CN116199846A - Hydroxy resin, preparation method thereof, fluorocarbon coating containing hydroxy resin and preparation method thereof - Google Patents

Hydroxy resin, preparation method thereof, fluorocarbon coating containing hydroxy resin and preparation method thereof Download PDF

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CN116199846A
CN116199846A CN202310011039.2A CN202310011039A CN116199846A CN 116199846 A CN116199846 A CN 116199846A CN 202310011039 A CN202310011039 A CN 202310011039A CN 116199846 A CN116199846 A CN 116199846A
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resin
hydroxyl
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agent
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车家福
熊邦虎
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Chongqing Dingdian Chemical Co ltd
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
    • C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass

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Abstract

The invention discloses a hydroxyl resin, a preparation method and a fluorocarbon coating containing the hydroxyl resin and a preparation method thereof, wherein the hydroxyl resin can be directly applied to the surface of a high-plasticizer pultrusion glass fiber reinforced polyurethane profile after the dehydrated polyester diol with the hydroxyl equivalent of 500-1000g/mol and 4,4' -dicyclohexylmethane diisocyanate are respectively dissolved in dehydrated butyl acetate solvent and added with a dibutyl tin laurate catalyst for reaction.

Description

Hydroxy resin, preparation method thereof, fluorocarbon coating containing hydroxy resin and preparation method thereof
Technical Field
The invention relates to the technical field of coatings, in particular to a hydroxyl resin, a preparation method thereof and a fluorocarbon coating containing the hydroxyl resin and a preparation method thereof.
Background
In the production of polyurethane composite profiles, the application of plasticizers and release agents is generally necessary in order to improve the smoothness and cleanliness of the profile surface, and excessive amounts occur, which brings about adjustments for further coating treatments. The patent CN113897085a only describes the effect of coating a waterborne polyurethane silica sol coating on the flat surface of glass fiber polyurethane gridding cloth, which is not applicable to the complex surface of door and window profiles, but also has huge differences in processing raw materials of glass fiber polyurethane gridding cloth and glass fiber reinforced polyurethane profiles, the latter relates to plasticizers and release agents, the surface energy is lower, and the glass fiber polyurethane gridding cloth and the glass fiber reinforced polyurethane profiles are more difficult to directly adhere.
Because the residue of the release agent and the high Wen Qianyi of the plasticizer lead to difficult infiltration and adhesion of the surface of the glass fiber reinforced polyurethane section bar, in the existing production and construction, a polishing process is inevitably introduced to improve the adhesive force of the coating on the polyurethane glass fiber section bar so as to achieve good service life, and the surface of the concave surface of the complex structure is difficult to polish well, so that the surface is also coated dead angle, and the coating is easy to fall off.
The conventional FEVE fluorocarbon resin is synthesized by copolymerizing trifluorochloroethylene or tetrafluoroethylene serving as a fluorine-containing monomer with alkyl vinyl ether or alkyl vinyl ester, introducing a vinyl compound containing hydroxyl and carboxyl and having the functions of increasing crosslinking, improving wettability and dispersibility, improving adhesive force and the like, and can form a super weather-resistant coating by matching with isocyanate or amino resin, even if the FEVE resin has good wettability, the FEVE resin is not suitable for the surfaces of glass fiber reinforced polyurethane profiles after the release agent residue and the plasticizer are migrated under any condition, and the adhesive force of the surfaces of different batches of profiles is not guaranteed to reach the 0-level requirement.
Disclosure of Invention
In view of this, the present invention provides a hydroxy resin, a method for preparing the same, and a fluorocarbon coating containing the same, and a method for preparing the same.
The technical scheme is as follows:
one of the objects of the present invention is achieved by: a preparation method of hydroxyl resin is characterized in that: the dehydrated polyester diol with the hydroxyl equivalent weight of 500-1000g/mol and 4,4' -dicyclohexylmethane diisocyanate are respectively dissolved in dehydrated butyl acetate solvent, and dibutyl tin laurate catalyst is added for reaction to obtain the hydroxyl resin.
Preferably:
dissolving the polyester diol in a dehydrated butyl acetate solvent, adding the dibutyl tin laurate catalyst, stirring until the mixture is uniformly dissolved to obtain a mixed solution I, and stirring the mixed solution I at a speed of 600-800 r/min at 60-70 ℃;
dissolving 4,4' -dicyclohexylmethane diisocyanate in dehydrated butyl acetate to obtain a mixed solution II, dropwise adding the mixed solution II into the mixed solution I within 15-30 minutes, and preserving heat for 2-4 hours after completion to obtain the hydroxyl resin with the solid content of 30-35% and the titration hydroxyl value of 15-30 mgKOH/g.
When the mixed solution I is prepared, the polyester diol is 100-120 parts by weight, and the butyl acetate solvent is 200 parts by weight;
when the mixed solution II is prepared, 13.72 parts of 4,4' -dicyclohexylmethane diisocyanate and 50 parts of butyl acetate solvent are calculated according to parts by weight.
The molecular weight of the polyester diol is 2000, and the metering ratio R value of the polyester diol and 4,4' -dicyclohexylmethane diisocyanate is 0.98.
The dibutyl tin laurate is 0.02-0.05 part by mass.
The second object of the invention is realized in that: a hydroxyl resin is characterized in that: the preparation method is adopted for preparation.
The third object of the present invention is achieved by: the high-temperature curing FEVE fluorocarbon coating for the glass fiber reinforced polyurethane profile is characterized by comprising the following components:
30-40 parts of FEVE fluorocarbon resin; 5-10 parts of the hydroxy resin according to claim 6; 5-8 parts of methyl amino resin; 1-5 parts of an auxiliary agent; 7-15 parts of mixed solvent; 30-40 parts of color paste ground by acrylic resin; 2-5 parts of extinction powder.
Preferably:
the auxiliary agent comprises a leveling agent, a defoaming agent and an anti-settling agent.
The mixed solvent is one or more of isobutyl acetate, propylene glycol methyl ether acetate and diethylene glycol butyl ether.
The fourth object of the present invention is achieved by: the preparation method of the glass fiber reinforced polyurethane profile high-temperature curing FEVE fluorocarbon coating is characterized by comprising the following steps:
s1, preparing color paste ground by acrylic resin;
s2, adding the extinction powder, the flatting agent, the antifoaming agent and the anti-settling agent into the mixed solvent, dispersing uniformly at a high speed, and then adding the color paste, and dispersing uniformly to obtain a mixed component;
and S3, adding FEVE fluorocarbon resin, the hydroxyl resin and the methylated amino resin into the mixed components, dispersing at a high speed until the mixture is uniform, and filtering to obtain a finished product.
Compared with the prior art, the invention has the beneficial effects that:
the invention develops the high-adhesion hydroxyl resin which can be directly applied to the surface of the glass fiber reinforced polyurethane profile formed by high-plasticizer pultrusion, and based on the hydroxyl resin, the FEVE fluorocarbon coating with excellent weather resistance and good wet heat resistance and corrosion resistance is prepared.
Drawings
FIG. 1 is a 313 nm photoaging comparison (2000 hours) of comparative example 3 and experimental example 1;
fig. 2 is a comparison of the adhesion after boiling in water of comparative example 3 and experimental example 1.
Detailed Description
Example 1, a method for preparing a hydroxy resin, comprises the following steps:
(1) according to the parts by weight, 100 parts of polyester diol with the molecular weight of 2000 are dissolved in 200 parts of butyl acetate solvent dehydrated by zeolite, 0.02 part of dibutyl tin laurate catalyst is added, stirring is carried out until the mixture is dissolved uniformly to obtain a mixed solution I, the mixed solution I is kept at a constant temperature in a bath pot provided with a condensing device at 70 ℃ and is stirred at a speed of 600 revolutions per minute; wherein the polyester dihydric alcohol is dehydrated in advance at 60 ℃ and under 0.08MPa until the hydroxyl equivalent weight is 500-1000g/mol;
(2) according to the mass portion, 13.72 portions of 4,4' -dicyclohexylmethane diisocyanate (NCO: 30% content) is taken and dissolved in 50 portions of butyl acetate dehydrated by zeolite to obtain a mixed solution II;
(3) and (3) dropwise adding the mixed solution II into the mixed solution I within 15-30 minutes, and preserving heat for 2 hours after completion, thereby obtaining the hydroxyl resin with the solid content of 30-35% and the titration hydroxyl value of 15-30 mgKOH/g.
The polyester diol is peak PE3556, the metering ratio R of the polyester diol and 4,4' -dicyclohexylmethane diisocyanate is 0.98, and the molar ratio of isocyanate to hydroxyl is the isocyanate index R.
Example 2: a preparation method of hydroxyl resin comprises the following specific steps:
(1) according to the parts by weight, 120 parts of polyester diol with the molecular weight of 2000 are dissolved in 200 parts of butyl acetate solvent dehydrated by zeolite, 0.05 part of dibutyl tin laurate catalyst is added, stirring is carried out until the mixture is dissolved uniformly to obtain a mixed solution I, the mixed solution I is kept at a constant temperature in a bath pot with a condensing device at the temperature of 60 ℃ and is stirred at the speed of 800 revolutions per minute; wherein the polyester dihydric alcohol is dehydrated in advance at 100 ℃ and under 0.04MPa until the hydroxyl equivalent weight is 500-1000g/mol;
(2) according to the mass portion, 13.72 portions of 4,4' -dicyclohexylmethane diisocyanate (NCO: 30% content) is taken and dissolved in 50 portions of butyl acetate dehydrated by zeolite to obtain a mixed solution II;
(3) and (3) dropwise adding the mixed solution II into the mixed solution I within 15-30 minutes, and preserving heat for 4 hours after completion, thereby obtaining the hydroxyl resin with the solid content of 30-35% and the titration hydroxyl value of 15-30 mgKOH/g.
The polyester diol is peak PE3556, and the metering ratio R of the polyester diol to the 4,4' -dicyclohexylmethane diisocyanate is 0.98.
Example 3: a preparation method of hydroxyl resin comprises the following specific steps:
(1) according to the parts by weight, 110 parts of polyester diol with the molecular weight of 2000 are dissolved in 200 parts of butyl acetate solvent dehydrated by zeolite, then 0.03 part of dibutyl tin laurate catalyst is added, the mixture is stirred until the mixture is uniformly dissolved to obtain a mixed solution I, the mixed solution I is kept at a constant temperature in a bath pot with a condensing device at the temperature of 65 ℃ and is stirred at the speed of 700 revolutions per minute; wherein the polyester dihydric alcohol is dehydrated in advance at 80 ℃ and under 0.06MPa until the hydroxyl equivalent weight is 500-1000g/mol;
(2) according to the mass portion, 13.72 portions of 4,4' -dicyclohexylmethane diisocyanate (NCO: 30% content) is taken and dissolved in 50 portions of butyl acetate dehydrated by zeolite to obtain a mixed solution II;
(3) and (3) dropwise adding the mixed solution II into the mixed solution I within 15-30 minutes, and preserving heat for 3 hours after completion, thereby obtaining the hydroxyl resin with the solid content of 30-35% and the titration hydroxyl value of 15-30 mgKOH/g.
The polyester diol is peak PE3556, and the metering ratio R of the polyester diol to the 4,4' -dicyclohexylmethane diisocyanate is 0.98.
Example 4, a preparation method of a glass fiber reinforced polyurethane profile high temperature cured FEVE fluorocarbon coating, comprising the following steps:
s1, preparing color paste ground by acrylic resin, and grinding the fineness of the color paste to be less than 15 mu m; the quantities of acrylic resin, pigment and solvent are added according to the design formula requirement of the product when preparing color paste, the types of the solvents are consistent with those of the mixed solvents, and the quality of the final product is not affected by the addition of the prepared color paste;
s2, taking 15 parts of isobutyl acetate, adding 4 parts of extinction powder, 1 part of flatting agent, 2 parts of defoaming agent and 2 parts of anti-settling agent, dispersing uniformly at a high speed, then adding 30 parts of color paste, and dispersing uniformly again to obtain a mixed component;
and step S3, adding 40 parts of FEVE fluorocarbon resin, 5 parts of the hydroxyl resin prepared in the embodiment 1 and 7 parts of the high-imino methylated amino resin into the mixed components, dispersing at a high speed until the mixture is uniform, and filtering to obtain a finished product.
Example 5, a preparation method of a glass fiber reinforced polyurethane profile high temperature cured FEVE fluorocarbon coating, comprising the following steps:
s1, preparing color paste ground by acrylic resin, and grinding the fineness of the color paste to be less than 15 mu m; the quantities of acrylic resin, pigment and solvent are added according to the design formula requirement of the product when preparing color paste, the types of the solvents are consistent with those of the mixed solvents, and the quality of the final product is not affected by the addition of the prepared color paste;
s2, taking 7 parts of a mixed solvent consisting of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1), adding 2 parts of extinction powder, 0.3 part of flatting agent, 0.4 part of defoamer and 0.3 part of anti-settling agent, dispersing uniformly at a high speed, and then adding 37 parts of color paste, and dispersing uniformly to obtain a mixed component;
and S4, finally adding 37 parts of FEVE fluorocarbon resin, 8 parts of the hydroxyl resin prepared in the example 3 and 8 parts of the high-imino methylated amino resin into the mixed components, dispersing at a high speed until the mixture is uniform, and filtering to obtain a finished product.
Example 6, a preparation method of a glass fiber reinforced polyurethane profile high temperature cured FEVE fluorocarbon coating, comprising the following steps:
s1, preparing color paste ground by acrylic resin, and grinding the fineness of the color paste to be less than 15 mu m; the quantities of acrylic resin, pigment and solvent are added according to the design formula requirement of the product when preparing color paste, the types of the solvents are consistent with those of the mixed solvents, and the quality of the final product is not affected by the addition of the prepared color paste;
s2, taking 12 parts of a mixed solvent consisting of isobutyl acetate, propylene glycol methyl ether acetate and diethylene glycol butyl ether (2:2:3), adding 5 parts of extinction powder, 1 part of flatting agent, 0.5 part of defoamer and 1 part of anti-settling agent, dispersing uniformly at a high speed, then adding 40 parts of color paste, and dispersing uniformly again to obtain a mixed component;
and step S3, adding 30 parts of FEVE fluorocarbon resin, 10 parts of the hydroxyl resin prepared in the embodiment 2 and 5 parts of the high-imino methylated amino resin into the mixed components, dispersing at a high speed until the mixture is uniform, and filtering to obtain a finished product.
In examples 4 to 6, FEVE fluorocarbon resin used was Japanese DajinGK 570 (65% solids, hydroxyl value 60 mgKOH/g); the methylated amino resin with high imino groups is a Zhanxing 325 amino resin; dispersing agents can be added when preparing color paste, and the dispersing agents can be super dispersing agents with good compatibility with FEVE fluorocarbon resin, such as Tech-5835 polyester dispersing agents of Shanghai Tegn auxiliary agents; the leveling agent is a Tech-178 fluorine modified polyacrylate leveling agent which is suitable for FEVE baking varnish application and does not influence recoating property, such as a sea Target auxiliary agent; the defoamer is fluorine modified organic silicon suitable for FEVE baking varnish spraying application, such as Tech-367N fluorine modified polysiloxane defoamer of the Shanghai Tegn auxiliary agent; the anti-settling agent is fumed silica suitable for outdoor weather resistance requirements, such as winning R972 hydrophobically modified fumed silica; the acrylic resin is B44 thermoplastic acrylic resin of Rogowski, and the average molecular weight is 20-30 ten thousand; pigments can be added according to the formula requirement of the product, and include calcined metal oxide pigments such as copper chrome black, titanium chrome yellow, titanium pigment, iron oxide red and the like; the matting agent is OK520 which is easy to disperse at high speed and has uniform gloss.
The present invention will be further described with reference to experimental examples, comparative examples and drawings.
Comparative example 1: the components of the product are as follows: according to the weight portions, 37 portions of Japanese DajinGK 570 tetrafluoro FEVE fluorocarbon resin, 8 portions of commercial common courtesy FS2050 hydroxy polyacrylic resin, 8 portions of Zhanxing 325 amino resin, 0.4 portion of Shanghai Tech-367N defoamer, 0.3 portion of Shanghai Tech-178 flatting agent and 0.3 portion of Yingzhang R972 fumed silica anti-settling agent; 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent, 37 parts of coffee color paste ground by Rongchus B44 acrylic resin and 2 parts of Desoxak-520 extinction powder;
the preparation method comprises the following steps:
(1) 42 parts of mixed solvent of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) are added with 14 parts of Roman Hasi B44 acrylic resin, and stirred and dissolved to clear and transparent liquid;
(2) adding 2.6 parts of Shanghai Tech-5835 dispersing agent, 32 parts of titanium dioxide, 1.2 parts of copper chrome black, 3.2 parts of titanium chrome yellow and 5 parts of iron oxide red into the resin mixed solution in the step (1), dispersing at a high speed, grinding for 2-4 hours by a sand mill, filtering to obtain color paste for later use after the fineness is lower than 15 um;
(3) 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent are weighed, 0.4 part of Shanghai Tech-367N defoamer is added, 0.3 part of Shanghai Tech-178 flatting agent, 0.3 part of Yingchuang R972 fumed silica anti-settling agent and 2 parts of De-solid Kai OK-520 flatting powder are stirred and dispersed uniformly, 37 parts of color paste is added, and high-speed dispersion is continued for 1-2 hours until uniform;
(4) 37 parts of Japanese gold GK570 tetrafluoro type FEVE resin, 8 parts of commercially available common Qingjin GK570 tetrafluoro type FEVE resin, 8 parts of Zhanxing 325 amino resin and filtering after stirring uniformly are added into the mixed components.
Comparative example 2: the components of the product are as follows: 37 parts of Japanese DajinGK 570 tetrafluoro type FEVE resin, which is commercially available
Figure BDA0004038452770000081
670BA hydroxyl polyester resin 8 parts, zhanxing 325 amino resin 8 parts, shanghai Tech-367N defoamer 0.4 parts, shanghai Tech-178 flatting agent 0.3 parts, and Yingzhang R972 fumed silica anti-settling agent 0.3 parts; 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent, 37 parts of coffee color paste ground by Rongchus B44 acrylic resin, and deluxe OK-520 extinction2 parts of powder;
the preparation method comprises the following steps:
(1) 42 parts of mixed solvent of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) are added with 14 parts of Roman Hasi B44 acrylic resin, and stirred and dissolved to clear and transparent liquid;
(2) adding 2.6 parts of Shanghai Tech-5835 dispersing agent, 32 parts of titanium dioxide, 1.2 parts of copper chrome black, 3.2 parts of titanium chrome yellow and 5 parts of iron oxide red into the resin mixed solution, dispersing at a high speed, grinding for 2-4 hours by a sand mill, filtering to obtain color paste for standby after the fineness is lower than 15 um;
(3) 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent are weighed, 0.4 part of Shanghai Tech-367N defoamer is added, 0.3 part of Shanghai Tech-178 flatting agent, 0.3 part of Yingchuang R972 fumed silica anti-settling agent and 2 parts of De-solid Kai OK-520 flatting powder are stirred and dispersed uniformly, 37 parts of color paste is added, and high-speed dispersion is continued for 1-2 hours until uniform;
(4) 37 parts of Japanese big gold GK570 tetrafluoro type FEVE resin, which is commercially available and common, is added to the mixed components
Figure BDA0004038452770000091
670BA hydroxyl polyester 8 parts, zhanxing 325 amino resin 8 parts, and filtering after uniformly stirring to obtain a finished product.
Comparative example 3: the components of the product are as follows: calculated according to parts by weight, 37 parts of Japanese big gold GK570 tetrafluoro type FEVE resin, and common road-bloodless resin sold in market
Figure BDA0004038452770000092
8 parts of TPU 5715 thermoplastic polyurethane resin, 8 parts of Zhanxing 325 amino resin, 0.4 part of Shanghai Tech-367N defoamer, 0.3 part of Shanghai Tech-178 flatting agent and 0.3 part of Yingzhang R972 fumed silica anti-settling agent; 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent, 37 parts of coffee color paste ground by Rongchus B44 acrylic resin and 2 parts of Desoxak-520 extinction powder;
the preparation method comprises the following steps:
(1) 42 parts of a mixed solvent of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1), and 14 parts of Rongmen Hasi B44 acrylic resin are added, and stirred and dissolved to form clear and transparent liquid;
(2) adding 2.6 parts of Shanghai Tech-5835 dispersing agent, 32 parts of titanium dioxide, 1.2 parts of copper chrome black, 3.2 parts of titanium chrome yellow and 5 parts of iron oxide red into the resin mixed solution in the step (1), dispersing at a high speed, grinding for 2-4 hours by a sand mill, filtering to obtain color paste for later use after the fineness is lower than 15 um;
(3) 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent are weighed, 0.4 part of Shanghai Tech-367N defoamer is added, 0.3 part of Shanghai Tech-178 flatting agent, 0.3 part of Yingchuang R972 fumed silica anti-settling agent and 2 parts of De-solid Kai OK-520 flatting powder are stirred and dispersed uniformly, 37 parts of color paste is added, and high-speed dispersion is continued for 1-2 hours until uniform;
(4) 37 parts of Japanese gold GK570 tetrafluoro type FEVE resin and common road-bloodless resin sold in the market are added into the mixed components
Figure BDA0004038452770000093
TPU 5715, namely 8 parts of thermoplastic polyurethane resin, 8 parts of Zhanxing 325 amino resin, is uniformly stirred and then filtered to obtain a finished product.
Comparative example 4: the components of the product are as follows: the high-strength heat-resistant adhesive comprises, by weight, 45 parts of Japanese DajinGK 570 tetrafluoro FEVE resin, 8 parts of Zhanxing 325 amino resin, 0.4 part of Shanghai Tech-367N defoamer, 0.3 part of Shanghai Tech-178 flatting agent and 0.3 part of Yingzhang R972 fumed silica anti-settling agent; 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent, 37 parts of coffee color paste ground by Rongchus B44 acrylic resin and 2 parts of Desoxak-520 extinction powder.
The preparation method comprises the following steps:
(1) 42 parts of a mixed solvent of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1), and 14 parts of Rongmen Hasi B44 acrylic resin are added, and stirred and dissolved to form clear and transparent liquid;
(2) adding 2.6 parts of Shanghai Tech-5835 dispersing agent, 32 parts of titanium dioxide, 1.2 parts of copper chrome black, 3.2 parts of titanium chrome yellow and 5 parts of iron oxide red into the resin mixed solution in the step (1), dispersing at a high speed, grinding for 2-4 hours by a sand mill, and filtering to obtain color paste for later use after the fineness is lower than 15 um;
(3) 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent are weighed, 0.4 part of Shanghai Tech-367N defoamer is added, 0.3 part of Shanghai Tech-178 flatting agent, 0.3 part of Yingchuang R972 fumed silica anti-settling agent and 2 parts of De-solid Kai OK-520 flatting powder are stirred and dispersed uniformly, 37 parts of color paste is added, and high-speed dispersion is continued for 1-2 hours until uniform;
(4) 45 parts of Japanese gold GK570 tetrafluoro type FEVE resin and 8 parts of Zhanxing 325 amino resin are added into the mixed components, and the mixture is stirred uniformly and filtered to obtain a finished product.
Experimental example 1: the components of the product are as follows: 37 parts of Japanese DajinGK 570 tetrafluoro type FEVE resin, 8 parts of hydroxy resin prepared in any one of examples 1-3, 8 parts of Zhanxing 325 amino resin, 0.4 part of Shanghai Tech-367N defoamer, 0.3 part of Shanghai Tech-178 flatting agent and 0.3 part of Yingzhang R972 fumed silica anti-settling agent; 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent, 37 parts of Rongkola Hasi B44 acrylic resin ground coffee color paste and 2 parts of Desoxak-520 matting powder (the composition of the product is the same as that of example 5).
The preparation method comprises the following steps:
(1) 42 parts of a mixed solvent of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1), and 14 parts of Rongmen Hasi B44 acrylic resin are added, and stirred and dissolved to form clear and transparent liquid;
(2) adding 2.6 parts of Shanghai Tech-5835 dispersing agent, 32 parts of titanium dioxide, 1.2 parts of copper chrome black, 3.2 parts of titanium chrome yellow and 5 parts of iron oxide red into the resin mixed solution in the step (1), dispersing at a high speed, grinding for 2-4 hours by a sand mill, and filtering to obtain color paste for later use after the fineness is lower than 15 um;
(3) 7 parts of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) mixed solvent are weighed, 0.4 part of Shanghai Tech-367N defoamer is added, 0.3 part of Shanghai Tech-178 flatting agent, 0.3 part of Yingchuang R972 fumed silica anti-settling agent and 2 parts of De-solid Kai OK-520 flatting powder are stirred and dispersed uniformly, 37 parts of color paste is added, and high-speed dispersion is continued for 1-2 hours until uniform;
(4) 37 parts of Japanese gold GK570 tetrafluoro type FEVE resin, 8 parts of hydroxy resin prepared in example 3 and 8 parts of Zhanxing 325 amino resin are added into the mixed components, and the mixture is stirred uniformly and filtered to obtain a finished product.
And (3) adjusting the finished products of the comparative example and the experimental example to proper spraying viscosity by using a mixed solvent of propylene glycol methyl ether acetate and diethylene glycol butyl ether (6:1) according to the air spraying viscosity requirement, cutting the glass fiber reinforced polyurethane profile with the plasticizer dosage of 4-6% into a plurality of sections, spraying sample paint into each 3 sections under the condition of no polishing treatment, drying the sample paint for 10 minutes, baking the sample paint in a baking oven at 125-130 ℃ for 30 minutes, taking out and cooling, and performing a plurality of performance tests, wherein the test results are shown in a table 1.
TABLE 1 Performance test results
Figure BDA0004038452770000111
Figure BDA0004038452770000121
The results of the basic properties of the coating film of experimental example 1 are shown in table 2.
TABLE 2 basic Properties of coating film
Figure BDA0004038452770000122
The adhesion after boiling and the aging comparison result of 313 nm light for 2000 hours of experimental example 1 and comparative example 3 are shown in fig. 1 and 2, wherein the right side of the graph is the spray finished product of experimental example 1, and the left side of the graph is the spray finished product of comparative example 3.
From the results, the glass fiber reinforced polyurethane FEVE fluorocarbon coating prepared by the invention has good construction property, certain surface scratch resistance, excellent adhesive force, good corrosion resistance and no abnormality in 2000 hours of salt fog; the weather resistance is outstanding, the ultraviolet irradiation for 2000 hours can be achieved, the coating has no obvious luster and color difference change, and the weather resistance is far higher than that of the traditional acrylic polyurethane anticorrosive material; the glass fiber reinforced polyurethane material also has good resistance to common acid and alkali, and can provide anticorrosion protection for widely applied places, especially the application anticorrosion of areas with high humidity and heat and high ultraviolet irradiation.
Finally, it should be noted that the above description is only a preferred embodiment of the present invention, and that many similar changes can be made by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. A preparation method of hydroxyl resin is characterized in that: the dehydrated polyester diol with the hydroxyl equivalent weight of 500-1000g/mol and 4,4' -dicyclohexylmethane diisocyanate are respectively dissolved in dehydrated butyl acetate solvent, and dibutyl tin laurate catalyst is added for reaction to obtain the hydroxyl resin.
2. The method for producing a hydroxyl resin according to claim 1, wherein: dissolving the polyester diol in a dehydrated butyl acetate solvent, adding the dibutyl tin laurate catalyst, stirring until the mixture is uniformly dissolved to obtain a mixed solution I, and stirring the mixed solution I at a speed of 600-800 r/min at 60-70 ℃;
dissolving 4,4' -dicyclohexylmethane diisocyanate in dehydrated butyl acetate to obtain a mixed solution II, dropwise adding the mixed solution II into the mixed solution I within 15-30 minutes, and preserving heat for 2-4 hours after completion to obtain the hydroxyl resin with the solid content of 30-35% and the titration hydroxyl value of 15-30 mgKOH/g.
3. The method for producing a hydroxyl resin according to claim 2, wherein: when the mixed solution I is prepared, the polyester diol is 100-120 parts by weight, and the butyl acetate solvent is 200 parts by weight;
when the mixed solution II is prepared, 13.72 parts of 4,4' -dicyclohexylmethane diisocyanate and 50 parts of butyl acetate solvent are calculated according to parts by weight.
4. A method for producing a hydroxyl resin according to claim 1, 2 or 3, wherein: the molecular weight of the polyester diol is 2000, and the metering ratio R value of the polyester diol and the 4,4' -dicyclohexylmethane diisocyanate is 0.98.
5. The method for producing a hydroxyl resin according to claim 4, wherein: the dibutyl tin laurate is 0.02-0.05 part by mass.
6. A hydroxyl resin characterized in that: prepared by the preparation method of any one of claims 1 to 5.
7. The glass fiber reinforced polyurethane profile high-temperature curing FEVE fluorocarbon coating is characterized by comprising the following components:
30-40 parts of FEVE fluorocarbon resin; 5-10 parts of the hydroxy resin according to claim 6; 5-8 parts of methyl amino resin; 1-5 parts of an auxiliary agent; 7-15 parts of mixed solvent; 30-40 parts of color paste ground by acrylic resin; 2-5 parts of extinction powder.
8. The glass fiber reinforced polyurethane profile high temperature cured FEVE fluorocarbon coating of claim 7, wherein: the auxiliary agent comprises a leveling agent, a defoaming agent and an anti-settling agent.
9. The glass fiber reinforced polyurethane profile high temperature curing FEVE fluorocarbon coating as claimed in claim 7 or 8, wherein: the mixed solvent is one or more of isobutyl acetate, propylene glycol methyl ether acetate and diethylene glycol butyl ether.
10. A method for preparing the glass fiber reinforced polyurethane profile high temperature curing FEVE fluorocarbon coating according to claim 9, which is characterized by comprising the following steps:
s1, preparing color paste ground by acrylic resin;
s2, adding the extinction powder, the flatting agent, the antifoaming agent and the anti-settling agent into the mixed solvent, dispersing uniformly at a high speed, and then adding the color paste, and dispersing uniformly to obtain a mixed component;
and S3, adding FEVE fluorocarbon resin, the hydroxyl resin and the methylated amino resin into the mixed components, dispersing at a high speed until the mixture is uniform, and filtering to obtain a finished product.
CN202310011039.2A 2023-01-05 2023-01-05 Hydroxy resin, preparation method thereof, fluorocarbon coating containing hydroxy resin and preparation method thereof Pending CN116199846A (en)

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