2014-07-02 郑州大学 Hardly-foamed one-component polyurethane sealant
CN106589286A (en) * 2016-11-21 2017-04-26 万华化学集团股份有限公司 Silane modified polyurethane resin and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115850642A (en) * 2022-12-05 2023-03-28 宁波聚泰新材料科技有限公司 Preparation method of high-performance polyurethane elastomer

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Application publication date: 20220930