CN106118388A - A kind of high solid content and low viscosity automotive OEM is coated with coating and preparation method thereof - Google Patents

A kind of high solid content and low viscosity automotive OEM is coated with coating and preparation method thereof Download PDF

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Publication number
CN106118388A
CN106118388A CN201610480835.0A CN201610480835A CN106118388A CN 106118388 A CN106118388 A CN 106118388A CN 201610480835 A CN201610480835 A CN 201610480835A CN 106118388 A CN106118388 A CN 106118388A
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resin
coating
acid
polyester resin
levelling agent
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CN106118388B (en
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刘成强
刘爱萍
徐海港
姚红蕾
刘金涛
杨金河
王爱文
徐名霞
刘昊
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Shandong Shifeng Group Co Ltd
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Shandong Shifeng Group Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • 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
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78—Preparation processes
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
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  • Paints Or Removers (AREA)

Abstract

The invention mainly relates to paint field, particularly relate to a kind of high solid content and low viscosity automotive OEM is coated with coating and preparation method thereof.Middle painting coating of the present invention, by percentage to the quality, its raw material consists of: by percentage to the quality, its raw material consists of: polyester resin 25 35%, resist sagging resin 5 12%, rutile titanium white lead 15 25%, hollow glass bead 0 2%, precipitated super-fine barium sulfate 12 18%, dispersant 1 3%, white carbon 0.1 0.3%, organosilicon levelling agent 0.1 0.3%, acrylate levelling agent 0.3 0.6%, surfactant 0.2 0.5%, anti-settling agent 0 2%, Ketohexamethylene 0 4%, ethylene glycol ether acetate 3 5%, white carbon black 0.05 0.2%, butylated amino resin 20 28%, part methyl-etherified amino resins 2 4%.Middle painting coating of the present invention, working viscosity is low, construction solid part is high, and outward appearance is good, economical, environmental protection.

Description

A kind of high solid content and low viscosity automotive OEM is coated with coating and preparation method thereof
Technical field
The invention mainly relates to paint field, particularly relate to a kind of high solid content and low viscosity automotive OEM is coated with coating and system thereof Preparation Method.
Background technology
2015, according to " ambient air quality " (GB3095-2012), 338 regions in the whole nation and above city (contained Ground, state, alliance location) natural law ratio up to standard is between 5.5%～100%, and average out to 72.7%, the natural law ratio that all exceeds standard is 27.3%, wherein slight pollution ratio is 18.7%, and intermediate pollution accounts for 5.2%, and serious pollution accounts for 2.7%, and severe contamination accounts for 0.7%, major pollutants are volatile organic matter, and it is the important carrier of haze, so improving quality of air environment gesture must OK.
The coating process of auto manufacturing belongs to the use process of volatile organic matter solvent, a large amount of miscellaneous coating Volatilize in coating process with organic solvent, cause air quality severe contamination, for implementing National Sustainable Development Strategies, protection Ecological environment, promotes that auto manufacturing's pollutant abatement technology promotes, it is necessary to carry out environment-friendly type coating energetically.
Along with the impact of new round haze weather, Green environmental protection, the novel industry of low-carbon energy-saving, it is to realize industry knot The only way that structure adjusts and Economic Development Mode changes, the mankind pursue the inevitable choice of healthy living especially, when such For under background, auto manufacturing bears major design and adjusts important task, need to formulate practicable energy-conserving and environment-protective embodiment.
Over more than 100 year, car paint has been achieved with four big updates, and so far, the Automobile Paints of China is still Traditional being coated with by two coating systems being coated with in anaphoretic priming and organic solvent type, finish paint the is supporting external eighties in 20th century Material, VOC emission amount is more than 120g/m2, in order to improve environment, both at home and abroad actively push forward develop environment-friendly type coating: water paint, height Solid part coating, powdery paints and PVC coating etc..
Owing to water paint there is also problems, as corollary equipment requires that high investment is big, cost of raw material amplification is many, dry Factors, powdery paints and the PVC coating such as dry speed is slow, and execution conditions are affected substantially by humiture, and outward appearance developability is not enough Range of application is narrower, and therefore exploitation high-solid lower-viscosity coating seems and is even more important.
Summary of the invention
For the problems referred to above, the present invention proposes one and can be used for being coated with in automotive OEM height light coating, has reached working viscosity Low, construction solid part is high, outward appearance is good, economical, the plurality of advantages of environmental protection.
Being coated with coating in a kind of high solid content and low viscosity automotive OEM of the present invention, by percentage to the quality, its raw material forms For: by percentage to the quality, its raw material consists of: polyester resin 25-35%, resist sagging resin 5-12%, rutile titanium white lead 15-25%, hollow glass bead 0-2%, precipitated super-fine barium sulfate 12-18%, dispersant 1-3%, white carbon 0.1-0.3%, Organosilicon levelling agent 0.1-0.3%, acrylate levelling agent 0.3-0.6%, surfactant 0.2-0.5%, anti-settling agent 0- 2%, Ketohexamethylene 0-4%, ethylene glycol ether acetate 3-5%, white carbon black 0.05-0.2%, butylated amino resin 20-28%, portion Divide methyl-etherified amino resins 2-4%.
Wherein, polyester resin is fundamental reaction resin, exists in uniform temperature with butyl ether and part methyl-etherified amino resins Cross-linking reaction；Resist sagging resin improves the resist sagging performance of paint；Titanium dioxide body pigment, it is provided that paint hides performance；Glass Cenosphere improves levelability and the intensity of paint；Precipitated super-fine barium sulfate plays filling effect in paint；White carbon is at paint In play anti-settling resist sagging performance；Dispersant is to aid in color stuffing wetting and dispersing to certain particle diameter, namely fineness of grind；Organosilicon Levelling agent and acrylate levelling agent improve and improve paint coating surface flatness；Anti-settling agent strengthens paint shelf characteric.In reality During border produces, paint line and painting environment gap are relatively big, the most different to the performance requirement of paint, data are limited to necessarily Scope, can carry out elastic adjustment to a certain specific indexes, and matrix resin dosage is excessive, and painting gloss is the brightest, surface smoothness The highest, it is unfavorable for the attachment of finish paint, affects finish paint supporting, otherwise resin is few, gloss is low, and surface smoothness is poor, affects finish paint Appearance.The consumption of resist sagging resin, is to consider paint line design difference, and paint spraying is complete, the length of levelling section and baking Stream pendant time roasting, dosage is the highest, affects cost, and dosage is low does not play sagging effect.Rutile titanium white lead dosage is too big, and cost is high, Paint coating surface gloss low, dosage is few, hide poor performance, pigment be added in suitable scope, according to performance requirement adjust, Raw material is controlled in certain limit in a word, be to meet different performance requirements and painting environment, taking into account again quality cost.
In the present invention, resist sagging resin selects trade mark button to wear this 91795 resin, and R706 selected by rutile titanium white lead, ultra-fine Blanc fixe selects 2500 mesh, and dispersant is BYK161, and organosilicon levelling agent selects BYK331 or enlightening high by 450, and white carbon selects Using Degussa R972, acrylate levelling agent selects the fluorine-containing levelling agent of BKY399 or afcona3670, surfactant trade mark moral Modest U99, butylated amino resin select button wear this 138 or BASF 018 resin, part methyl-etherified amino resins selects cyanogen special 717 resins.
Polyester resin of the present invention, in parts by weight, its raw material consists of: benzoic acid 0-1.5 part, isooctyl acid 0- 2.0 parts, adipic acid 20-28 part, THPA 0-5 part, phthalic anhydride 10-16 part, TMPD 0-5 part, new penta Glycol 25-35 part, tetramethylolmethane 4-7 part, hypophosphorous acid 0-0.3 part, antioxidant 1010 0-0.1 part, mixed dimethyl esters 0-15 Part, dimethylbenzene 0-2.0 part, propylene glycol methyl ether acetate 3-6 part, butyl acetate 2-5 part.
Wherein, benzoic acid and isooctyl acid primarily serve end-blocking effect, and consumption is too much, then form molecular weight polymers too much, Making the performance step-downs such as water-fast, impact, hardness, consumption is too low, then viscosity is bigger.Adipic acid is pliability monomer, and consumption is too much, tree Fat hardness is the lowest, and consumption is very few, then shock resistance is deteriorated.Phthalic anhydride consumption is too much, then product hardness is big, and impact is not Good, weather-proof bad；Consumption is too low, then gloss is the highest, and product hardness is the highest；THPA price is higher, but relatively phthalic acid Acid anhydride can reduce viscosity.The function of TMPD and neopentyl glycol is similar, but TMPD to have fall low viscous Effect, main framework, TMPD is expensive, has used many relatively costly, and neopentyl glycol provides the agent structure of polyester. Tetramethylolmethane contains four hydroxyls, and activity is higher, improves crosslink density, but is because the reason that activity is higher, has used many and then glued Spending big, with having lacked, the then degree of cross linking is inadequate.Hypophosphorous acid is catalyst, has added cost high, and reaction is excessively fierce, adds and has lacked reaction Time lengthens, and affects energy consumption, production efficiency.Antioxidant is with few, and color of resin is turned to be yellow, and affects outward appearance, has added relatively costly. Propylene glycol methyl ether acetate and butyl acetate are solvent.The present invention arranges in pairs or groups by raw material has carried out a large amount of screening, obtains one Plant the resin of high-solid lower-viscosity system, and this resin has pliability and hardness concurrently.
Present invention also offers the preparation method of coating in a kind of high solid content and low viscosity automotive OEM, it concretely comprises the following steps:
A, the preparation of polyester resin
(1) each raw material of polyester resin is weighed in proportion, standby；
(2), under inert gas environment, in reactor, neopentyl glycol, tetramethylolmethane, TMPD, different pungent is put into Acid, benzoic acid, adipic acid, THPA, phthalic anhydride, hypophosphorous acid, antioxidant 1010, stirring is warming up to 140 DEG C, and 2h is to slowly warm up to 180 DEG C, it is incubated 1h；1h is to slowly warm up to 200 DEG C, is incubated 1h；It is warming up to 210 DEG C, 210 DEG C of insulation reaction to acid number 17- 19mgKOH/g, cooling, add dimethylbenzene and divide water, point water is complete, is cooled to 130-140 DEG C, is sequentially added into propylene glycol monomethyl ether acetic acid Ester, butyl acetate, mixed dimethyl esters latting drown, filter and package, and obtains polyester resin, resin liquid outward appearance clear, solid part 80 ± 2%, viscosity (form pipe, 25 DEG C) 15-25S；
B, the preparation of semi-finished product mill base
(1) each raw material of coating in high solid content and low viscosity automotive OEM is weighed in proportion, standby；
(2) take the 1/2 of polyester resin quality to mix with dispersant, ethylene glycol ether acetate and Ketohexamethylene, stirring mixing Uniformly；
(3) rutile titanium dioxide, hollow glass bead, precipitated super-fine barium sulfate, white carbon black, the anti-settling agent above-mentioned mixing of addition are taken In solution, stir, be subsequently adding organosilicon levelling agent and acrylate levelling agent, be ground to sand mill after stirring Fineness is less than 10 microns；
(4) refer to that grinding test master grind color development effect reaches optimal, filters stand-by；
C, the preparation of resist sagging resin dispersion liquid
After remaining polyester resin, resist sagging resin and butylated amino resin are mixed being not less than 1400-1500 and turn/ Min high-speed stirred is less than 10 microns to fineness；
D, by qualified semi-finished product mill base and resist sagging resin dispersion liquid mix homogeneously, add leftover materials in formula, stir Mix uniformly, adjust viscosity, toning；
E, technical performance index detect；
F, strainer filtering with 300 mesh are packed and are i.e. obtained final products.
In the present invention, in the preparation process of polyester resin, using and first melt the synthetic method refluxed afterwards, the present invention is the most logical After crossing the polymer that melt phase polycondensation Step Condensation becomes the suitable size of molecular weight, then by retaining in dehydration by circumfluence method Suitable polymerization, so that the polymer of synthesis can keep again good shock resistance while having relatively low molecular weight. Pet reaction is the process of a Step Condensation, and the purpose progressively heated up mainly controls the structure of polyester molecule so that polyester Molecule is when little molecule, moreover it is possible to have a good impact, and current existing polyester resin, it is the most all that molecular weight is little When, impact bad, does not reaches the shock resistance of Automotive Primer Surfacer requirement, and the present invention was heated up polymerization by the described stage Mode, the resin of production just can meet the paint of painting in high solid low viscosity automobile while shock resistance does not reduces Requirement.
In the present invention, in the preparation process of semi-finished product mill base, reaching best surface effect during for paint spraying, fineness is more Little, coating surface effect exquisiteness and flatness are the best, otherwise poor, therefore, are ground to fineness less than 10 microns.In order to improve Process of lapping efficiency and effect, charging sequence has strict requirements.First, use some polyesters resin molten with dispersant and part Agent stirs after mixing, and then adds pigment and filler is ground.Because if dispersant is affine with color stuffing Property higher, if the most first making dispersant and polyester resin premix, affect production efficiency.
In the present invention, in the preparation process of semi-finished product mill base, rotating speed is that 1400-1500 turns/min, and rotating speed is low, resist sagging tree Fat dispersion effect is poor, can cause paint storage layered.
In the present invention, polyester resin production and coating material production have carried out a large amount of screening to raw material, to technological requirement essence skill Precisely, first of all for ensureing that molecular resin amount is little, solid part is high, and combination property is good, first passes through melt phase polycondensation Step Condensation, treats After molecular size range is suitable, then in dehydration, retain suitable polymerization by circumfluence method, so that the polymer of synthesis Good shock resistance can be kept again while having relatively low molecular weight.Mill base refers to grind color comparison, and levelling agent grinds the stage Add, be all to ensure that the technical advantage of the final construction effect of coating.The each raw material of the present invention is selected compounding reasonable, and the middle painting prepared is coated with Viscosity is low, solid content is high for material, save the engineering time, the ply adhesion of good leveling property and electrophoretic primer, finish paint is good, higher Glossiness, environmental-protecting performance are superior.
Detailed description of the invention
Embodiment 1
Being coated with coating in a kind of high solid content and low viscosity automotive OEM, by percentage to the quality, its raw material consists of: polyester resin 25%, resist sagging resin 12%, rutile titanium white lead 20%, precipitated super-fine barium sulfate 12%, dispersant 1%, white carbon 0.3%, organosilicon levelling agent 0.3%, acrylate levelling agent 0.6%, surfactant 0.4%, anti-settling agent 0.2%, hexamethylene Ketone 3%, ethylene glycol ether acetate 3%, white carbon black 0.2%, butylated amino resin 20%, part methyl-etherified amino resins 2%.
Described polyester resin, in parts by weight, its raw material consists of: isooctyl acid 2.0 parts, adipic acid 20 parts, tetrahydrochysene benzene Acid anhydride 5 parts, phthalic anhydride 16 parts, TMPD 1 part, neopentyl glycol 30 parts, tetramethylolmethane 7 parts, hypophosphorous acid 0.3 part, Antioxidant 1010 0.05 part, mixed dimethyl esters 15 parts, dimethylbenzene 2.0 parts, propylene glycol methyl ether acetate 3 parts, butyl acetate 2 Part.
Resist sagging resin selects trade mark button to wear this 91795 resin, and rutile titanium white lead selects R706, precipitated super-fine barium sulfate Selecting 2500 mesh, dispersant is BYK161, and organosilicon levelling agent selects BYK331 or enlightening high by 450, and Degussa selected by white carbon R972, acrylate levelling agent selection BKY399, the modest U99 of surfactant trade mark moral, butylated amino resin selects button to wear this 138, part methyl-etherified amino resins selects special 717 resins of cyanogen.
Its concrete preparation process is:
A, the preparation of polyester resin
(1) each raw material of polyester resin is weighed in proportion, standby；
(2), under inert gas environment, in reactor, neopentyl glycol, tetramethylolmethane, TMPD, different pungent is put into Acid, benzoic acid, adipic acid, THPA, phthalic anhydride, hypophosphorous acid, antioxidant 1010, stirring is warming up to 140 DEG C, and 2h is to slowly warm up to 180 DEG C, it is incubated 1h；1h is to slowly warm up to 200 DEG C, is incubated 1h；It is warming up to 210 DEG C, 210 DEG C of insulation reaction to acid number 17- 19mgKOH/g, cooling, add dimethylbenzene and divide water, point water is complete, is cooled to 130-140 DEG C, is sequentially added into propylene glycol monomethyl ether acetic acid Ester, butyl acetate, mixed dimethyl esters latting drown, filter and package, and obtains polyester resin, resin liquid outward appearance clear, solid part 80 ± 2%, viscosity (form pipe, 25 DEG C) 15-25S；
B, the preparation of semi-finished product mill base
(1) each raw material of coating in high solid content and low viscosity automotive OEM is weighed in proportion, standby；
(2) take the 1/2 of polyester resin quality to mix with dispersant, ethylene glycol ether acetate and Ketohexamethylene, stirring mixing Uniformly；
(3) rutile titanium dioxide, hollow glass bead, precipitated super-fine barium sulfate, white carbon black, the anti-settling agent above-mentioned mixing of addition are taken In solution, stir, be subsequently adding organosilicon levelling agent and acrylate levelling agent, be ground to sand mill after stirring Fineness is less than 10 microns；
(4) refer to that grinding test master grind color development effect reaches optimal, filters stand-by；
C, the preparation of resist sagging resin dispersion liquid
After remaining polyester resin, resist sagging resin and butylated amino resin are mixed being not less than 1400-1500 and turn/ Min high-speed stirred is less than 10 microns to fineness；
D, by qualified semi-finished product mill base and resist sagging resin dispersion liquid mix homogeneously, add leftover materials in formula, stir Mix uniformly, adjust viscosity, toning；
E, technical performance index detect；
F, strainer filtering with 300 mesh are packed and are i.e. obtained final products.
Embodiment 2
Being coated with coating in a kind of high solid content and low viscosity automotive OEM, by percentage to the quality, its raw material consists of: polyester resin 30%, resist sagging resin 10%, rutile titanium white lead 15%, hollow glass bead 1%, precipitated super-fine barium sulfate 12%, dispersion Agent 1%, white carbon 0.15%, organosilicon levelling agent 0.3%, acrylate levelling agent 0.3%, surfactant 0.2%, second two Alcohol ethyl ether acetate ester 5%, white carbon black 0.05%, butylated amino resin 23%, part methyl-etherified amino resins 2%.
Described polyester resin, in parts by weight, its raw material consists of: 1.5 parts of benzoic acid, isooctyl acid 1.5 parts, adipic acid 28 parts, phthalic anhydride 10 parts, TMPD 2 parts, neopentyl glycol 25 parts, tetramethylolmethane 4 parts, antioxidant 1010 0.1 Part, mixed dimethyl esters 5 parts, dimethylbenzene 1 part, propylene glycol methyl ether acetate 6 parts, butyl acetate 5 parts.
Resist sagging resin selects trade mark button to wear this 91795 resin, and rutile titanium white lead selects R706, precipitated super-fine barium sulfate Selecting 2500 mesh, dispersant is BYK161, and organosilicon levelling agent selects BYK331, and white carbon selects Degussa R972, acrylic acid Ester levelling agent selects BKY399, the modest U99 of surfactant trade mark moral, and butylated amino resin selects BASF 018 resin, part Methyl-etherified amino resins selects special 717 resins of cyanogen.
Its concrete preparation process is:
A, the preparation of polyester resin
(1) each raw material of polyester resin is weighed in proportion, standby；
(2), under inert gas environment, in reactor, neopentyl glycol, tetramethylolmethane, TMPD, different pungent is put into Acid, benzoic acid, adipic acid, THPA, phthalic anhydride, hypophosphorous acid, antioxidant 1010, stirring is warming up to 140 DEG C, and 2h is to slowly warm up to 180 DEG C, it is incubated 1h；1h is to slowly warm up to 200 DEG C, is incubated 1h；It is warming up to 210 DEG C, 210 DEG C of insulation reaction to acid number 17- 19mgKOH/g, cooling, add dimethylbenzene and divide water, point water is complete, is cooled to 130-140 DEG C, is sequentially added into propylene glycol monomethyl ether acetic acid Ester, butyl acetate, mixed dimethyl esters latting drown, filter and package, and obtains polyester resin, resin liquid outward appearance clear, solid part 80 ± 2%, viscosity (form pipe, 25 DEG C) 15-25S；
B, the preparation of semi-finished product mill base
(1) each raw material of coating in high solid content and low viscosity automotive OEM is weighed in proportion, standby；
(2) take the 1/2 of polyester resin quality to mix with dispersant, ethylene glycol ether acetate and Ketohexamethylene, stirring mixing Uniformly；
(3) rutile titanium dioxide, hollow glass bead, precipitated super-fine barium sulfate, white carbon black, the anti-settling agent above-mentioned mixing of addition are taken In solution, stir, be subsequently adding organosilicon levelling agent and acrylate levelling agent, be ground to sand mill after stirring Fineness is less than 10 microns；
(4) refer to that grinding test master grind color development effect reaches optimal, filters stand-by；
C, the preparation of resist sagging resin dispersion liquid
After remaining polyester resin, resist sagging resin and butylated amino resin are mixed being not less than 1400-1500 and turn/ Min high-speed stirred is less than 10 microns to fineness；
D, by qualified semi-finished product mill base and resist sagging resin dispersion liquid mix homogeneously, add leftover materials in formula, stir Mix uniformly, adjust viscosity, toning；
E, technical performance index detect；
F, strainer filtering with 300 mesh are packed and are i.e. obtained final products.
Embodiment 3
Being coated with coating in a kind of high solid content and low viscosity automotive OEM, by percentage to the quality, its raw material consists of: polyester resin 35%, resist sagging resin 5%, rutile titanium white lead 15%, hollow glass bead 2%, precipitated super-fine barium sulfate 15%, dispersant 2%, white carbon 0.1%, organosilicon levelling agent 0.1%, acrylate levelling agent 0.3%, surfactant 0.45%, ethylene glycol Ethyl ether acetate ester 3%, white carbon black 0.05%, butylated amino resin 20%, part methyl-etherified amino resins 2%.
Described polyester resin, in parts by weight, its raw material consists of: 0.5 part of benzoic acid, isooctyl acid 1 part, adipic acid 24 Part, THPA 2.5 parts, phthalic anhydride 13 parts, TMPD 0 part, neopentyl glycol 35 parts, tetramethylolmethane 5 parts, secondary Phosphoric acid 0.2 part, mixed dimethyl esters 10 parts, dimethylbenzene 0.5 part, propylene glycol methyl ether acetate 4 parts, butyl acetate 3 parts.
Resist sagging resin selects trade mark button to wear this 91795 resin, and rutile titanium white lead selects R706, precipitated super-fine barium sulfate Selecting 2500 mesh, dispersant is BYK161, and organosilicon levelling agent selects BYK331, and white carbon selects Degussa R972, acrylic acid Ester levelling agent selects the fluorine-containing levelling agent of afcona3670, the modest U99 of surfactant trade mark moral, and butylated amino resin selects button to wear This 138, part methyl-etherified amino resins selects special 717 resins of cyanogen.
Its concrete preparation process is:
A, the preparation of polyester resin
(1) each raw material of polyester resin is weighed in proportion, standby；
(2), under inert gas environment, in reactor, neopentyl glycol, tetramethylolmethane, TMPD, different pungent is put into Acid, benzoic acid, adipic acid, THPA, phthalic anhydride, hypophosphorous acid, antioxidant 1010, stirring is warming up to 140 DEG C, and 2h is to slowly warm up to 180 DEG C, it is incubated 1h；1h is to slowly warm up to 200 DEG C, is incubated 1h；It is warming up to 210 DEG C, 210 DEG C of insulation reaction to acid number 17- 19mgKOH/g, cooling, add dimethylbenzene and divide water, point water is complete, is cooled to 130-140 DEG C, is sequentially added into propylene glycol monomethyl ether acetic acid Ester, butyl acetate, mixed dimethyl esters latting drown, filter and package, and obtains polyester resin, resin liquid outward appearance clear, solid part 80 ± 2%, viscosity (form pipe, 25 DEG C) 15-25S；
B, the preparation of semi-finished product mill base
(1) each raw material of coating in high solid content and low viscosity automotive OEM is weighed in proportion, standby；
(2) take the 1/2 of polyester resin quality to mix with dispersant, ethylene glycol ether acetate and Ketohexamethylene, stirring mixing Uniformly；
(3) rutile titanium dioxide, hollow glass bead, precipitated super-fine barium sulfate, white carbon black, the anti-settling agent above-mentioned mixing of addition are taken In solution, stir, be subsequently adding organosilicon levelling agent and acrylate levelling agent, be ground to sand mill after stirring Fineness is less than 10 microns；
(4) refer to that grinding test master grind color development effect reaches optimal, filters stand-by；
C, the preparation of resist sagging resin dispersion liquid
After remaining polyester resin, resist sagging resin and butylated amino resin are mixed being not less than 1400-1500 and turn/ Min high-speed stirred is less than 10 microns to fineness；
D, by qualified semi-finished product mill base and resist sagging resin dispersion liquid mix homogeneously, add leftover materials in formula, stir Mix uniformly, adjust viscosity, toning；
E, technical performance index detect；
F, strainer filtering with 300 mesh are packed and are i.e. obtained final products.
Embodiment 4
Being coated with coating in a kind of high solid content and low viscosity automotive OEM, by percentage to the quality, its raw material consists of: polyester resin 25%, resist sagging resin 5%, rutile titanium white lead 15%, hollow glass bead 2%, precipitated super-fine barium sulfate 18%, dispersant 3%, white carbon 0.1%, organosilicon levelling agent 0.1%, acrylate levelling agent 0.3%, surfactant 0.2%, anti-settling agent 0.25%, Ketohexamethylene 4%, ethylene glycol ether acetate 3%, white carbon black 0.05%, butylated amino resin 20%, part methyl-etherified Amino resins 4%.
Described polyester resin, in parts by weight, its raw material consists of: 1 part of benzoic acid, isooctyl acid 0.5 part, adipic acid 22 Part, THPA 3 parts, phthalic anhydride 12 parts, TMPD 3 parts, neopentyl glycol 27 parts, tetramethylolmethane 6 parts, secondary phosphorus Acid 0.1 part, antioxidant 1010 0.02 part, dimethylbenzene 1.5 parts, propylene glycol methyl ether acetate 5 parts, butyl acetate 4 parts.
Resist sagging resin selects trade mark button to wear this 91795 resin, and rutile titanium white lead selects R706, precipitated super-fine barium sulfate Selecting 2500 mesh, dispersant is BYK161, and organosilicon levelling agent selects enlightening high by 450, and white carbon selects Degussa R972, acrylic acid Ester levelling agent selects the fluorine-containing levelling agent of afcona3670, the modest U99 of surfactant trade mark moral, and butylated amino resin selects Bath Husband 018 resin, part methyl-etherified amino resins selects special 717 resins of cyanogen.
Its concrete preparation process is:
A, the preparation of polyester resin
(1) each raw material of polyester resin is weighed in proportion, standby；
(2), under inert gas environment, in reactor, neopentyl glycol, tetramethylolmethane, TMPD, different pungent is put into Acid, benzoic acid, adipic acid, THPA, phthalic anhydride, hypophosphorous acid, antioxidant 1010, stirring is warming up to 140 DEG C, and 2h is to slowly warm up to 180 DEG C, it is incubated 1h；1h is to slowly warm up to 200 DEG C, is incubated 1h；It is warming up to 210 DEG C, 210 DEG C of insulation reaction to acid number 17- 19mgKOH/g, cooling, add dimethylbenzene and divide water, point water is complete, is cooled to 130-140 DEG C, is sequentially added into propylene glycol monomethyl ether acetic acid Ester, butyl acetate, mixed dimethyl esters latting drown, filter and package, and obtains polyester resin, resin liquid outward appearance clear, solid part 80 ± 2%, viscosity (form pipe, 25 DEG C) 15-25S；
B, the preparation of semi-finished product mill base
(1) each raw material of coating in high solid content and low viscosity automotive OEM is weighed in proportion, standby；
(2) take the 1/2 of polyester resin quality to mix with dispersant, ethylene glycol ether acetate and Ketohexamethylene, stirring mixing Uniformly；
(3) rutile titanium dioxide, hollow glass bead, precipitated super-fine barium sulfate, white carbon black, the anti-settling agent above-mentioned mixing of addition are taken In solution, stir, be subsequently adding organosilicon levelling agent and acrylate levelling agent, be ground to sand mill after stirring Fineness is less than 10 microns；
(4) refer to that grinding test master grind color development effect reaches optimal, filters stand-by；
C, the preparation of resist sagging resin dispersion liquid
After remaining polyester resin, resist sagging resin and butylated amino resin are mixed being not less than 1400-1500 and turn/ Min high-speed stirred is less than 10 microns to fineness；
D, by qualified semi-finished product mill base and resist sagging resin dispersion liquid mix homogeneously, add leftover materials in formula, stir Mix uniformly, adjust viscosity, toning；
E, technical performance index detect；
F, strainer filtering with 300 mesh are packed and are i.e. obtained final products.
Embodiment 5
Being coated with coating in a kind of high solid content and low viscosity automotive OEM, by percentage to the quality, its raw material consists of: polyester resin 25%, resist sagging resin 5%, rutile titanium white lead 15%, hollow glass bead 2%, precipitated super-fine barium sulfate 12%, dispersant 1%, white carbon 0.3%, organosilicon levelling agent 0.2%, acrylate levelling agent 0.5%, surfactant 0.5%, anti-settling agent 2%, Ketohexamethylene 3.3%, ethylene glycol ether acetate 3%, white carbon black 0.2%, butylated amino resin 28%, part methyl-etherified ammonia Base resin 2%.
Described polyester resin, in parts by weight, its raw material consists of: 1.5 parts of benzoic acid, adipic acid 23 parts, tetrahydrochysene benzene Acid anhydride 4 parts, phthalic anhydride 14 parts, TMPD 5 parts, neopentyl glycol 32 parts, tetramethylolmethane 6 parts, hypophosphorous acid 0.25 part, Antioxidant 1010 0.07 part, mixed dimethyl esters 15 parts, propylene glycol methyl ether acetate 4.5 parts, butyl acetate 3.5 parts.
Resist sagging resin selects trade mark button to wear this 91795 resin, and rutile titanium white lead selects R706, precipitated super-fine barium sulfate Selecting 2500 mesh, dispersant is BYK161, and organosilicon levelling agent selects BYK331, and white carbon selects Degussa R972, acrylic acid Ester levelling agent select BKY399, the modest U99 of surfactant trade mark moral, butylated amino resin select button wear this 138, part methyl ether Change amino resins and select special 717 resins of cyanogen.
Its concrete preparation process is:
A, the preparation of polyester resin
(1) each raw material of polyester resin is weighed in proportion, standby；
(2), under inert gas environment, in reactor, neopentyl glycol, tetramethylolmethane, TMPD, different pungent is put into Acid, benzoic acid, adipic acid, THPA, phthalic anhydride, hypophosphorous acid, antioxidant 1010, stirring is warming up to 140 DEG C, and 2h is to slowly warm up to 180 DEG C, it is incubated 1h；1h is to slowly warm up to 200 DEG C, is incubated 1h；It is warming up to 210 DEG C, 210 DEG C of insulation reaction to acid number 17- 19mgKOH/g, cooling, add dimethylbenzene and divide water, point water is complete, is cooled to 130-140 DEG C, is sequentially added into propylene glycol monomethyl ether acetic acid Ester, butyl acetate, mixed dimethyl esters latting drown, filter and package, and obtains polyester resin, resin liquid outward appearance clear, solid part 80 ± 2%, viscosity (form pipe, 25 DEG C) 15-25S；
B, the preparation of semi-finished product mill base
(1) each raw material of coating in high solid content and low viscosity automotive OEM is weighed in proportion, standby；
(2) take the 1/2 of polyester resin quality to mix with dispersant, ethylene glycol ether acetate and Ketohexamethylene, stirring mixing Uniformly；
(3) rutile titanium dioxide, hollow glass bead, precipitated super-fine barium sulfate, white carbon black, the anti-settling agent above-mentioned mixing of addition are taken In solution, stir, be subsequently adding organosilicon levelling agent and acrylate levelling agent, be ground to sand mill after stirring Fineness is less than 10 microns；
(4) refer to that grinding test master grind color development effect reaches optimal, filters stand-by；
C, the preparation of resist sagging resin dispersion liquid
After remaining polyester resin, resist sagging resin and butylated amino resin are mixed being not less than 1400-1500 and turn/ Min high-speed stirred is less than 10 microns to fineness；
D, by qualified semi-finished product mill base and resist sagging resin dispersion liquid mix homogeneously, add leftover materials in formula, stir Mix uniformly, adjust viscosity, toning；
E, technical performance index detect；
F, strainer filtering with 300 mesh are packed and are i.e. obtained final products.

Claims (4)

1. a high solid content and low viscosity automotive OEM is coated with coating, it is characterised in that: by percentage to the quality, its raw material consists of: Polyester resin 25-35%, resist sagging resin 5-12%, rutile titanium white lead 15-25%, hollow glass bead 0-2% are ultra-fine heavy Shallow lake barium sulfate 12-18%, dispersant 1-3%, white carbon 0.1-0.3%, organosilicon levelling agent 0.1-0.3%, acrylate stream Flat agent 0.3-0.6%, surfactant 0.2-0.5%, anti-settling agent 0-2%, Ketohexamethylene 0-4%, ethylene glycol ether acetate 3- 5%, white carbon black 0.05-0.2%, butylated amino resin 20-28%, part methyl-etherified amino resins 2-4%.
A kind of high solid content and low viscosity automotive OEM the most according to claim 1 is coated with coating, it is characterised in that: described is poly- Ester resin, in parts by weight, its raw material consists of: benzoic acid 0-1.5 part, isooctyl acid 0-2.0 part, adipic acid 20-28 part, tetrahydrochysene Phthalic anhydride 0-5 part, phthalic anhydride 10-16 part, TMPD 0-5 part, neopentyl glycol 25-35 part, tetramethylolmethane 4-7 Part, hypophosphorous acid 0-0.3 part, antioxidant 1010 0-0.1 part, mixed dimethyl esters 0-15 part, dimethylbenzene 0-2.0 part, propylene glycol first Ether acetate 3-6 part, butyl acetate 2-5 part.
A kind of high solid content and low viscosity automotive OEM the most according to claim 1 and 2 is coated with coating it is characterized in that: resist sagging Resin selects trade mark button to wear this 91795 resin, and R706 selected by rutile titanium white lead, and precipitated super-fine barium sulfate selects 2500 mesh, point Powder is BYK161, and organosilicon levelling agent selects BYK331 or enlightening high by 450, and white carbon selects Degussa R972, acrylate stream The fluorine-containing levelling agent of BKY399 or afcona3670, the modest U99 of surfactant trade mark moral are selected in flat agent, and butylated amino resin is selected Button wear this 138 or BASF 018 resin, part methyl-etherified amino resins selects special 717 resins of cyanogen.
4. the preparation method of coating in a high solid content and low viscosity automotive OEM, it is characterised in that: it concretely comprises the following steps:
A, the preparation of polyester resin
(1) each raw material of polyester resin is weighed in proportion, standby；
(2), under inert gas environment, in reactor, neopentyl glycol, tetramethylolmethane, TMPD, isooctyl acid, benzene are put into Formic acid, adipic acid, THPA, phthalic anhydride, hypophosphorous acid, antioxidant 1010, stirring is warming up to 140 DEG C, and 2h is to slowly warm up to 180 DEG C, it is incubated 1h；1h is to slowly warm up to 200 DEG C, is incubated 1h；It is warming up to 210 DEG C, 210 DEG C of insulation reaction to acid number 17-19mgKOH/ G, cooling, add dimethylbenzene and divide water, point water is complete, is cooled to 130-140 DEG C, is sequentially added into propylene glycol methyl ether acetate, acetic acid Butyl ester, mixed dimethyl esters latting drown, filter and package, and obtains polyester resin, resin liquid outward appearance clear, solid part 80 ± 2%, glues Degree (form pipe, 25 DEG C) 15-25S；
B, the preparation of semi-finished product mill base
(1) each raw material of coating in high solid content and low viscosity automotive OEM is weighed in proportion, standby；
(2) take the 1/2 of polyester resin quality to mix with dispersant, ethylene glycol ether acetate and Ketohexamethylene, be uniformly mixed；
(3) rutile titanium dioxide, hollow glass bead, precipitated super-fine barium sulfate, white carbon black, the anti-settling agent above-mentioned mixed solution of addition are taken In, stir, be subsequently adding organosilicon levelling agent and acrylate levelling agent, after stirring, be ground to fineness with sand mill Less than 10 microns；
(4) refer to that grinding test master grind color development effect reaches optimal, filters stand-by；
C, the preparation of resist sagging resin dispersion liquid
/ min is turned being not less than 1400-1500 after remaining polyester resin, resist sagging resin and butylated amino resin are mixed High-speed stirred is less than 10 microns to fineness；
D, by qualified semi-finished product mill base and resist sagging resin dispersion liquid mix homogeneously, add leftover materials in formula, stirring is all Even, adjust viscosity, toning；
E, technical performance index detect；
F, strainer filtering with 300 mesh are packed and are i.e. obtained final products.
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CN107903796A (en) * 2017-12-07 2018-04-13 江苏足迹涂料有限公司 Coating and preparation method thereof is applied in a kind of two-component large arch dam of low stain environment-friendly type
CN111138930A (en) * 2020-01-20 2020-05-12 东莞大宝化工制品有限公司 VOC (volatile organic compound) reducing odor-free automobile paint and preparation method thereof
CN112851920A (en) * 2020-12-31 2021-05-28 东胜化学(上海)有限公司 Alkyd resin and preparation method thereof
CN112851920B (en) * 2020-12-31 2021-12-07 东胜化学(上海)有限公司 Alkyd resin and preparation method thereof
CN114958157A (en) * 2022-06-29 2022-08-30 湖南湘江关西涂料有限公司 Acrylic resin paint, composite paint structure and preparation method thereof

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