CN104893517A - Powder coating containing filling material of calcium carbonate - Google Patents
Powder coating containing filling material of calcium carbonate Download PDFInfo
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- CN104893517A CN104893517A CN201510256690.1A CN201510256690A CN104893517A CN 104893517 A CN104893517 A CN 104893517A CN 201510256690 A CN201510256690 A CN 201510256690A CN 104893517 A CN104893517 A CN 104893517A
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Abstract
The invention discloses a powder coating containing a filling material of calcium carbonate, and belongs to the field of coating, particularly to the field of powder coating. The powder coating containing the filling material of calcium carbonate comprises a film-forming matter, the filling material, and a coupling agent. The film-forming matter comprises a main resin and a cured resin, wherein the main resin is compounded from terephthalic anhydride, pentanediol, diglycol, maleic anhydride, 1,2-dimethoxybenzene, hydroquinone, and paraphthaloyl chloride; and the cured resin is a mixture of one or two of styrene and methylmethacrylate and ethanolamine. Mechanical properties of the coating are effectively improved by adding the coupling agent and calcium carbonate into the film-forming matter composed of the main resin and the cured resin. The powder coating not only can be cured at a low temperature, but also has excellent mechanical properties.
Description
Technical field
The invention belongs to paint field, belong to the field of the powder coating of low-temperature curing especially.
Background technology
Powder coating is the coating type not containing solvent in a kind of component, and it does not in use produce volatile organic compound (VOC) substantially, minimum to the pollution of environment, is a kind of coating of energy-conserving and environment-protective.Powder coating generally comprises thermoplastic powder coating and thermosetting powder coating(s), if as the thermoplastic resin of the resin of filmogen, then it is thermoplastic powder coating in coating, if resin is heat cured resin, it is thermosetting powder coating(s), resin in heat cured powder coating is once after solidification, coating at high temperature there will not be melting, also dissolving is there will not be under different solvent environment, therefore relative to thermoplastic powder coating, there is better physics, chemical property, based on this, thermosetting powder coating(s) has captured rapidly the main positions in powder coating.
Common thermosetting powder coating(s) is according to the type of wherein resin, mainly comprise the powder coating of epoxies powder coating, polyester powder coating, acrylic powder coating, epoxy/polyester mixed powder coating, radiation-curable powder coating and other type, except resin, general also containing solidifying agent, pigment and/or auxiliary agent and/or filler etc. in thermosetting powder coating(s), the application mode of thermosetting powder coating(s) comprises hot application and cold application, especially based on the electrostatic spraying in cold application mode.
Although thermosetting powder coating(s) has energy-conservation, environmental protection, the advantages such as the thermotolerance of film, solvent resistance are better, but for solvent based coating, its solidification value higher (180 DEG C ~ 200 DEG C) needed, be unfavorable for widespread use on a different material, in mechanical property, also compare shortcoming simultaneously.
Summary of the invention
The object of the invention is to propose one can solidify at a lower temperature, the polyester powder coating of the modification of satisfactory mechanical property simultaneously.The present invention realizes above-mentioned purpose by following technical scheme:
Containing a powder coating for filler-calcium carbonate, comprise filmogen, filler and coupling agent, described filmogen comprises matrix resin and cured resin, and described matrix resin is by the resins synthesis of the following raw material as matrix resin:
Terephthalic anhydride, pentanediol, glycol ether, MALEIC ANHYDRIDE, 1,2-dimethoxy benzene, Resorcinol, p-phthaloyl chloride (TPC);
Described cured resin is the mixture of one or both and thanomin in vinylbenzene or methylbenzene e pioic acid methyl ester;
Described filler is calcium carbonate;
Described coupling agent is Borate Ester as Coupling;
The quality that described calcium carbonate adds is 5% ~ 15% of the quality of described filmogen;
The consumption of described boric acid ester coupler is 0.5% ~ 2% of the quality of described filmogen.
It is preferred embodiment: in the raw material of matrix resin, the ratio of the amount of substance of pentanediol, glycol ether is 1:2 ~ 2:1.
Its another be preferred embodiment: in the raw material of matrix resin, terephthalic anhydride is 1:1 ~ 2:1 with the ratio of the amount of substance of MALEIC ANHYDRIDE.
Its another be preferred embodiment: in the raw material of matrix resin, the ratio of the amount of substance of 1,2-dimethoxy benzene, Resorcinol is 2 ~ 3:4 ~ 5.
Its another be preferred embodiment: in the raw material of matrix resin, total amount of substance of pentanediol, glycol ether is 2:5 ~ 2:7 with the ratio of total amount of substance of terephthalic anhydride, MALEIC ANHYDRIDE.
Its another be preferred embodiment: in the raw material of matrix resin terephthalic anhydride, MALEIC ANHYDRIDE total amount of substance be 10:1 ~ 15:1 with the ratio of the amount of substance of TPC.
Its another be preferred embodiment: in the raw material of matrix resin, total amount of substance of terephthalic anhydride, MALEIC ANHYDRIDE is 3:1 ~ 4:1 with the ratio of total amount of substance of 1,2-dimethoxy benzene, Resorcinol.
Its another be preferred embodiment: one or both the amount of substance in described cured resin in vinylbenzene or methylbenzene e pioic acid methyl ester is 7:1 ~ 9:1 with the ratio of the amount of substance of thanomin.
Its another be preferred embodiment: the quality of described cured resin is 30% ~ 50% of matrix resin quality.
Its another be preferred embodiment: described filler-calcium carbonate is light calcium carbonate, and its median size is 2 ~ 3 μm.
Strengthen levelling effect if wish, should can also add other auxiliary agent containing in the powder coating of filler-calcium carbonate, as polymethylmethacrylate, its consumption is preferably 0.5% ~ 1.5% of described powder coating total mass.
Described auxiliary agent can also comprise in boron trifluoride ethyl ether complex, tin protochloride, stannous octoate one or more, its consumption is 1% ~ 2% of described filmogen total mass.
The synthetic method of the matrix resin in the filmogen of the described powder coating containing filler-calcium carbonate comprises the following steps:
1) terephthalic anhydride, MALEIC ANHYDRIDE, TPC are added in four-hole boiling flask, under nitrogen atmosphere, be heated to 150 ~ 190 DEG C, and constant temperature return stirring 20 ~ 40min;
2) to completing steps 1) four-hole boiling flask in add pentanediol, glycol ether, 190 ~ 210 DEG C are warming up under nitrogen atmosphere, and constant temperature return stirring 1 ~ 2h, thereafter four-hole boiling flask is vacuumized, maintaining pot temperature is 190 ~ 210 DEG C, continues constant temperature return stirring 3 ~ 4h;
3) to completing steps 2) four-hole boiling flask in add 1,2-dimethoxy benzene and Resorcinol, in nitrogen atmosphere borehole cooling to 170 ~ 180 DEG C, and constant temperature return stirring 20 ~ 40min.
The synthetic method of the filmogen of the described powder coating containing filler-calcium carbonate comprises the following steps:
1) terephthalic anhydride, MALEIC ANHYDRIDE, TPC are added in four-hole boiling flask, under nitrogen atmosphere, be heated to 150 ~ 190 DEG C, and constant temperature return stirring 20 ~ 40min;
2) to completing steps 1) four-hole boiling flask in add pentanediol, glycol ether, 190 ~ 210 DEG C are warming up under nitrogen atmosphere, and constant temperature return stirring 1 ~ 2h, thereafter four-hole boiling flask is vacuumized, maintaining pot temperature is 190 ~ 210 DEG C, continues constant temperature return stirring 3 ~ 4h;
3) to completing steps 2) four-hole boiling flask in add 1,2-dimethoxy benzene and Resorcinol, in nitrogen atmosphere borehole cooling to 170 ~ 180 DEG C, and constant temperature return stirring 20 ~ 40min;
4) by completing steps 3) four-hole boiling flask stop heating, drop to after below 140 DEG C to temperature, under nitrogen atmosphere, add described cured resin wherein.
After completing the preparation of filmogen, further, successively coupling agent, filler-calcium carbonate are added wherein at 70 ~ 90 DEG C, be cooled to after stirring normal temperature or further freezing, pulverize and can obtain the described powder coating containing filler-calcium carbonate.
In addition to the above components, if wish, this coating is also with color, can also add color stuffing in coating.
The present invention has following beneficial effect:
1) matrix resin of the powder coating containing filler-calcium carbonate of the present invention is by selecting suitable raw material, the matrix resin that it is synthesized can on the one hand because regularity better obtains higher second-order transition temperature, avoid the coating clayization at low temperatures obtained further, can, by crosslinking temperature lower between matrix resin and cured resin, make it can be solidified the powder coating of use at a lower temperature on the other hand;
2) filler is added of the present invention containing in the powder coating of filler-calcium carbonate, the mechanical property of the film obtained after being conducive to improving application;
3) preparation method of the powder coating containing filler-calcium carbonate of the present invention is simple, easy to prepare;
4) powder coating containing filler-calcium carbonate of the present invention in use can not produce volatile solvent, environmental protection.
Embodiment
1) terephthalic anhydride, MALEIC ANHYDRIDE, TPC are added in four-hole boiling flask, under nitrogen atmosphere, be heated to 150 ~ 190 DEG C, and constant temperature return stirring 20 ~ 40min;
2) to completing steps 1) four-hole boiling flask in add pentanediol, glycol ether, 190 ~ 210 DEG C are warming up under nitrogen atmosphere, and constant temperature return stirring 1 ~ 2h, thereafter four-hole boiling flask is vacuumized, maintaining pot temperature is 190 ~ 210 DEG C, continues constant temperature return stirring 3 ~ 4h;
3) to completing steps 2) four-hole boiling flask in add 1,2-dimethoxy benzene and Resorcinol, in nitrogen atmosphere borehole cooling to 170 ~ 180 DEG C, and constant temperature return stirring 20 ~ 40min, namely obtain matrix resin;
4) by completing steps 3) four-hole boiling flask stop heating, drop to after below 140 DEG C to temperature, under nitrogen atmosphere, add described cured resin wherein;
After completing above-mentioned preparation process, successively coupling agent, filler-calcium carbonate are added wherein at 70 ~ 90 DEG C, be cooled to after stirring normal temperature or further freezing, pulverize the powder coating that can obtain containing filler-calcium carbonate.
The analytical pure articles for use of the raw material used in said process in the present invention for buying, when practical application, can buy the industrial goods that purity is higher, also can prepare the few various raw materials of foreign matter content voluntarily.In reaction process, four-hole boiling flask need connect nitrogen gas conveying device, temperature measuring equipment, whipping appts and reflux condensate device, the seal degree of the strict hierarchy of control in reaction process, because some compositions in raw material are easily oxidized when reacting incomplete.Its second-order transition temperature of powder coating containing filler-calcium carbonate prepared is 30 ~ 50 DEG C, and acid number is 30 ~ 40mgKOH/g, and at 100 ~ 120 DEG C, heat 10 ~ 20min can solidify completely.
Below in conjunction with embodiment, the present invention is further detailed:
Embodiment one
225g terephthalic anhydride, 150g MALEIC ANHYDRIDE, 61gTPC are added in four-hole boiling flask, under nitrogen atmosphere, is heated to 180 DEG C, and return stirring 20min at a constant temperature; Add 32g pentanediol, 64g glycol ether in its backward four-hole boiling flask, under nitrogen atmosphere, be warming up to 190 DEG C, and constant temperature return stirring 1h, thereafter four-hole boiling flask is vacuumized, continue constant temperature return stirring 3h at 190 DEG C; Thereafter in flask, be filled with nitrogen again, add 41g 1,2-dimethoxy benzene with to 66g Resorcinol, in nitrogen atmosphere borehole cooling to 170 DEG C, and constant temperature return stirring 20min; Thereafter stop heating, when temperature drops to 130 DEG C, under nitrogen atmosphere, add 293g vinylbenzene and 27g thanomin wherein, after stirring, namely complete the preparation of filmogen.
Embodiment two
440g terephthalic anhydride, 150g MALEIC ANHYDRIDE, 91gTPC are added in four-hole boiling flask, under nitrogen atmosphere, is heated to 190 DEG C, and constant temperature return stirring 40min; Add 94g pentanediol, 95g glycol ether in its backward four-hole boiling flask, under nitrogen atmosphere, be warming up to 210 DEG C, and constant temperature return stirring 1h, thereafter four-hole boiling flask is vacuumized, continue constant temperature return stirring 2h at 210 DEG C; Thereafter in flask, be filled with nitrogen again, and add 41g 1,2-dimethoxy benzene with to 88g Resorcinol, in nitrogen atmosphere borehole cooling to 180 DEG C, and constant temperature return stirring 30min; Thereafter stop heating, when temperature drops to 135 DEG C, under nitrogen atmosphere, add 458g methylbenzene e pioic acid methyl ester and 42g thanomin wherein, after stirring, namely complete the preparation of filmogen.
Embodiment three
440g terephthalic anhydride, 150g MALEIC ANHYDRIDE, 61gTPC are added in four-hole boiling flask, under nitrogen atmosphere, is heated to 190 DEG C, and constant temperature return stirring 40min; Add 94g pentanediol, 95g glycol ether in its backward four-hole boiling flask, under nitrogen atmosphere, be warming up to 210 DEG C, and constant temperature return stirring 1h, thereafter four-hole boiling flask is vacuumized, continue constant temperature return stirring 2h at 210 DEG C; Thereafter in flask, be filled with nitrogen again, and add 41g 1,2-dimethoxy benzene with to 88g Resorcinol, in nitrogen atmosphere borehole cooling to 180 DEG C, and constant temperature return stirring 30min; Thereafter stop heating, when temperature drops to 135 DEG C, under nitrogen atmosphere, add 454g methylbenzene e pioic acid methyl ester and 30g thanomin wherein, after stirring, namely complete the preparation of filmogen.
Embodiment four
300g terephthalic anhydride, 150g MALEIC ANHYDRIDE, 55gTPC are added in four-hole boiling flask, under nitrogen atmosphere, is heated to 190 DEG C, and constant temperature return stirring 30min; Add 36g pentanediol, 37g glycol ether in its backward four-hole boiling flask, under nitrogen atmosphere, be warming up to 200 DEG C, and constant temperature return stirring 2h, thereafter four-hole boiling flask is vacuumized, continue constant temperature return stirring 4h at 200 DEG C; Thereafter in flask, be filled with nitrogen again, and add 44g 1,2-dimethoxy benzene with to 53g Resorcinol, in nitrogen atmosphere borehole cooling to 180 DEG C, and constant temperature return stirring 30min; Thereafter stop heating, temperature drops to after below 140 DEG C, adds 250g vinylbenzene and 21g thanomin wherein, namely complete the preparation of filmogen after stirring under nitrogen atmosphere.
Embodiment five
Get the filmogen 500g prepared according to the process of embodiment one, boric acid ester coupler 2.5g is added at 70 DEG C, coupling agent used is the SBW-III coupling agent of the four-dimensional Chemical Manufacture in Qingdao, after stirring, add filler-calcium carbonate 25g, this calcium carbonate is light calcium carbonate filler, median size is 2 ~ 3 μm, 15min will be heated in mixture beaker to being fully formed solid at 120 DEG C after stirring 5min, take out fraction solids and weigh, thereafter N is used, dinethylformamide (DMF) soaks 6h, and again weigh after washing drying, find that considerable change does not appear in solid masses, explanation paint solidification is complete, use DSC to record its Tg after described mixture being frozen into solid is 39 DEG C simultaneously.
Embodiment six
Get the filmogen 500g prepared according to the process of embodiment one, the coupling agent boric acid trimethyl carbinol-diethanolamine ester (tert-BE4) 5g is added at 80 DEG C, after stirring, add filler-calcium carbonate 50g, this calcium carbonate is light calcium carbonate filler, median size is 2 ~ 3 μm, a part in mixture is put in beaker after stirring and at 120 DEG C, heats 20min to being fully formed solid, take out fraction solids and weigh, thereafter N is used, dinethylformamide (DMF) soaks 6h, and again weigh after washing drying, find that considerable change does not appear in solid masses, explanation paint solidification is complete, remaining mixture is carried out freezing and pulverizing, recording its Tg by DSC is 40 DEG C, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, 20min solidification is heated at 120 DEG C, the painting film close formed, surface is aobvious coarse, without obvious bubble, pin hole, its shock resistance >=50kg.cm is recorded according to the testing method of GB/T1732, its pencil hardness >=2H level is recorded according to the testing method of GB/T6739.
Embodiment seven
Get the filmogen 500g prepared according to the process of embodiment one, coupling agent SBW-III10g is added at 90 DEG C, after stirring, add filler-calcium carbonate 30g, this calcium carbonate is light calcium carbonate filler, median size is 2 ~ 3 μm, auxiliary agent polymethylmethacrylate (trade names 701) 2.5g is added after stirring, thereafter auxiliary agent boron trifluoride ethyl ether complex is added, add-on is 5g, to stir after 1min mixture is freezing and pulverize, recording its Tg by DSC is 37 DEG C, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, 10min solidification is heated at 120 DEG C, the painting film close formed is smooth, without obvious bubble, pin hole, its shock resistance >=50kg.cm is recorded according to the testing method of GB/T1732, its pencil hardness >=2H level is recorded according to the testing method of GB/T6739.
Embodiment eight
Get the filmogen 500g prepared according to the process of embodiment two, coupling agent SBW-III5g is added at 80 DEG C, after stirring, add filler-calcium carbonate 40g, this calcium carbonate is light calcium carbonate filler, median size is 2 ~ 3 μm, thereafter auxiliary agent polymethylmethacrylate (trade names 701) 7g is added, auxiliary agent boron trifluoride ethyl ether complex 10g is added after stirring, to stir after 1min mixture is freezing and pulverize, recording its Tg by DSC is 38 DEG C, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, 20min solidification is heated at 100 DEG C, the painting film close formed is smooth, without obvious bubble, pin hole, its shock resistance >=50kg.cm is recorded according to the testing method of GB/T1732, its pencil hardness >=2H level is recorded according to the testing method of GB/T6739.
Embodiment nine
Get the filmogen 500g prepared according to embodiment one, coupling agent SBW-III8g is added at 70 DEG C, after stirring, add filler silica powder 50g, this silica powder is chemical grade 600 order silica powder, auxiliary agent polymethylmethacrylate (trade names 701) is added after stirring, add-on is 6g, thereafter photocatalyst DMPA5g is added, to stir after 2min mixture is freezing and pulverize, recording its Tg by DSC is 41 DEG C, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, it is 28min solidification under the UV-light of 1.0mW/cm2 in intensity, scrape partially cured after film weigh after be soaked in 6h in DMF, thereafter washed, drying is weighed again, find that quality is without considerable change, explanation paint solidification is complete.
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only the present invention's preferably embodiment, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (10)
1. the powder coating containing filler-calcium carbonate, described powder coating comprises filmogen, filler and coupling agent, described filmogen comprises matrix resin and cured resin, it is characterized in that: described matrix resin is by the resins synthesis of the following raw material as matrix resin:
Terephthalic anhydride, pentanediol, glycol ether, MALEIC ANHYDRIDE, 1,2-dimethoxy benzene, Resorcinol, p-phthaloyl chloride (TPC);
Described cured resin is the mixture of one or both and thanomin in vinylbenzene or methylbenzene e pioic acid methyl ester;
Described filler is calcium carbonate;
Described coupling agent is boric acid ester coupler;
The quality that described calcium carbonate adds is 5% ~ 15% of the quality of described filmogen;
The consumption of described boric acid ester coupler is 0.5% ~ 2% of the quality of described filmogen.
2. the powder coating containing filler-calcium carbonate according to claim 1, is characterized in that: in the raw material of described matrix resin, the ratio of the amount of substance of pentanediol, glycol ether is 1:2 ~ 2:1.
3. the powder coating containing filler-calcium carbonate according to claim 1, is characterized in that: in the raw material of described matrix resin, terephthalic anhydride is 1:1 ~ 2:1 with the ratio of the amount of substance of MALEIC ANHYDRIDE.
4. the powder coating containing filler-calcium carbonate according to claim 1, is characterized in that: in the raw material of described matrix resin, the ratio of the amount of substance of 1,2-dimethoxy benzene, Resorcinol is 2 ~ 3:4 ~ 5.
5. the powder coating containing filler-calcium carbonate according to claim 1, is characterized in that: in the raw material of described matrix resin, total amount of substance of pentanediol, glycol ether is 2:5 ~ 2:7 with the ratio of total amount of substance of terephthalic anhydride, MALEIC ANHYDRIDE.
6. the powder coating containing filler-calcium carbonate according to claim 1, is characterized in that: in the raw material of described matrix resin terephthalic anhydride, MALEIC ANHYDRIDE total amount of substance be 10:1 ~ 15:1 with the ratio of the amount of substance of TPC.
7. the powder coating containing filler-calcium carbonate according to claim 1, is characterized in that: in the raw material of described matrix resin, total amount of substance of terephthalic anhydride, MALEIC ANHYDRIDE is 3:1 ~ 4:1 with the ratio of total amount of substance of 1,2-dimethoxy benzene, Resorcinol.
8. the powder coating containing filler-calcium carbonate according to claim 1, is characterized in that: one or both the amount of substance in described cured resin in vinylbenzene or methylbenzene e pioic acid methyl ester is 7:1 ~ 9:1 with the ratio of the amount of substance of thanomin.
9. the powder coating containing filler-calcium carbonate according to claim 1, is characterized in that: the quality of described cured resin is 30% ~ 50% of matrix resin quality.
10. the powder coating containing filler-calcium carbonate according to claim 1, it is characterized in that: described filler-calcium carbonate is light calcium carbonate, its median size is 2 ~ 3 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510256690.1A CN104893517A (en) | 2015-05-19 | 2015-05-19 | Powder coating containing filling material of calcium carbonate |
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| CN201510256690.1A CN104893517A (en) | 2015-05-19 | 2015-05-19 | Powder coating containing filling material of calcium carbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762632A (en) * | 2019-01-15 | 2019-05-17 | 广西碳酸钙产业化工程院有限公司 | Calcium carbonate high-performance complex calcium sulfonate grease and preparation method thereof |
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| EP1055694A2 (en) * | 1999-05-28 | 2000-11-29 | Nippon Paint Co., Ltd. | Thermosetting powder coating composition and curing agent composition |
| CN101289592A (en) * | 2008-06-11 | 2008-10-22 | 上海彩奇亮粉末涂料有限公司 | Epoxy resins and polyester mixed powder paint at ultralow temperature |
| CN101880490A (en) * | 2010-07-07 | 2010-11-10 | 宁波南海化学有限公司 | De-lustering curing agent, de-lustering curing agent-containing powder paint and use thereof |
| CN103613745A (en) * | 2013-11-26 | 2014-03-05 | 天津翔盛粉末涂料有限公司 | Phase-transfer catalytic function type energy-saving polyester resin, and synthesis method and application thereof |
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2015
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1055694A2 (en) * | 1999-05-28 | 2000-11-29 | Nippon Paint Co., Ltd. | Thermosetting powder coating composition and curing agent composition |
| CN101289592A (en) * | 2008-06-11 | 2008-10-22 | 上海彩奇亮粉末涂料有限公司 | Epoxy resins and polyester mixed powder paint at ultralow temperature |
| CN101880490A (en) * | 2010-07-07 | 2010-11-10 | 宁波南海化学有限公司 | De-lustering curing agent, de-lustering curing agent-containing powder paint and use thereof |
| CN103613745A (en) * | 2013-11-26 | 2014-03-05 | 天津翔盛粉末涂料有限公司 | Phase-transfer catalytic function type energy-saving polyester resin, and synthesis method and application thereof |
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| CN109762632A (en) * | 2019-01-15 | 2019-05-17 | 广西碳酸钙产业化工程院有限公司 | Calcium carbonate high-performance complex calcium sulfonate grease and preparation method thereof |
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Application publication date: 20150909 |