CN112029338A - Preparation method of environment-friendly universal adhesion promoter - Google Patents

Preparation method of environment-friendly universal adhesion promoter Download PDF

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CN112029338A
CN112029338A CN202010771063.2A CN202010771063A CN112029338A CN 112029338 A CN112029338 A CN 112029338A CN 202010771063 A CN202010771063 A CN 202010771063A CN 112029338 A CN112029338 A CN 112029338A
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匡正
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Wuxi Shengyi Synthetic Material Co ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract

The invention discloses a preparation method of an environment-friendly universal adhesion promoter, which comprises the following steps: mixing diethylaminoethyl methacrylate, methyl methacrylate and benzophenone for reaction to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate); taking DMF as a solvent, and mixing poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 1- (bromoacetyl) pyrene for reaction to prepare a hyperbranched copolymer; dissolving the hyperbranched polymer in a solvent, dropwise adding gamma-aminopropyltriethoxysilane, and stirring for reaction to obtain a component A; mixing trimesic acid, succinic acid and isobutanol; adding bisphenol A diglycidyl ether and triphenylphosphine for reaction to obtain carboxyl-terminated hyperbranched polyester; and mixing the carboxyl-terminated hyperbranched polyester with the component A to prepare the environment-friendly universal adhesion promoter. The environment-friendly universal adhesion promoter prepared by the invention can obviously improve the adhesion between the coating and the base material.

Description

Preparation method of environment-friendly universal adhesion promoter
The technical field is as follows:
the invention relates to the field of chemical additives, in particular to a preparation method of an environment-friendly universal adhesion promoter.
Background art:
good adhesion between the hardened coating and the substrate is the basis for obtaining the desired properties of the optical film. The size of the adhesive force is related to the surface state of the base material, the surface substance composition and the compactness of the material, and is also related to the shrinkage stress, the surface tension, the crystallinity of a film forming material in the coating, the volume size of a polar functional group and other factors. For many years, efforts have been made not only to improve the tensile strength of the coating film itself, but also to find ways to continuously improve the adhesion of the coating layer, so as to prolong the adhesion time of the coating layer, thereby achieving long-term protection of the coating layer on the substrate and maintaining the properties thereof. To improve the adhesion of the coating, the basic mode of the coating adhesion must be understood and how to strengthen the existence of these forms, so as to better design the coating formulation and to find an ideal way to solve the long-term adhesion of the coating. In general, the mode of action of the coating on the substrate surface can be divided into 3 forms: physical adsorption, chemical bonding, electrostatic theory, the 3 modes of distinction exist in the form of steric hindrance and electrostatic adsorption, respectively, in the strict sense.
The adhesion promoter is one of the most commonly used methods in the coating industry for improving the coating performance of materials and enhancing the adhesion firmness of a coating film on a substrate, and has the characteristics of convenient use, remarkable effect and the like. The adhesion promoters commonly used at present are classified into silanes, titanates, zirconates, zircoaluminates, metallorganics, phenolic resins, etc. according to the molecular type. However, any adhesion promoter has obvious selectivity on a matrix and a paint film, and has different effects, which brings inconvenience to industrial practical application.
The invention content is as follows:
the invention aims to solve the technical problem of providing a preparation method of an environment-friendly universal adhesion promoter aiming at the defects of the prior art, the adhesion promoter prepared by the preparation method has good stability, and the bonding performance of a polymer and a base material can be effectively improved.
In order to better solve the technical problems, the invention adopts the following technical scheme:
a preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1) adding diethylaminoethyl methacrylate, methyl methacrylate and benzophenone into a reactor, carrying out irradiation reaction for 1-2h under air, adding excessive hexane into reaction liquid after the reaction is finished, precipitating, filtering, and carrying out vacuum drying on the precipitate to obtain poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) taking DMF as a solvent, mixing poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 1- (bromoacetyl) pyrene for reaction for 20-30h, adding excessive hexane into the reaction liquid after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving the hyperbranched polymer in a solvent, then dropwise adding gamma-aminopropyltriethoxysilane while stirring, stirring for reaction after the dropwise adding is finished, and cooling after the reaction is finished to obtain a component A;
(4) adding trimesic acid and succinic acid into isobutanol, stirring and mixing, and heating to 105-115 ℃; then sequentially adding bisphenol A diglycidyl ether and triphenylphosphine into the reaction system, stirring and reacting for 20-25h, adding excessive diethyl ether into the reaction system after the reaction is finished, precipitating, filtering, and vacuum-drying the prepared precipitate to obtain carboxyl-terminated hyperbranched polyester;
(5) adding the prepared carboxyl-terminated hyperbranched polyester into the component A, stirring and mixing uniformly, and adding a solvent to adjust a reaction system to a proper viscosity, thereby preparing the environment-friendly general adhesion promoter.
As a preferable technical scheme, in the step (1), the mol ratio of the diethylaminoethyl methacrylate to the methyl methacrylate is 10: (4-7).
As a preferable technical scheme, the wavelength of the light adopted during the irradiation is 300-350 nm.
As a preferable technical scheme, in the step (2), the mass ratio of the poly (diethylaminoethyl methacrylate-co-methyl methacrylate) to the 1- (bromoacetyl) pyrene is 4: (1-2).
As a preferable technical scheme, in the step (2), the temperature of the reaction is 40-50 ℃.
As a preferable technical solution, in the step (3), the solvent is acetone.
As a preferable technical scheme, in the step (3), the mass ratio of the hyperbranched polymer to the gamma-aminopropyltriethoxysilane is 10 (1-5).
As a preferable technical scheme, in the step (3), the reaction temperature is 60-70 ℃, and the reaction time is 1-3 h.
In a preferable technical scheme, in the step (4), the mass ratio of the trimesic acid, the succinic acid, the bisphenol A diglycidyl ether and the triphenylphosphine is (10-11): 2: (19-19.2): (0.3-0.4).
As a preferred technical solution, the mass ratio of the carboxyl-terminated hyperbranched polyester to the hyperbranched copolymer is 1: (1-3).
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the invention provides a preparation method of an environment-friendly universal adhesion promoter, which comprises the steps of firstly mixing diethylaminoethyl methacrylate, methyl methacrylate and benzophenone to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate); then 1- (bromoacetyl) pyrene is adopted to modify poly (diethylaminoethyl methacrylate-co-methyl methacrylate) to prepare a hyperbranched copolymer; the molecular chain of the hyperbranched copolymer has a plurality of active groups, such as free tertiary amine groups and acetyl groups, which can generate cross-linking reaction with the components of the coating polymer, thereby improving the adhesive force between the coating and the substrate; the invention mixes and reacts trimesic acid, succinic acid and isobutanol, and adds bisphenol A diglycidyl ether and triphenylphosphine to react to obtain carboxyl-terminated hyperbranched polyester; the tail end of the polymer has a large number of terminal carboxyl groups, the carboxyl groups can effectively improve the binding force of the polymer and a base material, and isobutanol is used as a reaction solvent, so that the polymer is non-toxic and environment-friendly, and the reaction condition is mild; and the crosslinking density of the polymer can be improved by adding the crosslinking agent into the polymer, so that the bonding force between the coating and the substrate is improved. And mixing the carboxyl-terminated hyperbranched polyester with the component A to prepare the environment-friendly universal adhesion promoter.
The environment-friendly universal adhesion promoter prepared by the invention has good wetting property on coating polymers and substrates: the binding force of the coating polymer and various substrates can be obviously improved; the adhesive force is good; the storage stability is good.
The specific implementation mode is as follows:
the present invention is further illustrated by the following examples, which are provided for the purpose of illustration only and are not intended to be limiting.
Example 1
A preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1)10mol of diethylaminoethyl methacrylate, 4mol of methyl methacrylate and 1ml of benzophenone are added into a reactor and irradiated by light with the wavelength of 300nm for 1h under the air, after the reaction is finished, excessive hexane is added into the reaction liquid for precipitation, the reaction liquid is filtered, and the precipitate is dried in vacuum to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) mixing 8g of poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 2g of 1- (bromoacetyl) pyrene by taking 100ml of DMF as a solvent, reacting at 40 ℃ for 20h, adding excessive hexane into a reaction solution after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving 10g of the hyperbranched polymer in 50ml of acetone, dropwise adding 1g of gamma-aminopropyltriethoxysilane while stirring, stirring at 60 ℃ for reaction for 1h after dropwise adding is finished, and cooling after the reaction is finished to obtain a component A;
(4) adding 10g of trimesic acid and 2g of succinic acid into 50ml of isobutanol, stirring and mixing, and heating to 105 ℃; then, adding 19g of bisphenol A diglycidyl ether and 0.3g of triphenylphosphine into the reaction system in sequence, stirring for reaction for 20 hours, adding excessive diethyl ether into the reaction system after the reaction is finished for precipitation, filtering, and drying the prepared precipitate in vacuum to obtain carboxyl-terminated hyperbranched polyester;
(5) and adding 3.5g of the prepared carboxyl-terminated hyperbranched polyester into the component A, stirring and mixing uniformly, and adding a solvent to adjust the reaction system to a proper viscosity, thereby preparing the environment-friendly universal adhesion promoter.
Example 2
A preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1)10mol of diethylaminoethyl methacrylate, 7mol of methyl methacrylate and 1ml of benzophenone are added into a reactor and irradiated by light with the wavelength of 350nm for 2 hours in the air, after the reaction is finished, excessive hexane is added into the reaction liquid for precipitation, the reaction liquid is filtered, and the precipitate is dried in vacuum to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) mixing 8g of poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 4g of 1- (bromoacetyl) pyrene by taking 100ml of DMF as a solvent, reacting at 50 ℃ for 30h, adding excessive hexane into a reaction solution after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving 10g of the hyperbranched polymer in 50ml of acetone, dropwise adding 5g of gamma-aminopropyltriethoxysilane while stirring, stirring at 70 ℃ for reaction for 3 hours after dropwise adding is finished, and cooling after the reaction is finished to obtain a component A;
(4) adding 11g of trimesic acid and 2g of succinic acid into 50ml of isobutanol, stirring and mixing, and heating to 115 ℃; then, adding 19.2g of bisphenol A diglycidyl ether and 0.4g of triphenylphosphine into the reaction system in sequence, stirring for reaction for 25 hours, adding excessive diethyl ether into the reaction system after the reaction is finished for precipitation, filtering, and drying the prepared precipitate in vacuum to obtain carboxyl-terminated hyperbranched polyester;
(5) and adding 10g of the prepared carboxyl-terminated hyperbranched polyester into the component A, uniformly stirring and mixing, and adding a solvent to adjust the reaction system to a proper viscosity, thereby preparing the environment-friendly universal adhesion promoter.
Example 3
A preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1)10mol of diethylaminoethyl methacrylate, 4.5mol of methyl methacrylate and 1ml of benzophenone are added into a reactor and irradiated by light with the wavelength of 310nm for 1.5h under the air, after the reaction is finished, excessive hexane is added into the reaction liquid for precipitation, the reaction liquid is filtered, and the precipitate is dried in vacuum to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) mixing 8g of poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 2.2g of 1- (bromoacetyl) pyrene by taking 100ml of DMF as a solvent, reacting at 45 ℃ for 22h, adding excessive hexane into a reaction solution after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving 10g of the hyperbranched polymer in 50ml of acetone, dropwise adding 2g of gamma-aminopropyltriethoxysilane while stirring, stirring at 60 ℃ for reaction for 2 hours after dropwise adding is finished, and cooling after the reaction is finished to obtain a component A;
(4) adding 10.2g of trimesic acid and 2g of succinic acid into 50ml of isobutanol, stirring and mixing, and heating to 110 ℃; then, adding 19.05g of bisphenol A diglycidyl ether and 0.35g of triphenylphosphine into the reaction system in sequence, stirring for reaction for 21 hours, adding excessive diethyl ether into the reaction system after the reaction is finished for precipitation, filtering, and drying the prepared precipitate in vacuum to obtain carboxyl-terminated hyperbranched polyester;
(5) and adding 4g of the prepared carboxyl-terminated hyperbranched polyester into the component A, uniformly stirring and mixing, and adding a solvent to adjust the reaction system to a proper viscosity, thereby preparing the environment-friendly universal adhesion promoter.
Example 4
A preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1)10mol of diethylaminoethyl methacrylate, 5mol of methyl methacrylate and 1ml of benzophenone are added into a reactor and irradiated by light with the wavelength of 320nm for 1h under the air, after the reaction is finished, excessive hexane is added into the reaction liquid for precipitation, the reaction liquid is filtered, and the precipitate is dried in vacuum to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) mixing 8g of poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 3g of 1- (bromoacetyl) pyrene by taking 100ml of DMF as a solvent, reacting at 40 ℃ for 24 hours, adding excessive hexane into a reaction solution after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving 10g of the hyperbranched polymer in 50ml of acetone, dropwise adding 3g of gamma-aminopropyltriethoxysilane while stirring, stirring at 65 ℃ for reaction for 2 hours after dropwise adding is finished, and cooling after the reaction is finished to obtain a component A;
(4) 10.4g of trimesic acid and 2g of succinic acid are added to 50ml of isobutanol, stirred and mixed, and heated to 105 ℃; then, adding 19.1g of bisphenol A diglycidyl ether and 0.32g of triphenylphosphine into the reaction system in sequence, stirring for reaction for 22 hours, adding excessive diethyl ether into the reaction system after the reaction is finished for precipitation, filtering, and drying the prepared precipitate in vacuum to obtain carboxyl-terminated hyperbranched polyester;
(5) and adding 5g of the prepared carboxyl-terminated hyperbranched polyester into the component A, uniformly stirring and mixing, and adding a solvent to adjust the reaction system to a proper viscosity, thereby preparing the environment-friendly universal adhesion promoter.
Example 5
A preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1)10mol of diethylaminoethyl methacrylate, 5mol of methyl methacrylate and 1ml of benzophenone are added into a reactor and irradiated by light with the wavelength of 330nm for 1.5h under the air, after the reaction is finished, excessive hexane is added into the reaction liquid for precipitation, the reaction liquid is filtered, and the precipitate is dried in vacuum to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) mixing 8g of poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 3g of 1- (bromoacetyl) pyrene by taking 100ml of DMF as a solvent, reacting at 50 ℃ for 26h, adding excessive hexane into a reaction solution after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving 10g of the hyperbranched polymer in 50ml of acetone, dropwise adding 3g of gamma-aminopropyltriethoxysilane while stirring, stirring at 65 ℃ for reaction for 2 hours after dropwise adding is finished, and cooling after the reaction is finished to obtain a component A;
(4) 10.12g of trimesic acid and 2g of succinic acid are added to 50ml of isobutanol, stirred and mixed, and heated to 110 ℃; then, adding 19.15g of bisphenol A diglycidyl ether and 0.36g of triphenylphosphine into the reaction system in sequence, stirring for reaction for 24 hours, adding excessive diethyl ether into the reaction system after the reaction is finished for precipitation, filtering, and drying the prepared precipitate in vacuum to obtain carboxyl-terminated hyperbranched polyester;
(5) and adding 6g of the prepared carboxyl-terminated hyperbranched polyester into the component A, uniformly stirring and mixing, and adding a solvent to adjust the reaction system to a proper viscosity, thereby preparing the environment-friendly universal adhesion promoter.
Example 6
A preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1)10mol of diethylaminoethyl methacrylate, 6.5mol of methyl methacrylate and 1ml of benzophenone are added into a reactor and irradiated by light with the wavelength of 350nm for 2 hours under the air, after the reaction is finished, excessive hexane is added into the reaction liquid for precipitation, the reaction liquid is filtered, and the precipitate is dried in vacuum to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) mixing 8g of poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 3.5g of 1- (bromoacetyl) pyrene by taking 100ml of DMF as a solvent, reacting at 50 ℃ for 28h, adding excessive hexane into a reaction solution after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving 10g of the hyperbranched polymer in 50ml of acetone, dropwise adding 4.5g of gamma-aminopropyltriethoxysilane while stirring, stirring at 70 ℃ for reaction for 2.5h after dropwise adding is finished, and cooling after the reaction is finished to obtain a component A;
(4) adding 10.55g of trimesic acid and 2g of succinic acid into 50ml of isobutanol, stirring and mixing, and heating to 110 ℃; then, adding 19.18g of bisphenol A diglycidyl ether and 0.38g of triphenylphosphine into the reaction system in sequence, stirring for reaction for 24 hours, adding excessive diethyl ether into the reaction system after the reaction is finished for precipitation, filtering, and drying the prepared precipitate in vacuum to obtain carboxyl-terminated hyperbranched polyester;
(5) adding 8g of the prepared carboxyl-terminated hyperbranched polyester into the component A, stirring and mixing uniformly, and adding a solvent to adjust the reaction system to a proper viscosity to prepare the environment-friendly universal adhesion promoter.
Comparative example 1
A preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1) adding 10.55g of trimesic acid and 2g of succinic acid into 50ml of isobutanol, stirring and mixing, and heating to 110 ℃; then, adding 19.18g of bisphenol A diglycidyl ether and 0.38g of triphenylphosphine into the reaction system in sequence, stirring for reaction for 24 hours, adding excessive diethyl ether into the reaction system after the reaction is finished for precipitation, filtering, and drying the prepared precipitate in vacuum to obtain carboxyl-terminated hyperbranched polyester; namely the environment-friendly universal adhesion promoter.
Comparative example 2
A preparation method of an environment-friendly universal adhesion promoter comprises the following steps:
(1)10mol of diethylaminoethyl methacrylate, 6.5mol of methyl methacrylate and 1ml of benzophenone are added into a reactor and irradiated by light with the wavelength of 350nm for 2 hours under the air, after the reaction is finished, excessive hexane is added into the reaction liquid for precipitation, the reaction liquid is filtered, and the precipitate is dried in vacuum to prepare poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) mixing 8g of poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 3.5g of 1- (bromoacetyl) pyrene by taking 100ml of DMF as a solvent, reacting at 50 ℃ for 28h, adding excessive hexane into a reaction solution after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving 10g of the hyperbranched polymer in 50ml of acetone, dropwise adding 4.5g of gamma-aminopropyltriethoxysilane while stirring, and reacting for 2.5 hours at 70 ℃ while stirring after dropwise adding is finished to prepare the environment-friendly universal adhesion promoter.
Application examples
The bisphenol A liquid epoxy primer sold in the market is used as a substrate, and the bisphenol A liquid epoxy primer specifically comprises the following components: 41.5g of bisphenol A liquid epoxy resin, 1.0g of wetting dispersant, 0.8g of defoamer, 0.2g of flatting agent, 30.0g of barium sulfate, 13.0g of talcum powder, 5.0g of iron oxide red, 8.5g of benzyl alcohol and 29.5g of polyamide curing agent; then 1.5g of the adhesion promoters prepared in examples 1-6 and comparative examples 1 and 2 are respectively added to prepare different coatings; respectively and uniformly coating the prepared coatings on the surface of a polycarbonate plate, drying at room temperature, curing for 2 hours in an oven at 50 ℃ to prepare a coating, and testing the performance of the coating; the test method and test results are as follows, wherein the control group is a primer without an adhesion promoter:
1. adhesion test
According to ASTM D3359: 2009, measurement by cross-cut method.
2. Abrasion resistance test
0000 according to QB 2506-#And (5) uniformly wiping the steel wool under a 500g weight, and calculating the wiping frequency when the scratch appears.
3. Resistance to boiling
And (3) curing the coating template, putting the cured coating template in boiling water at 100 ℃ for boiling for a certain time, and testing the adhesive force and the wear resistance.
The test results are shown in table 1:
TABLE 1
Figure BDA0002616638290000101
From the test results, the carboxyl-terminated polyester and the amino silane coupling agent modified hyperbranched polymer prepared by the method can improve the binding performance of the coating and the substrate to a certain extent; the adhesion of the coating is greatly improved after the two are compounded.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is to be understood that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.

Claims (10)

1. The preparation method of the environment-friendly universal adhesion promoter is characterized by comprising the following steps:
(1) adding diethylaminoethyl methacrylate, methyl methacrylate and benzophenone into a reactor, carrying out irradiation reaction for 1-2h under air, adding excessive hexane into reaction liquid after the reaction is finished, precipitating, filtering, and carrying out vacuum drying on the precipitate to obtain poly (diethylaminoethyl methacrylate-co-methyl methacrylate);
(2) taking DMF as a solvent, mixing poly (diethylaminoethyl methacrylate-co-methyl methacrylate) and 1- (bromoacetyl) pyrene for reaction for 20-30h, adding excessive hexane into the reaction liquid after the reaction is finished for precipitation, filtering, and drying the filtered precipitate in vacuum to obtain a hyperbranched copolymer;
(3) dissolving the hyperbranched polymer in a solvent, then dropwise adding gamma-aminopropyltriethoxysilane while stirring, stirring for reaction after the dropwise adding is finished, and cooling after the reaction is finished to obtain a component A;
(4) adding trimesic acid and succinic acid into isobutanol, stirring and mixing, and heating to 105-115 ℃; then sequentially adding bisphenol A diglycidyl ether and triphenylphosphine into the reaction system, stirring and reacting for 20-25h, adding excessive diethyl ether into the reaction system after the reaction is finished, precipitating, filtering, and vacuum-drying the prepared precipitate to obtain carboxyl-terminated hyperbranched polyester;
(5) adding the prepared carboxyl-terminated hyperbranched polyester into the component A, stirring and mixing uniformly, and adding a solvent to adjust a reaction system to a proper viscosity, thereby preparing the environment-friendly general adhesion promoter.
2. The method for preparing the environmental-friendly general adhesion promoter as claimed in claim 1, wherein in the step (1), the molar ratio of the diethylaminoethyl methacrylate to the methyl methacrylate is 10: (4-7).
3. The method as claimed in claim 1, wherein the wavelength of the light used for the irradiation is 300-350 nm.
4. The method for preparing the environmental-friendly general adhesion promoter as claimed in claim 1, wherein in the step (2), the mass ratio of the poly (diethylaminoethyl methacrylate-co-methyl methacrylate) to the 1- (bromoacetyl) pyrene is 4: (1-2).
5. The method for preparing the environmental-friendly general adhesion promoter as claimed in claim 1, wherein the reaction temperature in the step (2) is 40-50 ℃.
6. The method for preparing the environmental-friendly general adhesion promoter as claimed in claim 1, wherein in the step (3), the solvent is acetone.
7. The method for preparing the environmental-friendly general adhesion promoter as claimed in claim 1, wherein in the step (3), the mass ratio of the hyperbranched polymer to the gamma-aminopropyltriethoxysilane is 10 (1-5).
8. The method for preparing the environmental-friendly general adhesion promoter as claimed in claim 1, wherein in the step (3), the reaction temperature is 60-70 ℃ and the reaction time is 1-3 h.
9. The method for preparing the environmental-friendly general adhesion promoter as claimed in claim 1, wherein in the step (4), the mass ratio of the trimesic acid, the succinic acid, the bisphenol A diglycidyl ether and the triphenylphosphine is (10-11): 2: (19-19.2): (0.3-0.4).
10. The method for preparing the environment-friendly general adhesion promoter as claimed in claim 1, wherein the mass ratio of the carboxyl-terminated hyperbranched polyester to the hyperbranched copolymer is 1: (1-3).
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CN113024705A (en) * 2021-02-04 2021-06-25 东莞市德聚胶接技术有限公司 Adhesion promoter for polyurethane adhesive and polyurethane adhesive
CN113024705B (en) * 2021-02-04 2021-11-23 东莞市德聚胶接技术有限公司 Adhesion promoter for polyurethane adhesive and polyurethane adhesive

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