CN108484893A - A kind of processing method suitable for composite material application powdery paints - Google Patents
A kind of processing method suitable for composite material application powdery paints Download PDFInfo
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- CN108484893A CN108484893A CN201810364894.0A CN201810364894A CN108484893A CN 108484893 A CN108484893 A CN 108484893A CN 201810364894 A CN201810364894 A CN 201810364894A CN 108484893 A CN108484893 A CN 108484893A
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- polyester resin
- powdery paints
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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
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/695—Polyesters containing atoms other than carbon, hydrogen and oxygen containing silicon
- C08G63/6954—Polyesters containing atoms other than carbon, hydrogen and oxygen containing silicon derived from polxycarboxylic acids and polyhydroxy compounds
- C08G63/6956—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
- 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
- C09D5/03—Powdery paints
-
- 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
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
Abstract
The invention belongs to chemical material fields, and in particular to a kind of processing method suitable for composite material application powdery paints.The preparation method of polyester resin is：Temperature of reaction kettle is risen to 85~95 DEG C, neopentyl glycol, 1,6 hexylene glycols, Isosorbide-5-Nitrae cyclohexanediol, Isosorbide-5-Nitrae cyclohexane diacid, cis-aconitic, tartaric acid, germanium tetraiodide, trimethylolpropane is added；230 DEG C are warming up to, reaction to acid value reaches 10~15mgKOH/g；Silane coupling agent and terephthalic acid (TPA) is added, is warming up to 280 DEG C, adds three (2,4 di-tert-butyl-phenyl) phosphite esters and tetraethylammonium bromide, stir evenly, cools down up to polyester resin.Using polyester resin as raw material, 280 parts of polyester resin, 200~220 parts of TGIC, 5 parts of Resiflow PV88,3 parts of styrax, 155 parts of titanium dioxide, 155 parts of ultra-fine barium prepare powdery paints.Powdery paints provided by the invention, flat appearance, glossiness be good, weather resistance and excellent in mechanical performance, solidification temperature are low.
Description
Technical field
The invention belongs to chemical material fields, and in particular to a kind of processing suitable for composite material application powdery paints
Method.
Background technology
Polyester resin powder coating is a kind of novel weathering resistant powdery paints, is shunk at present with polyester-isocyanuric acid three sweet
Based on two kinds of systems of grease (TGIC) and polyester-hydroxyalkylamides (HAA).Polyester resin powder coating has good before curing
Mobility, the coating after film forming has the advantages such as levelling is good, gloss is high, mechanical strength is big again, therefore, in powdery paints
Occupation rate of market increase year by year.
But polyester-TGIC systems powdery paints there are solidification temperatures it is high, weatherability is bad the problems such as, and polyester-HAA systems
Again because its degree of functionality is high, activity is strong, there are the easy moisture absorption, levelling is high the problems such as.
Therefore, a kind of relatively low novel solidification temperature, high comprehensive performance, the good polyester-TGIC powder of weatherability are researched and developed
Last coating and its processing method, have important practical significance and promotional value.
Invention content
The object of the present invention is to provide a kind of processing methods suitable for composite material application powdery paints.
For achieving the above object, the technical solution adopted in the present invention is：A kind of preparation method of polyester resin, will
Temperature of reaction kettle rises to 85~95 DEG C, under nitrogen protection, neopentyl glycol, 1,6- hexylene glycols, Isosorbide-5-Nitrae cyclohexanediol, Isosorbide-5-Nitrae ring is added
Adipic acid, cis-aconitic, tartaric acid, germanium tetraiodide, trimethylolpropane continue under nitrogen protection, to be warming up to 230 DEG C,
Insulation reaction, reaction to clarification in system, without particle, acid value reaches 10~15mgKOH/g；Silane coupling agent is added and to benzene two
Formic acid is warming up to 280 DEG C, continues under nitrogen protection, reaction reaches 30~35mgKOH/g to acid value, adds three (2,4- bis-
Tert-butyl-phenyl) phosphite ester and tetraethylammonium bromide, it stirs evenly, cools down up to polyester resin.
Preferably, in parts by weight, 10~15 parts of neopentyl glycol, 10~15 parts of 1,6- hexylene glycols, Isosorbide-5-Nitrae cyclohexanediol 10~
15 parts, 10~15 parts of 1,4 cyclohexane diacid, 10~15 parts of cis-aconitic, 10~15 parts of terephthalic acid (TPA), 3~5 parts of tartaric acid,
0.08~0.1 part of germanium tetraiodide, 3~5 parts of silane coupling agent, three 0.5 part of (2,4- di-tert-butyl-phenyls) phosphite esters, three hydroxyl first
1 part of base propane, 0.5 part of tetraethylammonium bromide.
Preferably, 15 parts of the neopentyl glycol, 10 parts of 1,6- hexylene glycols, 15 parts of Isosorbide-5-Nitrae cyclohexanediol, Isosorbide-5-Nitrae cyclohexane diacid 10
Part, 15 parts of cis-aconitic, 10 parts of terephthalic acid (TPA), 5 parts of tartaric acid, 0.1 part of germanium tetraiodide, 3 parts of silane coupling agent.
Preferably, the polyester resin of preparation, acid value are 25~30mgKOH/g.
Correspondingly, the powdery paints prepared as raw material using the polyester resin.
Preferably, the powdery paints is formulated in parts by weight and is：280 parts of polyester resin, 200~220 parts of TGIC,
5 parts of Resiflow PV88,3 parts of styrax, 155 parts of titanium dioxide, 155 parts of ultra-fine barium.
Preferably, the TGIC is 200 parts.
The invention has the advantages that：Powdery paints provided by the invention, flat appearance, glossiness be good, weatherability
Energy and excellent in mechanical performance, solidification temperature are low.
Specific implementation mode
In parts by weight, the formula composition of polyester resin is：10~15 parts of neopentyl glycol, 10~15 parts of 1,6- hexylene glycols,
1,4 10~15 parts of cyclohexanediols, 10~15 parts of 1,4 cyclohexane diacid, 10~15 parts of cis-aconitic, terephthalic acid (TPA) 10~15
Part, 3~5 parts of tartaric acid, 0.08~0.1 part of germanium tetraiodide (catalyst), 3~5 parts of silane coupling agent (end-capping reagent), three (2,4-
Di-tert-butyl-phenyl) 0.5 part of phosphite ester (antioxidant), 1 part of trimethylolpropane (branching agent), tetraethylammonium bromide (solidification
Accelerating agent) 0.5 part.
Preparation method：Temperature of reaction kettle is risen to 85~95 DEG C, under nitrogen protection, be added neopentyl glycol, 1,6- oneself two
Alcohol, Isosorbide-5-Nitrae cyclohexanediol, Isosorbide-5-Nitrae cyclohexane diacid, cis-aconitic, tartaric acid, germanium tetraiodide, trimethylolpropane continue in nitrogen
Under protection, it is warming up to 230 DEG C, insulation reaction, clarification in reaction to system, without particle, acid value reaches 10~15mgKOH/g.Add
Entering silane coupling agent and terephthalic acid (TPA), be warming up to 280 DEG C, continues under nitrogen protection, reaction to acid value reaches 30~
35mgKOH/g adds three (2,4- di-tert-butyl-phenyl) phosphite esters and tetraethylammonium bromide, stirs evenly, cool down to obtain the final product
Polyester resin.
In parts by weight, the formula of powdery paints：250~280 parts of polyester resin, 20~210 parts of TGIC, Resiflow
5~7 parts of PV88 (levelling agent), 3~5 parts of styrax, 150~170 parts of titanium dioxide, 150~180 parts of ultra-fine barium (filler).It will be upper
State that component mixing in formula, extrusion, crushing, sieving is to get powdery paints.
Explanation is further explained to the present invention with reference to specific embodiment.
Embodiment 1：The preparation of polyester resin and performance
1, polyester resin is prepared
Preparation method：Temperature of reaction kettle is risen to 95 DEG C, under nitrogen protection, neopentyl glycol, 1,6- hexylene glycols, 1 is added,
4 cyclohexanediols, Isosorbide-5-Nitrae cyclohexane diacid, cis-aconitic, tartaric acid, germanium tetraiodide, 1 part of trimethylolpropane continue to protect in nitrogen
Under shield, it is warming up to 230 DEG C, insulation reaction, clarification in reaction to system, without particle measures acid value and reaches 10~15mgKOH/g.
Silane coupling agent and terephthalic acid (TPA) is added, is warming up to 280 DEG C, continues under nitrogen protection, reaction to acid value reaches 30~
35mgKOH/g, adds 0.5 part of 0.5 part of three (2,4- di-tert-butyl-phenyl) phosphite ester and tetraethylammonium bromide, and stirring is equal
It is even, cool down up to polyester resin.
In each group, each prescription weight being actually added into is as shown in table 1.
Prescription weight in 1 each group of table
2, polyester resin performance test
Polyester resin prepared by each group is as shown in table 2.
2 each group polyester resin performance of table is shown
| Performance indicator | Group 1 | Group 2 | Group 3 | Group 4 | Group 5 |
| Acid value (mg KOH/g) | 25 | 27 | 28 | 27 | 30 |
| Viscosity (200 DEG C, Pas) | 5.3 | 5.0 | 5.0 | 5.1 | 4.9 |
| Tg(℃) | 69 | 67 | 67 | 62 | 65 |
| Softening point (ring and ball method, DEG C) | 98 | 105 | 102 | 101 | 107 |
The acid value of polyester resin is lower to illustrate that the extent of reaction is higher, existing studies have shown that the acid value of polyester resin is low more has
Conducive to the weather resistance of raising powdery paints.In addition, in general, viscosity is higher, compactness, the flexibility of post-coatings film
Preferably, but appearance (flatness, finish etc.) is poor；Viscosity is relatively low, follow-up film good leveling property, appearance property and impact property
By force.Glass transition temperature (Tg) height can be to avoid powder agglomates, and Tg is relatively low, is more advantageous to the levelling of powder.
Comprehensive polyester resin indices, the polyester resin of selection group 1, the base-material as follow-up powdery paints.
Embodiment 2：The preparation of powdery paints and performance
1, prepared by powdery paints：
The polyester resin that in selection example 1 prepared by group 1.
In parts by weight, powder coating formulation：280 parts of polyester resin, 200~230 parts of TGIC, Resiflow PV88
5 parts of (levelling agent), 3 parts of styrax, 155 parts of titanium dioxide, 155 parts of ultra-fine barium (filler).By in above-mentioned formula component mixing, squeeze
Go out, crush, be sieved to get powdery paints.Hardening time is 15min.
Each group actual parameter is as shown in table 3.
Parameter Conditions in 3 each group of table
| Component | Group 1 | Group 2 | Group 3 | Group 4 | Group 5 |
| Polyester resin (part) | 280 | 280 | 280 | 280 | 280 |
| TGIC (part) | 200 | 200 | 210 | 220 | 230 |
| Solidification temperature (DEG C) | 180 | 130 | 180 | 180 | 180 |
2, performance test
(1) melt fluidity
By GB/T21782.11-2010《Tilt the measurement of version mobility》Method carries out.0.5g powdery paints is weighed first
It puts into steel press mold device, is pressed into the test piece that thickness is 6mm, test piece is put into oneself and pulls the substrate circle of a diameter of 12.7mm
Place, and be put into the metal frame of constant temperature (solidification temperature) baking oven, keep horizontal 3min.Then metal frame is controlled from horizontal position
65 ° of inclination is set, and keeps 30min in the position.Substrate, the standardized maximum label of flow distance are finally taken out from baking oven
Line finally measures the center line of test piece in original substrate to the distance of mark line, as sample powder melt fluidity.
(2) gel time
According to GB/T16995-1997《The measurement of thermosetting powder coating gel time at a given temperature》Method passes through
Gelatinization instrument carries out gel time measurement.It takes lml sample powder to be placed on hot plate, paves the range in diameter about 50mm quickly with scraper
It is interior, start timing when powder melts, is used in combination stirring glass bar to do cyclic motion in the resin of melting, when resin is unable to wire drawing
Or when cannot flow, it is considered as gelling point, stops timing.Experiment in triplicate, is averaged as gel time.
(3) gloss
Using GB/T9754-2007《20 °, 60 ° and 85 ° mirrors of colored paint paint film of the paint and varnish one without metallic pigments
The measurement of face gloss》In method measure.It is tested herein using 60 ° of glossometers, three is taken in coating surface different location
Reading records average value as coating gloss value if error is less than 5 units.
(4) impact strength
Using GB/T1732-93《Paint film impact resistance measuring method》Method is tested using coating impactor.Test ensures
Temperature carries out under conditions of 23 ± 2 DEG C and relative humidity are 50 ± 5%, sample coatings is lain on anvil upward, weight
(tup diameter 8mm, quality lkg) is fixed on a certain height of slide cartridge, presses control knob, and weight is freely fallen on punch.It carries
Weight is played, substrate is taken out.Same test plate (panel) carries out 3 Secondary Shocks experiments, and whether there are cracks for observation paint film, phenomena such as peeling off.
(5) adhesive force
Using GB/T928-1999《The frame of paint and varnish coating is tested》Method is surveyed using multi-edge cutting knife tool
Examination.Test carries out under conditions of 23 ± 2 DEG C and relative humidity are 50 ± 5%, uniformly exerts a force to cutting tool, and all cuttings are all
It should draw to surface of bottom material, ultimately form 90.Staggeredly, network graphic is formed.It is used in combination banister brush to be handled with adhesive tape, observes appearance of coat
Whether obscission is had.
(6) weather resistance
Using artificially roughening, in ultraviolet light accelerates weather-proof test-run a machine, with reference to the normal spaces GB/T1865-2009
Sampling, 4h irradiation, 4h condensations, 20min sprays (cycle 5 times) carry out weather-proof test to coating performance.
Performance powder coating prepared by above-mentioned each group is specifically as shown in table 4.
4 each group performance powder coating of table is shown
From table 4, it can be seen that using the technical solution of group 2, when curing at 130 DEG C, it is already possible to reach extremely excellent effect
Fruit, it is better when promotion to 180 DEG C (groups 1) cures.
Claims (7)
1. a kind of preparation method of polyester resin, it is characterised in that：Temperature of reaction kettle is risen to 85~95 DEG C, in nitrogen protection
Under, neopentyl glycol, 1,6- hexylene glycols, Isosorbide-5-Nitrae cyclohexanediol, Isosorbide-5-Nitrae cyclohexane diacid, cis-aconitic, tartaric acid, tetraiodide is added
Germanium, trimethylolpropane continue under nitrogen protection, to be warming up to 230 DEG C, and insulation reaction is reacted to clarification, nothing in system
Grain, acid value reach 10~15mgKOH/g；Silane coupling agent and terephthalic acid (TPA) is added, is warming up to 280 DEG C, continues to protect in nitrogen
Under shield, reaction reaches 30~35mgKOH/g to acid value, adds three (2,4- di-tert-butyl-phenyl) phosphite esters and tetrem bromide
Change ammonium, stir evenly, cools down up to polyester resin.
2. the preparation method of polyester resin according to claim 1, it is characterised in that：In parts by weight, neopentyl glycol 10~
15 parts, 10~15 parts of 1,6- hexylene glycols, 10~15 parts of Isosorbide-5-Nitrae cyclohexanediol, 10~15 parts of Isosorbide-5-Nitrae cyclohexane diacid, cis-aconitic 10
~15 parts, 10~15 parts of terephthalic acid (TPA), 3~5 parts of tartaric acid, 0.08~0.1 part of germanium tetraiodide, 3~5 parts of silane coupling agent,
Three 0.5 part of (2,4- di-tert-butyl-phenyls) phosphite esters, 1 part of trimethylolpropane, 0.5 part of tetraethylammonium bromide.
3. the preparation method of polyester resin according to claim 2, it is characterised in that：15 parts of the neopentyl glycol, 1,6- oneself
10 parts of glycol, 15 parts of 1,4 cyclohexanediol, 10 parts of 1,4 cyclohexane diacid, 15 parts of cis-aconitic, 10 parts of terephthalic acid (TPA), tartaric acid
5 parts, 0.1 part of germanium tetraiodide, 3 parts of silane coupling agent.
4. the preparation method of polyester resin according to claim 3, it is characterised in that：The polyester resin of preparation, acid value 25
~30mgKOH/g.
5. the powdery paints prepared as raw material using the polyester resin prepared by Claims 1 to 4 any one.
6. powdery paints according to claim 5, it is characterised in that：In parts by weight, it is formulated and is：280 parts of polyester resin,
200~220 parts of TGIC, 5 parts of Resiflow PV88,3 parts of styrax, 155 parts of titanium dioxide, 155 parts of ultra-fine barium.
7. powdery paints according to claim 6, it is characterised in that：The TGIC is 200 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810364894.0A CN108484893A (en) | 2018-04-23 | 2018-04-23 | A kind of processing method suitable for composite material application powdery paints |
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| CN201810364894.0A CN108484893A (en) | 2018-04-23 | 2018-04-23 | A kind of processing method suitable for composite material application powdery paints |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108530611A (en) * | 2018-04-23 | 2018-09-14 | 黄山学院 | A kind of polyester resin and the powdery paints containing the polyester resin |
| CN111333827A (en) * | 2020-04-22 | 2020-06-26 | 黄山市源润新材料科技有限公司 | High-hardness and high-stability 60/40 mixed type polyester resin for powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101076566A (en) * | 2004-12-13 | 2007-11-21 | 三菱化学株式会社 | Polyester resin composition, process for producing the same and molding thereof |
| CN102977346A (en) * | 2012-11-20 | 2013-03-20 | 广州擎天实业有限公司 | Polyester resin for triglycidyl isocyanurate (TGIC)-cured weather-resistant heat transfer printing powdery paint and preparation method thereof |
| CN108530611A (en) * | 2018-04-23 | 2018-09-14 | 黄山学院 | A kind of polyester resin and the powdery paints containing the polyester resin |
-
2018
- 2018-04-23 CN CN201810364894.0A patent/CN108484893A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101076566A (en) * | 2004-12-13 | 2007-11-21 | 三菱化学株式会社 | Polyester resin composition, process for producing the same and molding thereof |
| CN102977346A (en) * | 2012-11-20 | 2013-03-20 | 广州擎天实业有限公司 | Polyester resin for triglycidyl isocyanurate (TGIC)-cured weather-resistant heat transfer printing powdery paint and preparation method thereof |
| CN108530611A (en) * | 2018-04-23 | 2018-09-14 | 黄山学院 | A kind of polyester resin and the powdery paints containing the polyester resin |
Non-Patent Citations (2)
| Title |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108530611A (en) * | 2018-04-23 | 2018-09-14 | 黄山学院 | A kind of polyester resin and the powdery paints containing the polyester resin |
| CN111333827A (en) * | 2020-04-22 | 2020-06-26 | 黄山市源润新材料科技有限公司 | High-hardness and high-stability 60/40 mixed type polyester resin for powder and preparation method thereof |
| CN111333827B (en) * | 2020-04-22 | 2022-06-10 | 黄山市源润新材料科技有限公司 | High-hardness and high-stability 60/40 mixed type polyester resin for powder and preparation method thereof |
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