CN104910768A - Preparation method of film-forming material for low-temperature-curing powder paint - Google Patents
Preparation method of film-forming material for low-temperature-curing powder paint Download PDFInfo
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- CN104910768A CN104910768A CN201510257361.9A CN201510257361A CN104910768A CN 104910768 A CN104910768 A CN 104910768A CN 201510257361 A CN201510257361 A CN 201510257361A CN 104910768 A CN104910768 A CN 104910768A
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Abstract
The invention discloses a preparation method of a film-forming material of a low-temperature-curing powder paint. The invention relates to the field of paints, and especially relates to the field of powder paints. The film-forming material of the low-temperature-curing powder paint comprises main resin and curing resin. The main resin is obtained by synthesizing phthalic anhydride, pentanediol, diethylene glycol, maleic anhydride, veratrole, hydroquinone and terephthaloyl chloride. The curing resin is a mixture of ethanolamine and one or two selected from styrene or methyl methacrylate. The main resin and the curing resin are mixed, such that the film-forming material is obtained. Further, a photocatalyst, a filling material and additives are added into the film-forming material, such that the low-temperature-curing powder paint is obtained. The low-temperature-curing powder paint can be cured under a low temperature or under ultraviolet irradiation. The preparation method is convenient, and the curing temperature is low. The paint is green and environment-friendly.
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, for solvent based coating, its solidification value higher (180 DEG C ~ 200 DEG C) needed, is unfavorable for widespread use on a different material.
Summary of the invention
The object of the invention is to propose one can photocuring or directly solidify at a lower temperature, the preparation method of the filmogen of the polyester powder coating of the modification that use properties is good simultaneously, described filmogen forms the polyester powder coating of modification jointly with filler, auxiliary agent, photocatalyst etc. again.The present invention realizes above-mentioned purpose by following technical scheme:
A filmogen for the powder coating of low-temperature curing, it comprises matrix resin and cured resin, and this filmogen and photocatalyst, filler, auxiliary agent etc. together form a kind of powder coating of low-temperature curing, and described filmogen is prepared by following steps:
1) terephthalic anhydride, MALEIC ANHYDRIDE, p-phthaloyl chloride (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 cured resin wherein;
Described cured resin is the mixture of one or both and thanomin in vinylbenzene or methylbenzene e pioic acid methyl ester;
Completing steps 3) after namely prepare matrix resin in described filmogen, it is further advanced by step 4) and cured resin is mixed to get described filmogen.
Described pentanediol is preferably 1:2 ~ 2:1 with the ratio of the amount of substance of described glycol ether.
Described terephthalic anhydride is preferably 1:1 ~ 2:1 with the ratio of the amount of substance of described MALEIC ANHYDRIDE.
Described 1,2-dimethoxy benzene is preferably 2 ~ 3:4 ~ 5 with the ratio of the amount of substance of described Resorcinol.
Total amount of substance of described pentanediol, glycol ether is preferably 2:5 ~ 2:7 with the ratio of total amount of substance of described terephthalic anhydride, MALEIC ANHYDRIDE.
Total amount of substance of described terephthalic anhydride, MALEIC ANHYDRIDE be preferably 10:1 ~ 15:1 with the ratio of the amount of substance of described TPC.
Total amount of substance of described terephthalic anhydride, MALEIC ANHYDRIDE is preferably 3:1 ~ 4:1 with the ratio of total amount of substance of described 1,2-dimethoxy benzene, Resorcinol.
The quality of described cured resin is 30% ~ 50% of described matrix resin quality.
One or both amount of substance in described cured resin in vinylbenzene or methylbenzene e pioic acid methyl ester is preferably 7:1 ~ 9:1 with the ratio of the amount of substance of thanomin.
The filmogen prepared can add photocatalyst, filler, auxiliary agent thus obtain the powder coating of low-temperature curing further.
The photocatalyst of the powder coating of this low-temperature curing is preferably benzoin dimethylether (DMPA) or 2-hydroxy-2-methyl phenyl-acetone (HMPP), when photocatalyst is DMPA, its consumption is 1% ~ 5% of the quality of filmogen, when photocatalyst is HMPP, its consumption is 5% ~ 10% of the amount of filmogen.
The photocatalyst of the powder coating of this low-temperature curing can also be the semiconductor material of nanometer, and as nano titanium oxide, its consumption is 10% ~ 15% of filmogen.
The filler of the powder coating of this low-temperature curing be preferably in calcium carbonate, silica powder, barium sulfate, talcum powder, kaolin, mica powder, wollastonite one or more, its mass content is 5% ~ 15% of filmogen.
The auxiliary agent of the powder coating of this low-temperature curing preferably includes polymethylmethacrylate, and its consumption is 0.5% ~ 1.5% of described powder coating total mass.
The auxiliary agent of the powder coating of this low-temperature curing can also comprise in boron trifluoride ethyl ether complex, tin protochloride, stannous octoate one or more, its consumption is 1% ~ 2% of filmogen total mass.
The auxiliary agent of the powder coating of this low-temperature curing can also comprise coupling agent, and described coupling agent is boric acid ester coupler, and its consumption is 0.5% ~ 2% of filmogen total mass.
After completing the preparation of filmogen, further, at 70 ~ 90 DEG C, filler, photocatalyst, auxiliary agent are added wherein, be cooled to after stirring normal temperature or further freezing, pulverize and can obtain the powder coating of described low-temperature curing.
In addition to the above components, if wish coating also with color, color stuffing can also be added in coating.
The present invention has following beneficial effect:
1) raw material synthesizing matrix resin in the filmogen of the powder coating of low-temperature curing of the present invention is the good resin of regularity, the filmogen obtained thus has higher second-order transition temperature, avoid the coating clayization at low temperatures obtained further, in this filmogen, cured resin and matrix resin can be cross-linked at a lower temperature on the other hand, make it can be solidified the powder coating of use at a lower temperature;
2) the filmogen preparation method of the powder coating of low-temperature curing of the present invention is simple, can synthesize the powder coating be cured under photochemical catalysis further;
3) powder coating obtained by filmogen 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, be cooled to normal temperature after stirring and namely obtain filmogen.
After completing the preparation of filmogen, can at 70 ~ 90 DEG C, filler, photocatalyst, auxiliary agent be added wherein further, when containing coupling agent in auxiliary agent, addition sequence can according to first adding coupling agent, secondly add filler, add all the other auxiliary agents again, finally add the mode of photocatalyst and carry out, be cooled to after stirring normal temperature or further freezing, pulverize the powder coating that can obtain low-temperature curing.
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 the powder coating of the low-temperature curing prepared is 30 ~ 50 DEG C, acid number is 30 ~ 40mgKOH/g, if be added with photocatalyst in use, directly can be cured under ultraviolet light, not add photocatalyst and also can select to solidify 10 ~ 20min at 100 ~ 120 DEG C.
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, photocatalyst benzoin dimethylether (DMPA) 5g is added wherein at 70 DEG C, the filmogen adding photocatalyst to be poured into thickness be in the square dies of 2cm and be placed on high-precision electronic balance, be that after solidifying 20min under the UV-light of 1.0mW/cm2, its quality no longer changes in intensity, the solid matter formed after taking out solidification is also weighed, thereafter N is used, dinethylformamide (DMF) soaks 6h, and 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 filmogen being frozen into solid is 32 DEG C simultaneously.
Embodiment six
Get the filmogen 500g prepared according to the process of embodiment one, photocatalyst 2-hydroxy-2-methyl phenyl-acetone (HMPP) 25g is added at 70 DEG C, the filmogen adding photocatalyst to be poured into thickness be in the square dies of 2cm and be placed on high-precision electronic balance, be that after solidifying 30min under the UV-light of 1.0mW/cm2, its quality no longer changes in intensity, the solid matter formed after taking out solidification is also weighed, thereafter N is used, dinethylformamide (DMF) soaks 6h, and 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 filmogen being frozen into solid is 31 DEG C simultaneously.
Embodiment seven
Get the filmogen 500g prepared according to the process of embodiment one, nano titanium oxide 50g is added at 70 DEG C, described nano titanium oxide is the titanium dioxide nano-crystal of rutile structure, its particle diameter is 5 ~ 10nm, the filmogen adding photocatalyst to be poured into thickness be in the square dies of 2cm and be placed on high-precision electronic balance, be that after solidifying 40min under the UV-light of 0.8mW/cm2, its quality no longer changes in intensity, the solid matter formed after taking out solidification is also weighed, thereafter N is used, dinethylformamide (DMF) soaks 6h, and 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 filmogen being frozen into solid is 31 DEG C simultaneously.
Embodiment eight
Get the filmogen 500g prepared according to the process of embodiment two, photocatalyst DMPA10g is added at 80 DEG C, the filmogen adding photocatalyst to be poured into thickness be in the square dies of 2cm and be placed on high-precision electronic balance, be that after solidifying 20min under the UV-light of 1.0mW/cm2, its quality no longer changes in intensity, the solid matter formed after taking out solidification is also weighed, thereafter N is used, dinethylformamide (DMF) soaks 6h, and 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 filmogen being frozen into solid is 31 DEG C simultaneously.
Embodiment nine
Get the filmogen 500g prepared according to the process of embodiment three, photocatalyst HMPP40g is added at 80 DEG C, the filmogen adding photocatalyst to be poured into thickness be in the square dies of 2cm and be placed on high-precision electronic balance, be that after solidifying 27min under the UV-light of 1.0mW/cm2, its quality no longer changes in intensity, the solid matter formed after taking out solidification is also weighed, thereafter N is used, dinethylformamide (DMF) soaks 6h, and 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 filmogen being frozen into solid is 33 DEG C simultaneously.
Embodiment ten
Get the filmogen 500g prepared according to the process of embodiment four, photocatalyst HMPP50g is added at 80 DEG C, the filmogen adding photocatalyst to be poured into thickness be in the square dies of 2cm and be placed on high-precision electronic balance, be that after solidifying 28min under the UV-light of 1.0mW/cm2, its quality no longer changes in intensity, the solid matter formed after taking out solidification is also weighed, thereafter N is used, dinethylformamide (DMF) soaks 6h, and 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 filmogen being frozen into solid is 32 DEG C simultaneously.
Embodiment 11
Get the filmogen 500g prepared according to the process of embodiment one, boric acid ester coupler 2.5g is entered 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, auxiliary agent polymethylmethacrylate (trade names 701) 2.5g is added after stirring, 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 37 DEG C simultaneously.
Embodiment 12
Get the filmogen 500g prepared according to the process of embodiment one, coupling agent SBW-III5g is added at 80 DEG C, after stirring, add filler silica powder 25g, this silica powder is chemical grade 600 order silica powder, auxiliary agent polymethylmethacrylate (trade names 701) is added after stirring, add-on is 5g, to stir after 10min 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 120 DEG C, the painting film close formed shows slightly coarse, without obvious bubble, pin hole, there is slight granular sensation, 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 13
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, auxiliary agent polymethylmethacrylate (trade names 701) 2.5g is added after stirring, thereafter auxiliary agent tin protochloride is added, add-on is 5g, after stirring 3min, the part in mixture is put in beaker and at 120 DEG C, heats 10min 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, 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 14
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 15
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, 10min 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 16
Get the filmogen 500g prepared according to the process of embodiment three, coupling agent SBW-III10g is added at 70 DEG C, after stirring, add filler talcum powder 60g, this talcum powder is chemical grade 600 order talcum powder, thereafter auxiliary agent stannous octoate 7g is added, to stir after 1min mixture is freezing and pulverize, recording its Tg by DSC is 42 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 shows slightly coarse, without obvious bubble, pin hole, there is slight granular sensation, 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 17
Get the filmogen 500g prepared according to the process of embodiment four, coupling agent SBW-III10g is added at 70 DEG C, after stirring, add filler wollastonite 50g, this wollastonite grain is chemical grade 800 order wollastonite, thereafter auxiliary agent stannous octoate 5g is added, to stir after 1min mixture is freezing and pulverize, recording its Tg by DSC is 40 DEG C, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, 15min solidification is heated at 120 DEG C, the painting film close formed shows slightly coarse, without obvious bubble, pin hole, there is slight granular sensation, 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 18
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.
Embodiment 19
Get the filmogen 500g prepared according to the process of embodiment two, coupling agent SBW-III10g is added at 70 DEG C, after stirring, add filler wollastonite 40g, this wollastonite is chemical grade 800 order wollastonite, auxiliary agent polymethylmethacrylate (trade names 701) 7g is added after stirring, thereafter photocatalyst DMPA10g is added, to stir after 3min mixture is freezing and pulverize, recording its Tg by DSC is 42 DEG C, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, it is 25min 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.
Embodiment 20
Get the filmogen 500g obtained by the process of embodiment two preparation, coupling agent SBW-III7g is added at 70 DEG C, after stirring, add filler wollastonite 30g, this wollastonite is chemical grade 800 order wollastonite, auxiliary agent polymethylmethacrylate (trade names 701) 5g is added after stirring, thereafter photocatalyst HMPP30g is added, to stir after 3min mixture is freezing and pulverize, recording its Tg by DSC is 39 DEG C, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, be that after solidifying 30min under the UV-light of 1.0mW/cm2, observation painting film close is smooth in intensity, 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 21
Get the filmogen 500g prepared according to the process of embodiment three, coupling agent SBW-III5g is added at 80 DEG C, after stirring, add filler wollastonite 25g, this wollastonite is chemical grade 800 order wollastonite, auxiliary agent polymethylmethacrylate (trade names 701) 5g is added after stirring, thereafter photocatalyst HMPP30g is added, thereafter auxiliary agent stannous octoate 5g is added, to stir after 1min mixture is freezing and pulverize, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, it is 20min solidification under the UV-light of 1.0mW/cm2 in intensity, it is smooth that gained is coated with film close, 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 22
Get the filmogen 500g prepared according to the process of embodiment four, coupling agent SBW-III10g is added at 80 DEG C, after stirring, add filler wollastonite 60g, this wollastonite is chemical grade 800 order wollastonite, auxiliary agent polymethylmethacrylate (trade names 701) 7g is added after stirring, thereafter auxiliary agent tin protochloride 6g is added, thereafter photocatalyst DMPA5g is added, to stir after 1min mixture is freezing and pulverize, adopt electrostatic spraying by the mixture application after pulverizing on a metal plate, it is 20min solidification under the UV-light of 1.0mW/cm2 in intensity, it is smooth that gained is coated with film close, 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.
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 (9)
1. a preparation method for the filmogen of the powder coating of low-temperature curing, is characterized in that: comprise the following steps:
1) terephthalic anhydride, MALEIC ANHYDRIDE, p-phthaloyl chloride (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;
Completing steps 3) after namely synthesized the matrix resin of described filmogen, proceed step 4) thereafter:
4) by completing steps 3) four-hole boiling flask stop heating, drop to after below 140 DEG C to temperature, under nitrogen atmosphere, add cured resin wherein;
Described cured resin is the mixture of one or both and thanomin in vinylbenzene or methylbenzene e pioic acid methyl ester.
2. the preparation method of the filmogen of the powder coating of low-temperature curing according to claim 1, is characterized in that: the ratio of the amount of substance of described pentanediol, glycol ether is 1:2 ~ 2:1.
3. the preparation method of the filmogen of the powder coating of low-temperature curing according to claim 1, is characterized in that: described terephthalic anhydride is 1:1 ~ 2:1 with the ratio of the amount of substance of MALEIC ANHYDRIDE.
4. the preparation method of the filmogen of the powder coating of low-temperature curing according to claim 1, is characterized in that: the ratio of the amount of substance of described 1,2-dimethoxy benzene, Resorcinol is 2 ~ 3:4 ~ 5.
5. the preparation method of the filmogen of the powder coating of low-temperature curing according to claim 1, is characterized in that: total amount of substance of described pentanediol, glycol ether is 2:5 ~ 2:7 with the ratio of total amount of substance of terephthalic anhydride, MALEIC ANHYDRIDE.
6. the preparation method of the filmogen of the powder coating of low-temperature curing according to claim 1, is characterized in that: total amount of substance of described terephthalic anhydride, MALEIC ANHYDRIDE be 10:1 ~ 15:1 with the ratio of the amount of substance of TPC.
7. the preparation method of the filmogen of the powder coating of low-temperature curing according to claim 1, is characterized in that: total amount of substance of described 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 preparation method of the filmogen of the powder coating of low-temperature curing according to claim 1, is characterized in that: one or both the amount of substance in described 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 preparation method of the filmogen of the powder coating of low-temperature curing according to claim 1, is characterized in that: the quality of described cured resin is 30% ~ 50% of described matrix resin quality.
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| CN114464337A (en) * | 2020-11-09 | 2022-05-10 | 谢金龙 | Medium-low temperature curing electric heating slurry and preparation method thereof |
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