CN114085639B - Adhesive for C-grade insulating paper composite material and preparation method thereof - Google Patents

Adhesive for C-grade insulating paper composite material and preparation method thereof Download PDF

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CN114085639B
CN114085639B CN202111603135.3A CN202111603135A CN114085639B CN 114085639 B CN114085639 B CN 114085639B CN 202111603135 A CN202111603135 A CN 202111603135A CN 114085639 B CN114085639 B CN 114085639B
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parts
curing agent
ethyl acetate
adhesive
insulating paper
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CN114085639A (en
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隋学斌
范卫东
赫长生
丛斌
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Nantong Comens New Materials Co ltd
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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
    • C09J175/06—Polyurethanes from polyesters
    • 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
    • C08G18/4045—Mixtures of compounds of group C08G18/58 with other macromolecular compounds
    • 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
    • C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
    • C08G18/4247—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids
    • C08G18/425—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids the polyols containing one or two ether 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
    • C08G18/40—High-molecular-weight compounds
    • C08G18/58—Epoxy resins
    • 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
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
    • C08G18/778—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur silicon

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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)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses an adhesive for a C-level insulating paper composite material and a preparation method thereof, wherein the adhesive comprises a main agent and a curing agent; the weight ratio of the main agent to the curing agent is 10: 2; the main agent is an ethyl acetate solution containing high molecular weight polyester polyol and bisphenol A type epoxy resin, the rotational viscosity of the main agent is 600-1000 mPa & s at 25 ℃, and the solid content is 68-70%; the curing agent is an ethyl acetate solution containing polysilazane resin modified isocyanate prepolymer, the rotational viscosity of the curing agent is 600-1200 mPa & s at 25 ℃, the solid content is 58-62%, and the-NCO content is 8-10%. The invention has excellent adhesive property and high temperature resistance, can meet the composite requirement of a C-grade insulating paper composite material, and has excellent initial adhesion and final adhesion strength between Nomex paper/PET film and Nomex paper/PA film.

Description

Adhesive for C-grade insulating paper composite material and preparation method thereof
Technical Field
The invention relates to the field of chemical adhesives, in particular to an adhesive for a C-grade insulating paper composite material and a preparation method thereof.
Background
Nomex insulating paper has the characteristics of good mechanical strength, electrical performance, thermal stability, chemical compatibility and the like, and is widely applied to F-class motors and C-class motors. With the development of science and technology, the fields of aerospace, high-speed trains and the like put forward higher requirements on the capacity of motors, electrical equipment tends to be miniaturized and large in capacity, and higher requirements on the high temperature resistance, the strength performance, the insulating performance and the like of insulating materials are put forward.
The traditional motor insulating material mainly comprises pure insulating paper, pure insulating films and flexible insulating materials formed by compounding the insulating paper and the insulating films in a multi-layer mode. These insulation materials are classified as class a (maximum allowable temperature of at least 105 ℃, e.g., conventional kraft paper), class E (maximum allowable temperature of at least 120 ℃, e.g., american west house electrical)Company rate earlier than the 20 th century and the 50 th era, heat-modified cellulose insulating Paper TUK Paper was developed
Figure BDA0003432711270000011
) Class B (maximum allowable temperature at least 130 deg.C), new type high temperature resistant insulating paper developed by DuPont in U.S. through mixed-sheet process
Figure BDA0003432711270000012
T910), class H (maximum allowable temperature of at least 180 ℃, e.g. flexible insulating paper composite NHN, NMN, etc.), class C (maximum allowable temperature of at least 220 ℃, e.g. dupont, usa)
Figure BDA0003432711270000013
410 insulating paper). The C-grade insulating paper composite material has higher high temperature resistance, oil resistance, damp-heat aging resistance and other performances, which provides higher high temperature resistance, oil resistance, damp-heat aging resistance and other performance requirements for the used composite adhesive, and the existing polyurethane adhesive is difficult to meet the requirements.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide an adhesive for a C-grade insulating paper composite material and a preparation method thereof, which are used for solving the technical problems in the prior art. The invention has excellent adhesive property and high temperature resistance, can meet the composite requirement of a C-grade insulating paper composite material, has excellent initial adhesion and final adhesion strength between Nomex paper/PET film and Nomex paper/PA film, and can be used for the composite of flexible insulating paper composite material NMN (Nomex paper/PET/Nomex paper) and NHN (Nomex paper/PA/Nomex paper) structures.
The purpose of the invention is realized by the following technical scheme:
an adhesive for a C-grade insulating paper composite material comprises a main agent and a curing agent; the weight ratio of the main agent to the curing agent is 10: 2; the main agent is an ethyl acetate solution containing high molecular weight polyester polyol and bisphenol A type epoxy resin, the rotational viscosity of the main agent is 600-1000 mPa & s at 25 ℃, and the solid content is 68-70%; the curing agent is an ethyl acetate solution containing polysilazane resin modified isocyanate prepolymer, the rotational viscosity of the curing agent is 600-1200 mPa & s at 25 ℃, the solid content is 58-62%, and the-NCO content is 8-10%.
Preferably, the relative molecular mass of the high molecular weight polyester polyol in the main agent is 8000-10000, the acid value is less than 2mgKOH/g, the hydroxyl value is 10-15 mgKOH/g, and the glass transition temperature is-10-5 ℃.
Preferably, the main agent is mainly prepared from the following raw materials in parts by weight: 50-58 parts of high molecular weight polyester polyol, 16-22 parts of bisphenol A epoxy resin and 30-32 parts of ethyl acetate; the curing agent is mainly prepared from the following raw materials in parts by weight: 70-78 parts of isocyanate prepolymer solution, 1-3 parts of polysilazane resin and 23-27 parts of ethyl acetate;
the high molecular weight polyester polyol is mainly prepared from the following raw materials in parts by weight: 8-25 parts of isophthalic acid, 8-25 parts of terephthalic acid, 12-24 parts of adipic acid, 12-24 parts of diethylene glycol, 20-34 parts of 1, 6-hexanediol, 0.002-0.006 part of catalyst and 0.01-0.03 part of antioxidant.
Preferably, the isocyanate prepolymer solution employs an aromatic isocyanate curing agent.
Preferably, the bisphenol A epoxy resin has an epoxy value of 0.2-0.52.
A preparation method of a binder for a C-grade insulating paper composite material is used for preparing the binder for the C-grade insulating paper composite material, and comprises the following steps: preparing a main agent and a curing agent;
the preparation of the main agent comprises the following steps: adding high molecular weight polyester polyol, bisphenol A epoxy resin and ethyl acetate into a reaction kettle, heating to 80-90 ℃, stirring for 3-4 hours, uniformly mixing, and cooling to room temperature to prepare an ethyl acetate solution with solid content of 68-70% and rotary viscosity of 600-1000 mPa & s at 25 ℃, namely a main agent;
the preparation of the curing agent comprises: adding an isocyanate prepolymer solution, polysilazane resin and ethyl acetate into another reaction kettle, heating to 70-80 ℃, reacting for 3-4 hours, and cooling to room temperature to prepare an ethyl acetate solution which has a solid content of 58-62%, an NCO content of 8-10% and a rotational viscosity of 600-1200 mPa & s at 25 ℃ as a curing agent;
and mixing the main agent and the curing agent according to the weight ratio of 10:2 to obtain the adhesive for the C-grade insulating paper composite material.
Preferably, the main agent is mainly prepared from the following raw materials in parts by weight: 50-58 parts of high molecular weight polyester polyol, 16-22 parts of bisphenol A epoxy resin and 30-32 parts of ethyl acetate; the curing agent is mainly prepared from the following raw materials in parts by weight: 70-78 parts of isocyanate prepolymer solution, 1-3 parts of polysilazane resin and 23-27 parts of ethyl acetate.
Preferably, the preparation method of the high molecular weight polyester polyol comprises:
weighing the following raw materials in parts by weight: 8-25 parts of isophthalic acid, 8-25 parts of terephthalic acid, 12-24 parts of adipic acid, 12-24 parts of diethylene glycol, 20-34 parts of 1, 6-hexanediol, 0.002-0.006 part of catalyst and 0.01-0.03 part of antioxidant;
esterification reaction: adding diethylene glycol, adipic acid, isophthalic acid, terephthalic acid, 1, 6-hexanediol, a catalyst and an antioxidant into a polyester synthesis kettle, heating to 120 ℃, preserving heat for 1h, after the solid raw materials are completely dissolved, gradually heating to 210-230 ℃ at the heating rate of 10 ℃/30min, controlling the water outlet speed, controlling the temperature of a fractionating column to be not higher than 110 ℃, and reacting for 6-10 h to complete the esterification reaction; the water yield accounts for 10-15% of the total weight of the raw materials, and the acid value of the esterification product is less than or equal to 15 mgKOH/g;
and (3) polycondensation reaction: after the esterification reaction is finished, vacuumizing the polyester synthesis kettle for 30 minutes according to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, controlling the kettle temperature of the polyester synthesis kettle to be 245-255 ℃, then carrying out long vacuumizing operation, wherein the vacuum degree reaches-0.1 MPa, the long vacuumizing time is 3-4 hours, the distilled alcohol of the polyester synthesis kettle accounts for 4-8% of the total weight of the raw materials after long vacuumizing, the obtained hydroxyl value is 10-15 mgKOH/g, the acid value is less than or equal to 2mgKOH/g, the glass transition temperature is-10-5 ℃, and the final product with the relative molecular mass of 8000-10000 is the high molecular weight polyester polyol.
Compared with the prior art, the adhesive for the C-grade insulating paper composite material comprises a main agent and a curing agent, wherein the main agent adopts high molecular weight polyester polyol with a specific structural design as a main component, and the high molecular weight polyester polyol has excellent initial adhesion and final adhesion strength between Nomex paper/PET film and Nomex paper/PA film after reacting with the curing agent. The main agent adopts the flexible chain segment polyester resin which takes diethylene glycol and 1, 6-hexanediol type polyhydric alcohol as main raw materials, and has excellent bonding strength to Nomex insulating paper, PET sheets and PA films; by adding the bisphenol A type epoxy resin, the adhesive force to the PET sheet and the PA film can be enhanced, and the heat resistance of the adhesive layer at high temperature can be improved. The curing agent adopts polysilazane resin modified isocyanate prepolymer with excellent high temperature resistance and corrosion resistance, and the curing agent has excellent bonding strength to Nomex paper materials after being crosslinked and cured with the main agent, and has excellent high temperature resistance, oil resistance, corrosion resistance, acid and alkali resistance and other properties. The composite adhesive composed of the main agent and the curing agent is used for composite bonding of C-grade insulating paper composite materials, and can meet the requirements of the composite adhesive on the properties of bonding, high temperature resistance, hydrolysis resistance, alkali resistance, chemical resistance and the like.
Detailed Description
The technical scheme in the embodiment of the invention is clearly and completely described below; it is to be understood that the described embodiments are merely exemplary of the invention, and are not intended to limit the invention to the particular forms disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The terms that may be used herein are first described as follows:
the terms "comprising," "including," "containing," "having," or other similar terms of meaning should be construed as non-exclusive inclusions. For example: including a feature (e.g., material, component, ingredient, carrier, formulation, material, dimension, part, component, mechanism, device, process, procedure, method, reaction condition, processing condition, parameter, algorithm, signal, data, product, or article of manufacture), is to be construed as including not only the particular feature explicitly listed but also other features not explicitly listed as such which are known in the art.
The term "consisting of … …" is meant to exclude any technical feature elements not explicitly listed. If used in a claim, the term shall render the claim closed except for the inclusion of the technical features that are expressly listed except for the conventional impurities associated therewith. If the term occurs in only one clause of the claims, it is defined only as specifically listed in that clause, and elements recited in other clauses are not excluded from the overall claims.
The term "parts by weight" is intended to indicate the relationship of mass proportions between the various components, for example: if X parts by weight of the X component and Y parts by weight of the Y component are described, the mass ratio of the X component to the Y component is X: Y; 1 part by weight may represent any mass, for example: 1 part by weight may be expressed as 1kg or 3.1415926 kg. The sum of the parts by weight of all components is not necessarily 100 parts and may be greater than 100 parts, less than 100 parts or equal to 100 parts. Parts, ratios and percentages described herein are by mass unless otherwise indicated.
When concentrations, temperatures, pressures, dimensions, or other parameters are expressed as ranges of values, the ranges are to be understood as specifically disclosing all ranges formed from any pair of upper, lower, and preferred values within the range, regardless of whether ranges are explicitly recited; for example, if a numerical range of "2 ~ 8" is recited, then the numerical range should be interpreted to include ranges of "2 ~ 7", "2 ~ 6", "5 ~ 7", "3 ~ 4 and 6 ~ 7", "3 ~ 5 and 7", "2 and 5 ~ 7", and the like. Unless otherwise indicated, the numerical ranges recited herein include both the endpoints thereof and all integers and fractions within the numerical range.
The binder for the grade C insulating paper composite material and the preparation method thereof provided by the present invention are described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to a person skilled in the art. Those not specifically mentioned in the examples of the present invention were carried out according to the conventional conditions in the art or conditions suggested by the manufacturer. The reagents or instruments used in the examples of the present invention are not specified by manufacturers, and are all conventional products available by commercial purchase.
Adhesive for C-grade insulating paper composite material
The invention provides an adhesive for a C-grade insulating paper composite material, which comprises a main agent and a curing agent; the weight ratio of the main agent to the curing agent is 10: 2; wherein the content of the first and second substances,
the main agent is an ethyl acetate solution containing high molecular weight polyester polyol and bisphenol A type epoxy resin, the rotational viscosity of the main agent is 600-1000 mPa & s at 25 ℃, and the solid content is 68-70%;
the curing agent is an ethyl acetate solution containing polysilazane resin modified isocyanate prepolymer, the rotational viscosity of the curing agent is 600-1200 mPa & s at 25 ℃, the solid content is 58-62%, and the-NCO content is 8-10%.
Specifically, the adhesive for the grade C insulating paper composite material includes the following embodiments:
(1) the main agent is mainly prepared from the following raw materials in parts by weight: 50-58 parts of high molecular weight polyester polyol, 16-22 parts of bisphenol A epoxy resin and 30-32 parts of ethyl acetate.
(2) The curing agent is mainly prepared from the following raw materials in parts by weight: 70-78 parts of isocyanate prepolymer solution, 1-3 parts of polysilazane resin and 23-27 parts of ethyl acetate.
(3) In the main agent, the relative molecular mass of the high molecular weight polyester polyol is 8000-10000, the acid value is less than 2mgKOH/g, the hydroxyl value is 10-15 mgKOH/g, and the glass transition temperature is-10-5 ℃. The high molecular weight polyester polyol of the main agent is prepared by taking isophthalic acid, terephthalic acid, adipic acid, diethylene glycol and 1, 6-hexanediol as raw materials, adding a catalyst and an antioxidant, and carrying out esterification and polycondensation; the high molecular weight polyester polyol is mainly prepared from the following raw materials in parts by weight: 8-25 parts of isophthalic acid, 8-25 parts of terephthalic acid, 12-24 parts of adipic acid, 12-24 parts of diethylene glycol, 20-34 parts of 1, 6-hexanediol, 0.002-0.006 part of catalyst and 0.01-0.03 part of antioxidant; the catalyst adopts one of stannous octoate, antimony trioxide, dibutyltin dilaurate, antimony acetate or tetra-n-butyl titanate; the antioxidant is one of pentaerythritol tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and isooctyl 3, 5-di-tert-butyl-4-hydroxyphenyl propionate.
(4) In the main component, the bisphenol A epoxy resin has an epoxy value of 0.2 to 0.52, and preferably any one of bisphenol A epoxy resins E51, E44, E32, E20, and the like is used.
(5) As the curing agent, any one of aromatic isocyanate curing agents such as Bayer aromatic curing agent L-75 and Korean aromatic curing agent L-75 is used for the isocyanate prepolymer solution.
(6) In the curing agent, the polysilazane resin is any one of KB-8812, KB-8806 and KB-8801 which have a molecular weight of 2000-6000 and are produced by Kubei chemical technology.
Preparation method of adhesive for C-grade insulating paper composite material
The invention also provides a preparation method of the adhesive for the C-grade insulating paper composite material, which is used for preparing the adhesive for the C-grade insulating paper composite material and comprises the following steps: preparing a main agent and a curing agent; wherein the content of the first and second substances,
the preparation of the main agent comprises the following steps: weighing the following raw materials in parts by weight: 50-58 parts of high molecular weight polyester polyol, 16-22 parts of bisphenol A epoxy resin and 30-32 parts of ethyl acetate. Adding high molecular weight polyester polyol, bisphenol A epoxy resin and ethyl acetate into a reaction kettle, heating to 80-90 ℃, stirring for 3-4 hours, uniformly mixing, and cooling to room temperature to prepare an ethyl acetate solution with solid content of 68-70% and rotary viscosity of 600-1000 mPa & s at 25 ℃, wherein the ethyl acetate solution is a main agent (namely the ethyl acetate solution containing the high molecular weight polyester polyol and the bisphenol A epoxy resin).
The preparation of the curing agent comprises: weighing the following raw materials in parts by weight: 70-78 parts of isocyanate prepolymer solution, 1-3 parts of polysilazane resin and 23-27 parts of ethyl acetate. Adding the isocyanate prepolymer solution, the polysilazane resin and ethyl acetate into another reaction kettle, heating to 70-80 ℃, reacting for 3-4 hours, and cooling to room temperature to prepare an ethyl acetate solution with a solid content of 58-62%, an NCO content of 8-10% and a rotational viscosity of 600-1200 mPa & s at 25 ℃, namely the curing agent (namely the ethyl acetate solution containing the polysilazane resin modified isocyanate prepolymer).
And mixing the main agent and the curing agent according to the weight ratio of 10:2 to obtain the adhesive for the C-grade insulating paper composite material.
Specifically, the preparation method of the adhesive for the C-grade insulating paper composite material comprises the following embodiments:
(1) in the main component, the bisphenol A epoxy resin has an epoxy value of 0.2 to 0.52, and preferably any one of bisphenol A epoxy resins E51, E44, E32, E20, and the like is used.
(2) As the curing agent, any one of aromatic isocyanate curing agents such as Bayer aromatic curing agent L-75 and Korean aromatic curing agent L-75 is used for the isocyanate prepolymer solution.
(3) In the curing agent, the polysilazane resin is any one of KB-8812, KB-8806 and KB-8801 which have a molecular weight of 2000-6000 and are derived from Kubei chemical.
(4) In the main agent, the preparation method of the high molecular weight polyester polyol comprises the following steps:
weighing the following raw materials in parts by weight: 8-25 parts of isophthalic acid, 8-25 parts of terephthalic acid, 12-24 parts of adipic acid, 12-24 parts of diethylene glycol, 20-34 parts of 1, 6-hexanediol, 0.002-0.006 part of catalyst and 0.01-0.03 part of antioxidant;
esterification reaction: adding diethylene glycol, adipic acid, isophthalic acid, terephthalic acid, 1, 6-hexanediol, a catalyst and an antioxidant into a polyester synthesis kettle, heating to 120 ℃, keeping the temperature for 1h, gradually heating the kettle to 210-230 ℃ at the heating rate of 10 ℃/30min after the solid raw materials are completely dissolved, controlling the water outlet speed, controlling the temperature of a fractionating column to be not higher than 110 ℃, and reacting for 6-10 h to complete the esterification reaction; the water yield accounts for 10-15% of the total weight of the raw materials, and the acid value of the esterification product is less than or equal to 15 mgKOH/g;
and (3) polycondensation reaction: after the esterification reaction is finished, vacuumizing the polyester synthesis kettle for 30 minutes according to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, controlling the kettle temperature of the polyester synthesis kettle to be 245-255 ℃, and then carrying out long vacuumizing operation, wherein the vacuum degree reaches-0.1 MPa, the long vacuumizing time is 3-4 hours, the distilled alcohol of the polyester synthesis kettle accounts for 4-8% of the total weight of the raw materials after long vacuumizing, the hydroxyl value obtained after discharging is 10-15 mgKOH/g, the acid value is less than or equal to 2mgKOH/g, the glass transition temperature is-10-5 ℃, and the final product with the relative molecular mass of 8000-10000 is the high molecular weight polyester polyol.
Furthermore, the adhesive for the C-grade insulating paper composite material provided by the invention is composed of a main agent and a curing agent; wherein the main agent is ethyl acetate solution of high molecular weight polyester polyol synthesized by isophthalic acid, terephthalic acid, adipic acid, 1, 6-hexanediol, diethylene glycol and the like and bisphenol A epoxy resin; the curing agent is an ethyl acetate solution of an isocyanate prepolymer modified with a polysilazane resin, which is obtained by reacting a polysilazane resin with an isocyanate prepolymer solution. The main agent and the curing agent can be directly used for bonding and compounding the C-grade insulating paper composite material after being mixed according to a certain proportion. MNM insulating paper structures (Nomex paper/PET/Nomex paper) and NHN insulating paper structures (Nomex paper/PA/Nomex paper) made of cured products have excellent performances such as peeling strength, high temperature resistance and the like, and can meet the use requirements of C-grade flexible insulating paper composite materials.
Compared with the prior art, the addition amount of bisphenol A epoxy resin is increased in the main agent, short-oil alkyd resin is not needed, and polysilazane resin is adopted in the curing agent to modify isocyanate prepolymer, so that the high-temperature resistance of the invention is greatly improved, the excellent adhesive property of the invention is ensured, and the composite requirement of a C-grade insulating paper composite material can be met.
In conclusion, the embodiment of the invention has excellent bonding performance and high temperature resistance, can meet the compounding requirement of a C-grade insulating paper composite material, has excellent initial adhesion and final adhesion strength between Nomex paper/PET film and Nomex paper/PA film, and can be used for compounding flexible insulating paper composite materials NMN (Nomex paper/PET/Nomex paper) and NHN (Nomex paper/PA/Nomex paper).
In order to more clearly show the technical scheme and the technical effects provided by the present invention, the binder for the grade C insulating paper composite material and the preparation method thereof provided by the present invention are described in detail with specific examples.
Example 1
The adhesive for the C-grade insulating paper composite material is prepared by the following steps: preparing high molecular weight polyester polyol, preparing a main agent and preparing a curing agent;
(1) preparing high molecular weight polyester polyol:
esterification reaction: sequentially adding 22 parts by weight of adipic acid, 22 parts by weight of diethylene glycol, 16 parts by weight of isophthalic acid, 16 parts by weight of terephthalic acid, 24 parts by weight of 1, 6-hexanediol, 0.003 part by weight of antimony trioxide and 0.02 part by weight of 3, 5-di-tert-butyl-4-hydroxy-ethyl-benzenepropanoate into a polyester synthesis kettle, fully and uniformly stirring, heating to 120 ℃, keeping the temperature for 1h, gradually heating the kettle to 210-230 ℃ at the heating rate of 10 ℃/30min after solid raw materials are completely dissolved, controlling the water outlet speed, controlling the temperature of a fractionating column to be not higher than 110 ℃, and reacting for 6-10 h to complete the esterification reaction; the water yield was 12 parts by weight, and the acid value of the esterification product was 12 mgKOH/g.
And (3) polycondensation reaction: after the esterification reaction is finished, vacuumizing the polyester synthesis kettle, pre-vacuumizing for 30 minutes in sequence of-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, controlling the kettle temperature of the polyester synthesis kettle to be 245-255 ℃, then carrying out long-time vacuumizing operation, wherein the vacuum degree reaches-0.1 MPa, the long-time vacuumizing is 4 hours, the distillate is 4.5 parts by weight, discharging to obtain a final product with the hydroxyl value of 12mgKOH/g, the acid value of 0.05mgKOH/g, the glass transition temperature of-5 ℃, and the relative molecular mass of 9000, namely the high molecular weight polyester polyol.
(2) Preparing a main agent: adding 54 parts by weight of the high molecular weight polyester polyol, 16 parts by weight of bisphenol A epoxy resin E4416 and 30 parts by weight of ethyl acetate into a reaction kettle, heating to 80-90 ℃, stirring and dissolving for 4 hours, fully and uniformly mixing, and cooling to room temperature to prepare an ethyl acetate solution (namely the ethyl acetate solution containing the high molecular weight polyester polyol and the bisphenol A epoxy resin) with a solid content of 70% and a rotational viscosity of 800mPa & s at 25 ℃, wherein the ethyl acetate solution is a main agent.
(3) Preparing a curing agent: adding Kesimao L-7576 parts by weight of aromatic isocyanate curing agent, KB-88061 parts by weight of polysilazane resin with molecular weight of 2000-6000 and 23 parts by weight of ethyl acetate into another reaction kettle, heating to 70-80 ℃, reacting for 4 hours, and cooling to room temperature to prepare an ethyl acetate solution with solid content of 58%, -NCO content of 9.5% and rotational viscosity of 1100mPa & s at 25 ℃, namely the curing agent (namely the ethyl acetate solution containing polysilazane resin modified isocyanate prepolymer).
And mixing the main agent and the curing agent according to the weight ratio of 10:2 to obtain the adhesive for the C-grade insulating paper composite material.
Specifically, the adhesive for the grade-C insulating paper composite material obtained in the embodiment 1 of the invention is used for composite bonding of an MNM insulating paper structure (Nomex paper/PET/Nomex paper) and an NHN insulating paper structure (Nomex paper/PA/Nomex paper), and after curing for 72 hours at 60 ℃, Nomex paper is peeled or cannot be peeled off between layers of the composite material; the composite film is directly baked at 240 ℃ for 10min and subjected to a high-temperature-resistant experiment, and the foaming and delamination phenomena are avoided. The mechanical property and the high temperature resistance of the composite film can meet the use requirement of the C-level flexible insulating paper composite material.
Example 2
The adhesive for the C-grade insulating paper composite material is prepared by the following steps: preparing high molecular weight polyester polyol, preparing a main agent and preparing a curing agent;
(1) preparing high molecular weight polyester polyol:
esterification reaction: sequentially adding 12 parts by weight of adipic acid, 12 parts by weight of diethylene glycol, 25 parts by weight of isophthalic acid, 17 parts by weight of terephthalic acid, 34 parts by weight of 1, 6-hexanediol, 0.004 part by weight of tetra-n-butyl titanate and 0.01 part by weight of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester into a polyester synthesis kettle, fully and uniformly stirring, heating to 120 ℃, keeping the temperature for 1h, gradually heating the kettle to 210-230 ℃ at a heating rate of 10 ℃/30min after solid raw materials are completely dissolved, controlling the water discharging speed, controlling the temperature of a fractionating column to be not higher than 110 ℃, and reacting for 6-10 h to complete the esterification reaction; the water yield was 12.5 parts by weight, and the acid value of the esterified product was 10 mgKOH/g.
And (3) polycondensation reaction: after the esterification reaction is finished, vacuumizing the polyester synthesis kettle, pre-vacuumizing for 30 minutes in sequence of-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, controlling the kettle temperature of the polyester synthesis kettle to be 245-255 ℃, and then carrying out long vacuumizing operation, wherein the vacuum degree reaches-0.1 MPa, the long vacuumizing time is 3.5 hours, the distilled alcohol of the polyester synthesis kettle accounts for about 5% of the total weight of the raw materials after long vacuumizing, the hydroxyl value is 10mgKOH/g, the acid value is 0.08mgKOH/g, the glass transition temperature is-2 ℃, and the final product with the relative molecular mass of 10000 is the high molecular weight polyester polyol.
(2) Preparing a main agent: adding 50 parts by weight of the high molecular weight polyester polyol, 5119 parts by weight of bisphenol A epoxy resin E and 31 parts by weight of ethyl acetate into a reaction kettle, heating to 80-90 ℃, stirring and dissolving for 4 hours, fully and uniformly mixing, and cooling to room temperature to prepare an ethyl acetate solution with solid content of 69% and rotational viscosity of 900mPa & s at 25 ℃, namely a main agent (namely the ethyl acetate solution containing the high molecular weight polyester polyol and the bisphenol A epoxy resin).
(3) Preparing a curing agent: adding Kesimao L-7576 parts by weight of aromatic isocyanate curing agent, 2000-6000 parts by weight of polysilazane resin KB-88121 parts by weight of Kubei chemical molecular weight and 23 parts by weight of ethyl acetate into another reaction kettle, heating to 70-80 ℃, reacting for 4 hours, and cooling to room temperature to prepare an ethyl acetate solution with solid content of 59%, -NCO content of 9.0%, and rotational viscosity of 900mPa s at 25 ℃, namely the curing agent (namely the ethyl acetate solution containing polysilazane resin modified isocyanate prepolymer).
And mixing the main agent and the curing agent according to the weight ratio of 10:2 to obtain the adhesive for the C-grade insulating paper composite material.
Example 3
The adhesive for the C-grade insulating paper composite material is prepared by the following steps: preparing high molecular weight polyester polyol, preparing a main agent and preparing a curing agent;
(1) preparing high molecular weight polyester polyol:
esterification reaction: sequentially adding 24 parts by weight of adipic acid, 24 parts by weight of diethylene glycol, 8 parts by weight of isophthalic acid, 24 parts by weight of terephthalic acid, 20 parts by weight of 1, 6-hexanediol, 0.006 part by weight of antimony acetate and 0.03 part by weight of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate into a polyester synthesis kettle, fully and uniformly stirring, heating to 120 ℃, keeping the temperature for 1h, gradually heating the kettle to 210-230 ℃ at the heating speed of 10 ℃/30min after the solid raw materials are completely dissolved, controlling the water outlet speed, controlling the temperature of a fractionating column to be not higher than 110 ℃, and reacting for 6-10 h to complete the esterification reaction; the water yield was 13 parts by weight, and the acid value of the esterification product was 15 mgKOH/g.
And (3) polycondensation reaction: after the esterification reaction is finished, vacuumizing the polyester synthesis kettle for 30 minutes according to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, controlling the kettle temperature of the polyester synthesis kettle to be 245-255 ℃, then carrying out long vacuumizing operation, wherein the vacuum degree reaches-0.1 MPa, the long vacuumizing time is 4 hours, the polycondensation distillate is 4.6 parts by weight, discharging to obtain the final product with the hydroxyl value of 14mgKOH/g, the acid value of 0.02mgKOH/g, the glass transition temperature of 4 ℃, and the relative molecular mass of 8000, namely the high molecular weight polyester polyol.
(2) Preparing a main agent: adding 50 parts by weight of the high molecular weight polyester polyol, 2018 parts by weight of bisphenol A epoxy resin E and 32 parts by weight of ethyl acetate into a reaction kettle, heating to 80-90 ℃, stirring and dissolving for 4 hours, fully and uniformly mixing, and cooling to room temperature to prepare an ethyl acetate solution with solid content of 68% and rotational viscosity of 700mPa & s at 25 ℃, namely a main agent (namely the ethyl acetate solution containing the high molecular weight polyester polyol and the bisphenol A epoxy resin).
(3) Preparing a curing agent: adding aromatic isocyanate curing agent Umai L-7570 parts by weight, polysilazane resin KB-88013 with molecular weight of 2000-6000 and ethyl acetate 27 parts by weight of Kubei chemical, heating to 70-80 ℃, reacting for 4 hours, cooling to room temperature, and preparing an ethyl acetate solution with solid content of 58%, -NCO content of 8.2% and rotational viscosity of 1200mPa s at 25 ℃, namely the curing agent (namely the ethyl acetate solution containing the polysilazane resin modified isocyanate prepolymer).
And mixing the main agent and the curing agent according to the weight ratio of 10:2 to obtain the adhesive for the C-grade insulating paper composite material.
Comparative example 1
The preparation method of the adhesive for the H-grade insulating paper composite material comprises the following steps:
(1) preparation of high molecular weight polyester polyols
Esterification reaction: adding 29 parts by weight of sebacic acid, 23 parts by weight of neopentyl glycol and 5 parts by weight of deionized water into a polyester synthesis kettle, heating and starting stirring, heating to 80 ℃, preserving heat for 2 hours to completely dissolve and uniformly mix solid raw materials, and gradually continuing heating the kettle to 125 ℃ to evaporate water; after the water is completely evaporated, keeping the temperature of the kettle unchanged, adding 18 parts by weight of isophthalic acid, 15 parts by weight of phthalic anhydride, 15 parts by weight of 1, 4-butanediol and 0.006 part by weight of antimony acetate into the polyester synthesis kettle, fully and uniformly stirring, heating to 210-230 ℃, and reacting for 6 hours to complete the esterification reaction; the total effluent amount is 10 parts by weight, and the acid value of the esterification product is 10 mgKOH/g;
and (3) polycondensation reaction: and after the esterification reaction is finished, vacuumizing the polyester synthesis kettle, and pre-vacuumizing for 40 minutes in sequence of-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, wherein the kettle temperature of the polyester synthesis kettle is controlled to be 245-255 ℃, long vacuumizing operation is performed after pre-vacuumizing is finished, the vacuum degree reaches-0.1 MPa, the long vacuumizing time is 8 hours, the distilled alcohol of the polyester synthesis kettle is 9 parts by weight after long vacuumizing, the hydroxyl value obtained after discharging is 6mgKOH/g, the acid value is 0.01mgKOH/g, the glass transition temperature is 4 ℃, and the final product with the relative molecular mass of 15000 is the high molecular weight polyester polyol.
(2) Preparation of the base
Adding 45 parts by weight of the prepared high molecular weight polyester polyol, 2012 parts by weight of bisphenol A epoxy resin E and ETERKYD (short soybean oil alkyd resin) into a reaction kettle TM 31065 and 38 parts by weight of ethyl acetate, heating to 80-90 deg.C, stirring for 4 hr, mixing, and cooling to room temperature to obtain ethyl acetate solution with solid content of 62% and rotary viscosity of 1000 mPa.s at 25 deg.C as main agent.
(3) Preparation of the curing agent
Adding polycaprolactone diol Capa into another reaction kettle TM 21019 parts by weight, 38 parts by weight of ethyl acetate and 45 parts by weight of carbodiimide-modified MDI, heating to 80-90 ℃, reacting for 4 hours, cooling to 60 ℃, adding polycaprolactone triol Capa TM 32018 parts by weight, heating to 80-90 ℃, reacting for 3 hours, detecting that the hydroxyl value is 0mgKOH/g, finishing the reaction, and finally cooling to room temperature to prepare an ethyl acetate solution which has a solid content of 62%, an NCO content of 10% and a rotational viscosity of 1400mPa & s at 25 ℃, namely the curing agent.
(4) The main agent and the curing agent are mixed according to the proportion
And mixing the main agent and the curing agent according to the weight ratio of 10:1 to obtain the adhesive for the H-grade insulating paper composite material.
Performance detection
The adhesives for grade C insulating paper composites prepared in examples 1, 2 and 3 of the present invention and the adhesives for grade H insulating paper composites prepared in comparative example 1 were subjected to the following parallel comparative property tests under the same conditions:
according to the proportion of the main agent and the curing agent in the adhesives prepared in the above examples 1, 2, 3 and 1 of the invention, the main agent and the curing agent in each adhesive are respectively mixed uniformly according to the proportion, ethyl acetate is added to dilute the mixture to the working solution concentration of 35 wt%, a No. 5 gluing rod is used for gluing two sides of a PET sheet (or a PA sheet) with the thickness of 50 mu respectively, after gluing, the PET sheet (or the PA sheet) is dried in an oven at the temperature of 60 ℃ for about 2-3 minutes, the solvent is dried, Nomex insulating paper is attached to two sides of the PET sheet (or the PA sheet), and a 2kg rubber roller is used for pressing, so that the NMN composite film (or NHN composite film) corresponding to the above examples and comparative examples is obtained.
(1) And (3) detecting initial adhesion: the NMN composite films (or NHN composite films) corresponding to the above examples and comparative examples were respectively left at room temperature for about 10min, and then T-type peel strength was examined.
(2) And (3) detecting the peel strength after curing: after the NMN composite film (or NHN composite film) corresponding to the above examples and comparative examples was respectively placed in an oven at 60 ℃ and cured for 72 hours, the interlayer T-type peel strength of the NMN composite film (or the NHN composite film) was examined.
(3) And (3) high temperature resistance detection: the NMN composite film (or NHN composite film) corresponding to the above examples and comparative examples was baked in a high temperature oven at 220 ℃ and 240 ℃ for 10 minutes, respectively, and whether or not there were any undesirable phenomena such as delamination and blistering in the NMN composite film (or the NHN composite film) was observed.
The detection results of the above performance detection are shown in table 1 below:
TABLE 1
Figure BDA0003432711270000111
As can be seen from table 1 above: compared with the comparative example 1, the examples 1, 2 and 3 have better initial adhesion and high temperature resistance, can meet the bonding and using requirements of the C-grade insulating paper composite material, and show that the adhesive has excellent bonding performance and high temperature resistance, can meet the bonding and using requirements of the C-grade insulating paper composite material, and can be used for the composition of flexible insulating paper composite materials NMN (Nomex paper/PET/Nomex paper) and NHN (Nomex paper/PA/Nomex paper) structures.
In conclusion, the embodiment of the invention has excellent bonding performance and high temperature resistance, can meet the bonding and using requirements of the C-grade insulating paper composite material, has excellent initial adhesion and final adhesion strength between the Nomex paper/PET film and the Nomex paper/PA film, and can be used for the composition of flexible insulating paper composite material NMN (Nomex paper/PET/Nomex paper) and NHN (Nomex paper/PA/Nomex paper) structures.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art that is already known to a person skilled in the art.

Claims (6)

1. The adhesive for the C-grade insulating paper composite material is characterized by comprising a main agent and a curing agent; the weight ratio of the main agent to the curing agent is 10: 2;
the main agent is an ethyl acetate solution containing high molecular weight polyester polyol and bisphenol A type epoxy resin, the rotational viscosity of the main agent is 600-1000 mPa & s at 25 ℃, and the solid content is 68-70%;
the curing agent is an ethyl acetate solution containing polysilazane resin modified isocyanate prepolymer, the rotational viscosity of the curing agent is 600-1200 mPa & s at 25 ℃, the solid content is 58-62%, and the-NCO content is 8-10%;
the main agent is mainly prepared from the following raw materials in parts by weight: 50-58 parts of high molecular weight polyester polyol, 16-22 parts of bisphenol A epoxy resin and 30-32 parts of ethyl acetate; the curing agent is mainly prepared from the following raw materials in parts by weight: 70-78 parts of isocyanate prepolymer solution, 1-3 parts of polysilazane resin and 23-27 parts of ethyl acetate;
the high molecular weight polyester polyol is mainly prepared from the following raw materials in parts by weight: 8-25 parts of isophthalic acid, 8-25 parts of terephthalic acid, 12-24 parts of adipic acid, 12-24 parts of diethylene glycol, 20-34 parts of 1, 6-hexanediol, 0.002-0.006 part of catalyst and 0.01-0.03 part of antioxidant.
2. The adhesive for the class-C insulating paper composite material according to claim 1, wherein the high molecular weight polyester polyol in the main agent has a relative molecular mass of 8000 to 10000, an acid value of less than 2mgKOH/g, a hydroxyl value of 10 to 15mgKOH/g, and a glass transition temperature of-10 to 5 ℃.
3. The adhesive for the grade C insulation paper composite according to claim 2, wherein the isocyanate prepolymer solution employs an aromatic isocyanate curing agent.
4. The adhesive for the grade-C insulating paper composite material according to claim 1 or 2, wherein the bisphenol-A epoxy resin having an epoxy value of 0.2 to 0.52 is used as the bisphenol-A epoxy resin.
5. A method for preparing an adhesive for C-grade insulating paper composite material, which is used for preparing the adhesive for C-grade insulating paper composite material of any one of the claims 1 to 4, and is characterized by comprising the following steps: preparing a main agent and a curing agent;
the preparation of the main agent comprises the following steps: adding high molecular weight polyester polyol, bisphenol A epoxy resin and ethyl acetate into a reaction kettle, heating to 80-90 ℃, stirring for 3-4 hours, uniformly mixing, and cooling to room temperature to prepare an ethyl acetate solution with solid content of 68-70% and rotary viscosity of 600-1000 mPa & s at 25 ℃, namely a main agent;
the preparation of the curing agent comprises the following steps: adding the isocyanate prepolymer solution, polysilazane resin and ethyl acetate into another reaction kettle, heating to 70-80 ℃, reacting for 3-4 hours, and cooling to room temperature to prepare an ethyl acetate solution which has a solid content of 58-62%, an NCO content of 8-10% and a rotational viscosity of 600-1200 mPa & s at 25 ℃ as a curing agent;
mixing the main agent and the curing agent according to a weight ratio of 10:2 to obtain the adhesive for the C-grade insulating paper composite material as claimed in any one of claims 1 to 4.
6. The method for preparing the adhesive for the grade C insulating paper composite according to claim 5, wherein the method for preparing the high molecular weight polyester polyol comprises:
weighing the following raw materials in parts by weight: 8-25 parts of isophthalic acid, 8-25 parts of terephthalic acid, 12-24 parts of adipic acid, 12-24 parts of diethylene glycol, 20-34 parts of 1, 6-hexanediol, 0.002-0.006 part of catalyst and 0.01-0.03 part of antioxidant;
esterification reaction: adding diethylene glycol, adipic acid, isophthalic acid, terephthalic acid, 1, 6-hexanediol, a catalyst and an antioxidant into a polyester synthesis kettle, heating to 120 ℃, preserving heat for 1h, after the solid raw materials are completely dissolved, gradually heating to 210-230 ℃ at the heating rate of 10 ℃/30min, controlling the water outlet speed, controlling the temperature of a fractionating column to be not higher than 110 ℃, and reacting for 6-10 h to complete the esterification reaction; the water yield accounts for 10-15% of the total weight of the raw materials, and the acid value of the esterification product is less than or equal to 15 mgKOH/g;
and (3) polycondensation reaction: after the esterification reaction is finished, vacuumizing the polyester synthesis kettle for 30 minutes according to-0.02 MPa, -0.04MPa, -0.06MPa and-0.08 MPa, controlling the kettle temperature of the polyester synthesis kettle to be 245-255 ℃, and then carrying out long vacuumizing operation, wherein the vacuum degree reaches-0.1 MPa, the long vacuumizing time is 3-4 hours, the distilled alcohol of the polyester synthesis kettle accounts for 4-8% of the total weight of the raw materials after long vacuumizing, the hydroxyl value obtained after discharging is 10-15 mgKOH/g, the acid value is less than or equal to 2mgKOH/g, the glass transition temperature is-10-5 ℃, and the final product with the relative molecular mass of 8000-10000 is the high molecular weight polyester polyol.
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CN104559903A (en) * 2015-02-09 2015-04-29 北京高盟新材料股份有限公司 Binder for compounding cold-molded aluminum and preparation method of binder
CN105112010A (en) * 2015-09-15 2015-12-02 中国科学院化学研究所 Room-temperature curing adhesive based on silazane and modified silazane polymer and preparation method thereof
CN112430448A (en) * 2020-11-23 2021-03-02 南通高盟新材料有限公司 Adhesive for H-grade insulating paper composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012003648A1 (en) * 2010-07-05 2012-01-12 广东多正化工科技有限公司 Method of producing solvent-free two-component polyurethane adhesive having low content of free diphenylmethane diisocyanate
CN104559903A (en) * 2015-02-09 2015-04-29 北京高盟新材料股份有限公司 Binder for compounding cold-molded aluminum and preparation method of binder
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