CN110330871A - The application method that epoxy modified polyester resin is synthesized in pre-coated metal coil coating priming paint - Google Patents
The application method that epoxy modified polyester resin is synthesized in pre-coated metal coil coating priming paint Download PDFInfo
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- CN110330871A CN110330871A CN201910681725.4A CN201910681725A CN110330871A CN 110330871 A CN110330871 A CN 110330871A CN 201910681725 A CN201910681725 A CN 201910681725A CN 110330871 A CN110330871 A CN 110330871A
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- polyester resin
- modified polyester
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- epoxy modified
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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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
- 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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
Abstract
The application method that epoxy modified polyester resin is synthesized in pre-coated metal coil coating priming paint, first synthesizing epoxy modified polyester resin, is then made finished product paint for epoxy modified polyester resin.The method of the present invention is epoxy-modified by carrying out in advance to polyester resin, then pre-coated metal coil coating priming paint is prepared using epoxy modified polyester resin as base-material, graft reaction occurs for epoxy resin and polyester resin, obtain epoxy modified polyester resin, such epoxy modified polyester resin than the priming paint that blending method is worked it out performance such as in adhesive force, flexibility, resistance to boiling water, wet-heat resisting etc. is eager to excel very much, in the case where guaranteeing hardness of paint film, significantly enhancing flexibility improves the curved performance of T, increase crosslink density enhancing corrosion resistance simultaneously, coating production process can be reduced using epoxy modified polyester resin, reduce addition variety of raw material, production control cost can also thus be reduced, stability between increase batch, reduce quality risk.
Description
Technical field
The present invention relates to pre-coated metal coil coating priming paint synthesis technical fields, and in particular to a kind of epoxy-modified polyester tree
The application method that rouge is synthesized in pre-coated metal coil coating priming paint.
Background technique
Epoxy resin is widely used in pre-coated metal coil coating priming paint at present, and used by epoxy primer
E-06 or E-03 of the epoxy resin based on bisphenol A-type, epoxy coating formed film in have the dielectric breakdown that can not be corroded
Chemical bond and polarity group, thus have fabulous chemical resistance, while be crosslinked after epoxy resin paint film contain
Many hydroxyls and ehter bond thus have strong polar bond power with ground, have shielding action to corrosive medium, and can be passivated and be protected
Metal is protected, plays inhibition and electrochemical action, but its flexibility is poor.
Polyester priming paint is also to use a kind of more priming paint in coil coating, contains carboxyl, hydroxyl isoreactivity in strand
Group and ester bond, ehter bond isopolarity group, can be with the crosslinking of a variety of curing agent.There is a good binding force to substrate, it is adhesive force, flexible
Property it is preferable, machining property be better than epoxy primer, but its Corrosion Protection be not so good as epoxy resin.
In actual use, in order to meet the market demand and make up epoxy coating and Polyester resin lacquer
Performance shortcomings, usually using polyester resin spell plus epoxy resin method, be desirably to obtain the precoating of an excellent combination property
Metal coiled material base coat.Now widely used spelling plus Epoxy Resin Technology after being polyester resin, i.e., in Polyester resin lacquer
The epoxy resin of production phase split a part increases attachment to reach, improves hardness, increase the purpose of corrosion-resistant, asphalt mixtures modified by epoxy resin
Contain many hydroxyls, epoxy group and ehter bond in rouge structure, therefore has very strong adhesive force, while its chemical resistance to substrate
Excellent, such as alkali resistance, salt fog resistance etc., therefore, common pre-coated coil priming paint generally use polyester resin and epoxy resin blending
Using adding both ingredients respectively that is, in formulation for coating material, make the priming paint while there is the characteristic of polyester and epoxy, but the body
System's collocation performance is general, and in actual use, cold spelling adds epoxy resin to have problems, such as spells plus the rear curved performance of T declines,
Flexibility is deteriorated, and dosage fluctuates between batch, and storage layering is obvious etc..
Summary of the invention
The present invention is in view of the deficienciess of the prior art, provide a kind of epoxy modified polyester resin in pre-coated metal coiled material
The application method of base coat synthesis.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of application method that epoxy modified polyester resin is synthesized in pre-coated metal coil coating priming paint, first synthesizing epoxy change
Property polyester resin, is then made finished product paint for epoxy modified polyester resin, the specific process steps are as follows:
(1) synthesis of epoxy modified polyester resin, raw material include methyl propanediol, M-phthalic acid, adipic acid, adjacent benzene two
Formic anhydride, trimellitic acid glycosides, epoxy resin, Mono-n-butyltin, dimethylbenzene, BTX aromatics solvent S-100, mixed type binary acid
Diformazan ester solvent, wherein each ingredient uses mass content are as follows: methyl propanediol 18%-20%；M-phthalic acid 2%-3%；Oneself
Diacid 9%-10%；Phthalic anhydride 12%-13%；Trimellitic acid glycosides 2%-3%；Epoxy resin 7%-8%；Monobutyl oxygen
Change tin 0.05%-1%；Dimethylbenzene 1%-2%；BTX aromatics solvent S-10032%-35%；Mixed type dibasic acid dimethyl ester is molten
Agent 10%-15%, by methyl propanediol, M-phthalic acid, adipic acid, phthalic anhydride, trimellitic acid glycosides, epoxy resin,
Mono-n-butyltin is put into synthesis reactor, and slow heating is warming up to material thawing, opens stirring；Control temperature of charge 150 DEG C-
160 DEG C of heat preservations dehydration rises to 230 DEG C with every 10 minutes speed for rising 3 DEG C -5 DEG C, and to transparent, control evaporates a temperature in 98- for heat preservation
102℃；Be cooled to after transparent 180 DEG C hereinafter, into material plus dimethylbenzene carry out reflux dewatering, until acid value 10mgKOH/g hereinafter,
BTX aromatics solvent S-100 is added after cooling and mixed type dibasic acid dimethyl ester solvent is diluted, after being diluted to suitable viscosity
Discharging；
(2) epoxy modified polyester resin, the cyclohexanone, dispersing agent, zinc yellow, strontium chromium of step (1) preparation is first added in painting
Yellow, titanium dioxide and organobentonite are ground to fineness less than 20 microns, discharging, be added solvent, Lauxite, amino resins,
Adhesion promoter ADP, acidic catalyst BYK-450 and levelling agent stir evenly to get finished product paint, and above-mentioned each component uses
Mass fraction are as follows: 90-100 parts of epoxy modified polyester resin；5-7 parts of cyclohexanone；2-4 parts of dispersing agent；16-20 parts of zinc yellow；
12-15 parts of strontium chromate；25-30 parts of titanium dioxide；1-2 parts of organobentonite；13-18 parts of solvent；2-5 parts of Lauxite；Amino tree
8-12 parts of rouge；ADP2-4 parts of adhesion promoter；1-3 parts of acidic catalyst BYK-450；1-3 parts of levelling agent.
The epoxy resin being added in above-mentioned steps (1) is small-molecular-weight epoxy resin, such as E-20 type or E-12 type ring oxygen
Resin.
Dispersing agent used in above-mentioned steps (2) is Efka-4010 dispersing agent；Levelling agent is Efka-3777 dispersing agent.
The method of the present invention is epoxy-modified by carrying out in advance to polyester resin, then using epoxy modified polyester resin as base
Material prepares pre-coated metal coil coating priming paint, therefore by way of graft reaction, in resin synthesis process, epoxy resin with
Graft reaction occurs for polyester resin, obtains epoxy modified polyester resin, such epoxy modified polyester resin is done than blending method
The performance of priming paint out is such as in adhesive force, and flexibility, resistance to boiling water, wet-heat resisting etc. is eager to excel very much.Graft reaction is to set
In rouge synthesis process, because epoxy resin itself contains great amount of hydroxy group, therefore the portion in polyester formulation is replaced with epoxy resin
Divide polyalcohol.Meanwhile it is demonstrated experimentally that epoxy resin will select the E-20 or E-12 of small-molecular-weight, the E- of macromolecule cannot be used
03 epoxy resin, and epoxy resin additive amount has lacked in certain OK range and has not been obviously improved effect, more resin meetings
Gelatinization.
The method of the present invention is in the case where guaranteeing epoxy resin coating hardness of paint film, hence it is evident that promoting flexibility improves the curved performance of T,
Increase crosslink density enhancing corrosion resistance simultaneously, coating production process can be reduced using epoxy modified polyester resin, reduction adds
Add variety of raw material, thus production control cost can also be reduced, increases stability between batch, reduce quality risk.
Specific embodiment
The present invention passes through first synthesizing epoxy modified polyester resin, then spells again and afterwards plus the polyester resin of epoxy resin is pre-
Performance difference in matel coated coil coating priming paint is compared.
(1) synthesis of epoxy modified polyester resin
Main raw material(s) and equipment
Methyl propanediol, M-phthalic acid, adipic acid, phthalic anhydride, trimellitic acid glycosides, E-12 resin, monobutyl
Tin oxide, dimethylbenzene, S-100 (BTX aromatics solvent S-100), DBE (mixed type dibasic acid dimethyl ester).
KDM type adjustable temperature control electric jacket, accurate reinforcement electric mixer, refrigerator.
Raw material ratio (is shown in Table 1)
1 raw material ratio of table
Synthesis technology
(1) three-necked flask by first 7 investments with thermometer, blender and condensing unit, slow heating are warming up to object
Material melts, and opens stirring.
(2) control temperature of charge is dehydrated in 150~160 DEG C of heat preservations, was risen 3-5 DEG C with every 10 minutes and is risen to 230 DEG C, heat preservation is extremely
Transparent, control evaporates a temperature at 98-102 DEG C.
(3) it is cooled to 180 DEG C after transparent hereinafter, add reflux unit, adds dimethylbenzene to help reflux dewatering, until acid value
10mgKOH/g hereinafter, cooling after be added S-100 and DBE, discharge after being diluted to suitable viscosity.
The epoxy modified polyester resin quality index of above-mentioned synthesis
(1) viscosity: 15-25 seconds Jia Shi viscositys (25 DEG C)
(2) contain admittedly: 50%
(3) acid value: 5-8mgKOH/g.
(2) painting and performance test
2.1 main raw material(s)s and equipment
Epoxy modified polyester resin: Plain Wen Te；902 polyester resin: Plain Wen Te；Epoxy resin: three wood；5747 amino
Resin: Zhejiang Xinhua；5265 Lauxites: Zhejiang Xinhua；Titanium dioxide: Shandong east is good；Zinc yellow: domestic；Strontium chromate: domestic；
Organobentonite: domestic；Efka-4010；Efka company；ADP: De Qian company；BYK-450: Bick chemistry；Efka-3777:
Efka company；Cyclohexanone: domestic；Mixed solvent: Plain Wen Te
Electronic balance: upper Nereid section；The curved tester of T: domestic；Press: domestic；Precise salt mist tester: domestic；Paint
Film Apparatus for Impacting at low-temp: Zhejiang Ford；Cupping testing machine: domestic；Magnetic thickness tester Mikrotest IV: German Bi Kaote company；Bar:
The Shanghai Weng Kaier International Trade Corporation；Constant temperature oven: domestic；Shake uniform machine: domestic；ZN-P ultraviolet light weather resistance test chamber；
It is domestic.
2.2 painting
2 precoated coil coating base paint formulation of table
Sample 1, sample 2 are prepared respectively according to the formula of table 2, and raw material 1-9 is first added respectively, is ground to fineness micro- less than 20
Rice, discharging are added raw material 10-15, stir evenly to get finished product paint.
Making sheet
Selecting length and width in an experiment is 15cm × 8cm, is substrate with a thickness of the galvanized sheet of 0.3mm, with chromium treatment fluid surface
Processing, takes out after 150 degree of baking 1min, scratches above-mentioned prepared sample 1 with scraper respectively, and 2 priming paint of sample is placed at room temperature for
270 degree of constant temperature ovens are put into after several seconds rapidly, dries about 28-30 seconds (224 degree of plate temperature) and takes out rapidly with originally water quick cooling afterwards, be made
Template sample 1, sample 2 with priming paint.Then finishing coat is being coated in the same way on this template respectively, (this experiment uses
Warm spy's WTA series lime finishing coat), obtain required bottom surface composite paint film.
2.4 performance test
After template prepares, properties are tested, comprising: film thickness, pencil hardness draw lattice adhesive force, T curved, are cupping, resistance to
MEK wiping, impact, cupping, salt spray resistance, resistance to artificial accelerated aging performance etc..
3 results and discussion
3.1 result
Template is prepared with method in 2.3, examines mechanical performance, obtained results of property is as shown in table 3
3 sample 1 of table, 2 priming paint plate performance comparisons
4 sample 1 of table, 2 mating lime finishing coat plate performance comparisons
Sample 1,2 lime plates are subjected to salt mist experiment, salt spray resistance comparing result is as shown in table 4
5 sample 1 of table, 2 mating lime finishing coat plate salt fog performance comparisons
Sample 1,2 lime plates are subjected to artificially roughening, resistance to artificially roughening performance comparison result is such as
Shown in table 5
6 sample 1 of table, 2 mating lime finishing coat plate artificial ageing resistance experimental performance comparisons
In this trial, sample 1 is compared with sample sample 2, and sample 2 is better than comparative sample sample 1 in the curved performance of T, simultaneously
Better than comparison on the resistance to MEK number of priming paint, in salt-fog resistant test, 2 salt spray corrosion resistance of sample is hard in pencil better than comparison
Degree impacts, stroke lattice, in cupping and artificially roughening project, can reach standard, meet requirement.In addition exist
In the storage stability test of sample, the layering during storage of epoxy modified polyester resin paint and loose colour situation better than pair
Than item.
In conclusion epoxy modified polyester resin paint is equal in paint film flexibility, resisting salt fog corrosion and storage stability
It is spelled after being better than and adds epoxy resin coating.It and can be in the case where guaranteeing epoxy resin coating hardness of paint film, hence it is evident that promoting flexibility improves T
Curved performance, while increasing crosslink density enhancing corrosion resistance.
Coating production process can be reduced using epoxy modified polyester resin, reduce addition variety of raw material, thus can also be with
Production control cost is reduced, increases stability between batch, reduces quality risk.
Conclusion
Epoxy modified polyester resin as described herein is applied in pre-coated metal coil coating, coating excellent combination property,
The some performance shortcomings for adding epoxy resin coating are spelled after can improving in the case where guaranteeing that other performances such as hardness are constant, are had good
Hardness, flexibility, storage stability performance and salt spray corrosion resistance, while can reduce production control cost.
Claims (3)
1. the application method that a kind of epoxy modified polyester resin is synthesized in pre-coated metal coil coating priming paint, it is characterized in that first synthesizing
Then finished product paint is made in epoxy modified polyester resin by epoxy modified polyester resin, the specific process steps are as follows:
(1) synthesis of epoxy modified polyester resin, raw material include methyl propanediol, M-phthalic acid, adipic acid, phthalic acid
Acid anhydride, trimellitic acid glycosides, epoxy resin, Mono-n-butyltin, dimethylbenzene, BTX aromatics solvent S-100, mixed type binary acid diformazan
Ester solvent, wherein each ingredient uses mass content are as follows: methyl propanediol 18%-20%；M-phthalic acid 2%-3%；Adipic acid
9%-10%；Phthalic anhydride 12%-13%；Trimellitic acid glycosides 2%-3%；Epoxy resin 7%-8%；Mono-n-butyltin
0.05%-1%；Dimethylbenzene 1%-2%；BTX aromatics solvent S-10032%-35%；Mixed type dibasic acid dimethyl ester solvent
10%-15%, by methyl propanediol, M-phthalic acid, adipic acid, phthalic anhydride, trimellitic acid glycosides, epoxy resin, list
Butyl tin oxide is put into synthesis reactor, and slow heating is warming up to material thawing, opens stirring；Control temperature of charge 150 DEG C-
160 DEG C of heat preservations dehydration rises to 230 DEG C with every 10 minutes speed for rising 3 DEG C -5 DEG C, and to transparent, control evaporates a temperature in 98- for heat preservation
102℃；Be cooled to after transparent 180 DEG C hereinafter, into material plus dimethylbenzene carry out reflux dewatering, until acid value 10mgKOH/g hereinafter,
BTX aromatics solvent S-100 is added after cooling and mixed type dibasic acid dimethyl ester solvent is diluted, after being diluted to suitable viscosity
Discharging；
(2) painting, first be added step (1) preparation epoxy modified polyester resin, cyclohexanone, dispersing agent, zinc yellow, strontium chromate,
Titanium dioxide and organobentonite are ground to fineness less than 20 microns, discharging, and solvent, Lauxite, amino resins, attached is added
Adhesion promoter ADP, acidic catalyst BYK-450 and levelling agent are stirred evenly and are used to get finished product paint, above-mentioned each component
Mass fraction are as follows: 90-100 parts of epoxy modified polyester resin；5-7 parts of cyclohexanone；2-4 parts of dispersing agent；16-20 parts of zinc yellow；Strontium
12-15 parts of chrome yellow；25-30 parts of titanium dioxide；1-2 parts of organobentonite；13-18 parts of solvent；2-5 parts of Lauxite；Amino resins
8-12 parts；ADP2-4 parts of adhesion promoter；1-3 parts of acidic catalyst BYK-450；1-3 parts of levelling agent.
2. epoxy modified polyester resin according to claim 1 is in the application side that pre-coated metal coil coating priming paint synthesizes
Method, it is characterized in that the epoxy resin being added in step (1) is small-molecular-weight epoxy resin, such as E-20 type or E-12 type asphalt mixtures modified by epoxy resin
Rouge.
3. epoxy modified polyester resin according to claim 1 is in the application side that pre-coated metal coil coating priming paint synthesizes
Method, it is characterized in that dispersing agent used in step (2) is Efka-4010 dispersing agent；Levelling agent is Efka-3777 levelling agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910681725.4A CN110330871A (en) | 2019-07-26 | 2019-07-26 | The application method that epoxy modified polyester resin is synthesized in pre-coated metal coil coating priming paint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910681725.4A CN110330871A (en) | 2019-07-26 | 2019-07-26 | The application method that epoxy modified polyester resin is synthesized in pre-coated metal coil coating priming paint |
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| CN110330871A true CN110330871A (en) | 2019-10-15 |
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| CN201910681725.4A Pending CN110330871A (en) | 2019-07-26 | 2019-07-26 | The application method that epoxy modified polyester resin is synthesized in pre-coated metal coil coating priming paint |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778529A (en) * | 2020-12-30 | 2021-05-11 | 万博新材料科技（南通）有限公司 | Preparation method of polyester modified epoxy resin for coil primer |
| CN114621451A (en) * | 2022-03-31 | 2022-06-14 | 兰州金睿合新材料科技有限责任公司 | Pure polyester resin modified epoxy resin and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102993422A (en) * | 2012-11-30 | 2013-03-27 | 无锡市虎皇漆业有限公司 | Epoxy modified saturated polyester resin for undercoat of coil coating and undercoat of coil coating |
-
2019
- 2019-07-26 CN CN201910681725.4A patent/CN110330871A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102993422A (en) * | 2012-11-30 | 2013-03-27 | 无锡市虎皇漆业有限公司 | Epoxy modified saturated polyester resin for undercoat of coil coating and undercoat of coil coating |
Non-Patent Citations (1)
| Title |
|---|
| 王禹阶主编: "《玻璃钢与复合材料的生产及应用 有机、无机玻璃钢及其相关材料的综述》", 30 November 2005 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778529A (en) * | 2020-12-30 | 2021-05-11 | 万博新材料科技（南通）有限公司 | Preparation method of polyester modified epoxy resin for coil primer |
| CN114621451A (en) * | 2022-03-31 | 2022-06-14 | 兰州金睿合新材料科技有限责任公司 | Pure polyester resin modified epoxy resin and preparation method and application thereof |
| CN114621451B (en) * | 2022-03-31 | 2023-05-23 | 兰州金睿合新材料科技有限责任公司 | Pure polyester resin modified epoxy resin and preparation method and application thereof |
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Application publication date: 20191015 |