CN1250795A - Powder paint contg. polyethylene glycol terephthalate, and method for preparing same - Google Patents
Powder paint contg. polyethylene glycol terephthalate, and method for preparing same Download PDFInfo
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- CN1250795A CN1250795A CN 98120949 CN98120949A CN1250795A CN 1250795 A CN1250795 A CN 1250795A CN 98120949 CN98120949 CN 98120949 CN 98120949 A CN98120949 A CN 98120949A CN 1250795 A CN1250795 A CN 1250795A
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Abstract
A powder coating composition includes 100 wt. portions of PET resin granules of flakes obtained from recovered PET moulding product and (i) 5-40 wt. portions of polyester (not PET) or modified polyester resin, (ii) 3-30 wt. portions of modified polyolefin resin or ethylene-acrylic acid copolymer resin, or (iii) 3-30 wt. portions of fused blend material of polycarbonate resin. The said powder material exhibits improved adhesion with metallic surface.
Description
The present invention relates to and can film or the PET toner of analogue such as paint film by forming with surperficial tight adhesion such as metal, and its preparation method.The present invention can use the small shreds of returnable such as PET bottle as the PET resin raw material.
PET (polyethylene terephthalate) is low with the adhesivity of metallic surface.Simultaneously, even this material is when forming baking and film, the degree of crystallinity of filming increases, the trend aggravation that also causes crackle or peel off.Therefore, this resin is not usually as powder coating (powder paints).In addition, PET resin and the common thermotolerance of other thermoplastic resins are low and have elasticity.Therefore, when grinding at normal temperatures, the particle of grinding has the projection of the length of similar wire rod or whisker above 1mm, makes and can not handle this polymkeric substance with powder type.Usually, requiring the powder particle size as static coating is 5-150 μ m (median size 40 μ m), and the powder that is used for fluidization dipping is 60-350 μ m (average particle size particle size 40 μ m).Therefore, grind the fine powder (5-350 μ m) that is difficult to prepare suitable powder coating or similar coating by standard machinery.Grinding at present is to be undertaken by the freeze grinding method of using liquid nitrogen.Freeze grinding needs a large amount of liquid nitrogen, the special applications that also must make shredder and other utility appliance be suitable for bearing low temperature environment simultaneously.This just needs to be equipped with huge equipment, and the result has increased the grinding cost.
Therefore, an object of the present invention is in order to make the PET resin with metlbond power difference have tight adhesion power and a kind of powder coating that can be used as static coating and fluidization dipping is provided.
Another object of the present invention provides a kind of food container that uses recovery such as PET bottle as the powder coating of raw material, has become serious social concern at present and abandon these containers.
In brief, following description can obviously embody these purposes of the present invention and other purposes can realize by a kind of composition as powder coating, said composition comprises 100 weight part PET resin granular materials or the small pieces that obtained by the PET layered product that reclaims and (i) 5-40 weight part polyester (except that PET) or modified polyester resin, (ii) 3-30 weight part modified polyolefin resin or ethylene unsaturated carboxylic acid's copolymer resin, or the (iii) melt blended material of 3-30 weight part polycarbonate resin, the adhesive power that this powdered material demonstrates itself and metallic surface is improved.
In the methods of the invention, the sheet stock that obtains with the PET resin granular material or by the PET product that " mechanical mill " reclaims or mix with the improving agent that improves metlbond power and formation fused films performance by the pellet that the above-mentioned sheet stock of the further melt kneading of forcing machine obtains.The gained mixture is obtained composite particles by the forcing machine melt kneading, make it reach 35% or higher degree of crystallinity at 170 ℃ of heating preset times this pellet then.Then with this pellet mechanical mill or be dissolved in the conventional solvent and obtain fine powder with chemical process.
The suitable example of properties-correcting agent comprises the vibrin except that PET, for example polybutylene terephthalate, PEN, modified polyester resin, with unsaturated carboxylic acid or its acid anhydrides (for example vinylformic acid, methacrylic acid, toxilic acid, fumaric acid and methylene-succinic acid; Maleic anhydride, itaconic anhydride etc.) polyolefin resin of modification, also have the copolymer resin of acid and alkene or polycarbonate resin.
Modified polyester resin is converted into the mixture that (for example) 40wt% PET resin, 40wt% PBT resin and 20wt% have the low molecular weight olefins wax of bond properties can make its storing temperature reduce.The dosage of corresponding properties-correcting agent is the 5-40 weight part, about preferred 20 weight parts (by the raw material PET resin of 100 weight parts).With unsaturated carboxylic acid or its anhydride modified polyolefine, maleic anhydride modified polyolefine is preferably to have the adhering resin of driving fit.Maleic anhydride modified polyolefine is to prepare by 100 weight part low molecular weight olefins resins are mediated with 10-40 weight part maleic anhydride, and using 30 weight part maleic anhydrides is preferred for tight adhesion.The dosage of maleic anhydride modified olefin resin is 3 to 30 weight parts, the maleic anhydride of preferred 5 to 20 weight parts (by 100 weight part PET resins).Equally for the copolymer resin that uses vinylformic acid or its analogue and alkene or polycarbonate resin as properties-correcting agent, its dosage is the 3-30 weight part.Given this and need the properties-correcting agent consumption of blend is as much as possible little because it be to utilize the PET resin that reclaims that a purpose is arranged in the object of the invention.But because the properties-correcting agent add-on causes itself and the improvement of metal adhesion power little for a short time, the hardness of filming increases, and shock resistance reduces, so will regulate its add-on according to required film performance.
Properties-correcting agent can use or mix use separately.The degree of crystallinity that contains the composition pellet of corresponding properties-correcting agent is 20-30%, and can produce the brilliant projection of similar palpus by the pellet of ordinary method mechanical mill on the surface of abrasive grains, causes it can not be used as powder coating.Yet, pellet is heated to 166 ± 10 ℃ (this temperature is the crystallization range of base-material PET resin) or is heated to 170 ℃ of a few hours (temperature that is fit to industrial purposes), can increase degree of crystallinity (confirming) by dsc analysis.When reach in degree of crystallinity 35% or bigger after when carrying out mechanical mill, no longer producing must brilliant projection, particle is mainly sphere.Simultaneously, milling time is tending towards in the ratio of degree of crystallinity shortening.
Described the present invention till now prevailingly, by further understanding the present invention with reference to following specific embodiment, the purpose of these embodiment that provide only is used to illustrate the present invention, rather than limits the invention (except as otherwise noted).
Embodiment 1
Will be by the PET bottle regenerated PET resin granular material (commercial product), polybutylene terephthalate (PBT) resin (the Ube Kosan KK that reclaim, PET 1000F01) and titanium dioxide (Ishihara SangyoKK.CR-97) add to roll in the machine of mixing by the proportion scale that provides in the table 1 and mix, and under 270 ℃, mediate-extrude with biaxial extruder (PMT-32, IKG KK).After the water stretching made it reach diameter 2mm, it is long that they are cut into about 3mm with cutting machine, and make it become the pellet that is used for corresponding prescription with gained line material.
Table 1
| The PET weight part | The polybutylene terephthalate weight part | The titanium dioxide weight part | |
| Prescription 1 | ????99 | ????1 | ????2.63 |
| Prescription 2 | ????95 | ????5 | ????2.63 |
| Prescription 3 | ????90 | ????10 | ????2.63 |
| Prescription 4 | ????80 | ????20 | ????2.63 |
The pellet degree of crystallinity that obtains in all prescriptions all is 30% or lower.These pellets are ground at normal temperatures, on the abrasive grains surface, produce the brilliant projection of the long palpus of 1-2mm, therefore hindered their uses in formulation for coating material.
When these pellets were heated 6 hours down at 170 ℃ with the taper blending machine that has oil jacket, degree of crystallinity increases to 35% or bigger.Then it is cooled to normal temperature, then it is added under 30 kg/h feed rates and have rotating blade and the rotating speed 5 of 0.4mm at interval, in the high-speed screw mill of 000rpm (KK Seishin Kigyo, SP-420 type), and grind by desk-top charging machine.Then with this abrasive product by in the sorter that 300 μ m sieves (Hi-sieve-NR-460S, Shin Tokyo Kikai KK) is housed, so remove the coarse particles that surpasses 300 μ m.The Powder Recovery of removing is gone in the above-mentioned high-speed screw mill.This sealing and circulating grinding was carried out 1 hour.The median size of the powder that obtains is about 180 μ m (particle size range 45-355 μ m).When be 17 decimals heat-up time, the degree of crystallinity of each prescription provided in table 2, and the load electric current and the degree of crystallinity of shredder reduce pro rata simultaneously.(KKSeishin Kigyo PRS-85) measures particle size distribution with the screening metering facility.
Table 2
| Degree of crystallinity | |
| Batching 1 | ????47％ |
| Batching 2 | ????45％ |
| Batching 3 | ????51％ |
| Batching 4 | ????48％ |
*The figure that degree of crystallinity is drawn by the dsc analysis data obtains.
Embodiment 2
To add by the PET bottle regenerated 80kgPET resin granular material (commercial product) that reclaims, 20kg polycarbonate resin (Teijin KK, Panlite K-1300) and 2.63kg titanium dioxide (Ishihara Sangyo KK.CR-97) and roll in the mixed machine and mix.Mediate with equipment similar to Example 1 and under condition similar to Example 1 subsequently, obtain coarse particles.Making particle degree of crystallinity surpass for 35% required heat-up time is 8 hours.The shredder running obtained median size 190 μ m (particle size range: powder 53-425 μ m) after 1 hour.These coarse particless were heated 17 hours down at 170 ℃, and degree of crystallinity increases to 41%, handles the post crystallization degree through 40 hours and increases to 45%.Obtain median size 180 μ m (particle size range: powder mass 53-425 μ m).
Embodiment 3
To add by the PET bottle regenerated 100kgPET resin granular material that reclaims, 5kg ethylene acrylic acid co polymer resin (Dow Chemical, Primacol 3460) and 2.63kg titanium dioxide (Ishihara SangyoKK.CR-97) and roll in the mixed machine and mix.Mediate and grind with equipment similar to Example 1 subsequently.Making particle degree of crystallinity surpass for 35% required heat-up time is 8.5 hours, and the continuation heating made degree of crystallinity increase to 39% in 17 hours.After the pellet that obtains ground 1 hour, obtain median size 200 μ m (particle size range: powder particle 53-425 μ m).
Embodiment 4
To add by the PET bottle regenerated 80kgPET resin granular material that reclaims, 20kg PEN (Teijin) and 2.63kg titanium dioxide (Ishihara Sangyo KK.CR-97) and roll in the mixed machine and mix.Mediate and grind with equipment similar to Example 1 subsequently.Making particle degree of crystallinity surpass for 35% required heat-up time is 6 hours, and the continuation heating makes degree of crystallinity increase to 52%.After the particle that obtains ground 1 hour, obtain median size 190 μ m (particle size range: powder 53-425 μ m).
Embodiment 5
To add by the PET bottle regenerated 80kgPET resin granular material that reclaims, 20kg polymaleic acid glycol ester (KK Nakada Coating) and 2.63kg titanium dioxide (Ishihara Sangyo KK.CR-97) and roll in the mixed machine and mix.Mediate and grind with equipment similar to Example 1 subsequently.Through obtain degree of crystallinity about 36% and median size 210 μ m (particle size range: powder 75-425 μ m) after 10 hours 170 ℃ of following heat treated.
After mechanical mill in 1 hour, obtain the powder particle size of corresponding embodiment, obviously, prolong milling time and will increase the more ratio of small diameter particles.Therefore, in actual production, milling time should be fit to practical use, and predetermined granulometric range is carried out classification.
Embodiment 6
The mixture (PET resin, PBT resin and titanium dioxide) of preparation among the 2kg embodiment 1 is added in the strap clamp cover stirring and dissolving jar that the 40l N,N-DIMETHYLACETAMIDE is housed, and with this mixture by being heated to 172 ℃ of dissolvings.Through be water-cooled to be lower than 60 ℃ after, isolate particle, filter isolating solvent by pressure filter then, filter cake is added in the vacuum drier that band stirs, dry under 12rpm, 70 ℃ and 10Torr vacuum tightness, obtain powder.Yield is 95wt%.Subsequently, the processing speed of this powder with 1kg/h added among the Jet Mill (KK Seishin Kigyo FS-4),, obtain median size 45 μ m (particle size range: fine powder 10-128 μ m) to pulverize agglomerant particle.Particle size survey meter (KK Seishin Kigyo LMS-30) by laser diffraction dispersion system with 0.1% lauryl sodium sulfate aqueous solution as dispersion medium, and by ultra-sonic dispersion effect mensuration distribution of particle sizes.
Embodiment 7
The mixture of preparation among the 2kg embodiment 2 is added in the strap clamp cover stirring and dissolving jar that 40 l methylacetamides are housed, and with this mixture by being heated to 172 ℃ of dissolvings.Through be water-cooled to be lower than 60 ℃ after, isolate particle, filter isolating solvent by pressure filter then, filter cake is added in the vacuum drier that band stirs, dry under 12rpm, 70 ℃ and 10Torr vacuum tightness, obtain powder.Yield is 95wt%.Subsequently, the processing speed of this powder with 1kg/h added among the Jet Mill (KK SeishinKigyo FS-4),, obtain median size 40 μ m (particle size range: fine powder 10-128 μ m) to pulverize agglomerated particle.Measure distribution of particle sizes by the method identical with embodiment 1.
Be coated with film test
With the powder of embodiment 1-5 preparation through the sub-classification of 300 mesh sieves, and corresponding fraction added in the fluidization dipping jar, (50 * 100 * 1.5mm) dipping 3 seconds are to form thick the filming of about 400 μ m thereon will to be heated to the SS steel plate of 300 ℃ of surface temperatures in this jar.The steel plate of this coating is used as the sample that is coated with film test.
In addition, with the fine powder of preparation in embodiment 6 and 7 with electrostatic applications machine (Niho parkarizingKK) apply under voltage-50KV with top similar steel plate under sprayed 4 seconds, then these steel plates are put into the electric oven 2 minutes that is heated to 350 ℃, formed thick the filming of about 50 μ m.
With these samples according to JIS K 5400 usefulness grid bond test method (tape stripping methods, 2 * 2mm grid, 25 grids) and duPont impact tester (Toyo Seiki KK, 1m height, heavy 300g, front-end radius 7mm) carry out shock test and measure pencil shape hardness.These are measured under 23 ± 2 ℃ of room temperatures and carry out.
The result provides in following table.
Table 3
The test-results of filming: (making its cooling)
| Bounding force (X/25) X: sample adherent number of squares | Shock-resistance | Pencil hardness | |
| Embodiment 1 prescription 1 | ????4/25 | Crackle occurs and peel off | ????2H |
| Embodiment 1 prescription 2 | ????25/25 | Some crackles appear | ????2H |
| Embodiment 1 prescription 3 | ????25/25 | Some crackles appear | ????2H |
| Embodiment 1 prescription 4 | ????25/25 | Some crackles appear | ????2H |
| Embodiment 2 | ????25/25 | Some crackles appear | ????4H |
| Embodiment 3 | ????25/25 | Some crackles appear | ????4H |
| Embodiment 4 | ????25/25 | Some crackles appear | ????4H |
| Embodiment 5 | ????25/25 | Flawless | ????4H |
| Embodiment 6 | ????25/25 | Some crackles appear | ????2H |
| Embodiment 7 | ????25/25 | Some crackles appear | ????2H |
*In 25 grids of the numeric representation of bounding force behind the tape stripping sample keep adherent number of squares,
*After " making its cooling " and be meant the coating baking, it is cooled to room temperature.
Table 4
| Bounding force (X/25) X: sample adherent number of squares | Shock-resistance | Pencil hardness | |
| Embodiment 1 prescription 1 | ????25/25 | Some crackles appear | ????B |
| Embodiment 1 prescription 2 | ????25/25 | Flawless | ????B |
| Embodiment 1 prescription 3 | ????25/25 | Flawless | ????HB |
| Embodiment 1 prescription 4 | ????25/25 | Flawless | ????HB |
| Embodiment 2 | ????25/25 | Flawless | ????H |
| Embodiment 3 | ????25/25 | Flawless | ????F |
| Embodiment 4 | ????25/25 | Flawless | ????HB |
| Embodiment 5 | ????25/25 | Flawless | ????4H |
| Embodiment 6 | ????25/25 | Flawless | ????B |
| Embodiment 7 | ????25/25 | Flawless | ????H |
" water cooling " is meant that baked paint after 30 seconds, puts into water with coated sample and cool off.
The result of dielectric breakdown test:
According to JIS-C-2100 the powder coated sample of embodiment 1, prescription 4 is tested.
Table 5
| Coating thickness (m) | The speed (KV/sec) that voltage increases | Voltage breakdown (KV) |
| ????370-390 | ????1 | ????13 |
*Condition: 26.5 ℃ of oil temperature, AC 50Hz.
Top its insulating property of data declaration are almost the twice of the commercial PET coated film product of same thin film thickness.
The present invention makes with the low PET resin of metlbond power has performance with metal adhesion, thereby makes this resin can be used as powder coating.Simultaneously, the present invention optionally improves coating characteristic, as shock resistance, hardness, resistance to boiling water and electrical insulating property by the properties-correcting agent material of variation with PET resin melt blending.Therefore expect of the present invention of many uses.In addition, because except that the PET resin, the PET product of recovery can be used as raw material.Therefore help to reclaim and re-use the PET product.
Obviously, according to top description, can carry out a lot of changes and improvements to the present invention.Therefore, in appended claim scope, the present invention can implement by being different from specifically described mode here.
Claims (12)
1. powder paint compositions, comprise 100 weight part pet resin pellets or the small pieces and the melt blended material of 5-40 weight part vibrin (except that polyethylene terephthalate) or modified polyester resin that obtain by the polyethylene terephthalate layered product that reclaims, the adhesive power of the improved and metallic surface of this powdered material demonstration.
2. powder paint compositions, comprise 100 weight part pet resin pellets or the small pieces and the melt blended material of 3-30 weight part modified polyolefin resin or ethylene acrylic acid co polymer resin that are obtained by the polyethylene terephthalate layered product that reclaims, this powdered material shows the adhesive power of improved and metallic surface.
3. powder paint compositions, comprise 100 weight part pet resin pellets or the small pieces and the melt blended material of 3-30 weight part polycarbonate resin that are obtained by the polyethylene terephthalate layered product that reclaims, this powdered material shows the adhesive power of improved and metallic surface.
4. method for preparing powder coating comprises:
The product of claim 1 is converted into Coarse Aggregate;
Heating this pellet makes its degree of crystallinity increase to 35% or bigger; With
At normal temperatures with this pellet mechanical mill to the particle that is lower than 350 μ m.
5. method for preparing powder coating comprises:
The product of claim 2 is converted into Coarse Aggregate;
Heating this pellet makes its degree of crystallinity increase to 35% or bigger; With
At normal temperatures with this pellet mechanical mill to the particle that is lower than 350 μ m.
6. method for preparing powder coating comprises:
The product of claim 3 is converted into Coarse Aggregate;
Heating this pellet makes its degree of crystallinity increase to 35% or bigger; With
At normal temperatures with this pellet mechanical mill to the particle that is lower than 350 μ m.
7. the method for claim 4 wherein is heated to pellet 170 ℃ to reach described 35% degree of crystallinity.
8. the method for claim 5 wherein is heated to pellet 170 ℃ to reach described 35% degree of crystallinity.
9. the method for claim 6 wherein is heated to pellet 170 ℃ to reach described 35% degree of crystallinity.
10. the method for a fine grainding powder coating comprises:
The coarse particles that will be obtained by the molten mixture of claim 1 carries out chemical grinding in dimethylacetamide solvent.
11. the method for a fine grainding powder coating comprises:
The coarse particles that will be obtained by the molten mixture of claim 2 carries out chemical grinding in dimethylacetamide solvent.
12. the method for a fine grainding powder coating comprises:
The coarse particles that will be obtained by the molten mixture of claim 3 carries out chemical grinding in dimethylacetamide solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98120949 CN1205290C (en) | 1998-10-13 | 1998-10-13 | Powder paint contg. polyethylene glycol terephthalate, and method for preparing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98120949 CN1205290C (en) | 1998-10-13 | 1998-10-13 | Powder paint contg. polyethylene glycol terephthalate, and method for preparing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1250795A true CN1250795A (en) | 2000-04-19 |
| CN1205290C CN1205290C (en) | 2005-06-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98120949 Expired - Fee Related CN1205290C (en) | 1998-10-13 | 1998-10-13 | Powder paint contg. polyethylene glycol terephthalate, and method for preparing same |
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| CN (1) | CN1205290C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100381521C (en) * | 2002-08-30 | 2008-04-16 | Ppg工业俄亥俄公司 | Compositions and methods for coating food cans |
| CN103333593A (en) * | 2013-05-30 | 2013-10-02 | 蚌埠市鸿安精密机械有限公司 | Oil-resistance bisphenol A type polycarbonate powder coating and preparation method thereof |
| CN107043453A (en) * | 2017-03-24 | 2017-08-15 | 九江市杰克西涂料有限公司 | Saturated polyester resin and preparation method, the tangerine line powdery paints containing it and preparation method |
| CN115926591A (en) * | 2023-03-09 | 2023-04-07 | 广东清森美新材料科技有限公司 | Formaldehyde-removing antibacterial powder coating and preparation method and application thereof |
-
1998
- 1998-10-13 CN CN 98120949 patent/CN1205290C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100381521C (en) * | 2002-08-30 | 2008-04-16 | Ppg工业俄亥俄公司 | Compositions and methods for coating food cans |
| CN103333593A (en) * | 2013-05-30 | 2013-10-02 | 蚌埠市鸿安精密机械有限公司 | Oil-resistance bisphenol A type polycarbonate powder coating and preparation method thereof |
| CN103333593B (en) * | 2013-05-30 | 2016-06-15 | 蚌埠市鸿安精密机械有限公司 | The powder coating of a kind of oil-proofness bisphenol A polycarbonate and its preparation method |
| CN107043453A (en) * | 2017-03-24 | 2017-08-15 | 九江市杰克西涂料有限公司 | Saturated polyester resin and preparation method, the tangerine line powdery paints containing it and preparation method |
| CN115926591A (en) * | 2023-03-09 | 2023-04-07 | 广东清森美新材料科技有限公司 | Formaldehyde-removing antibacterial powder coating and preparation method and application thereof |
| CN115926591B (en) * | 2023-03-09 | 2023-05-16 | 广东清森美新材料科技有限公司 | Formaldehyde-removing antibacterial powder coating and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN1205290C (en) | 2005-06-08 |
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