CN104017417A - Leveling agent for powder coating, preparation method thereof and powder coating - Google Patents
Leveling agent for powder coating, preparation method thereof and powder coating Download PDFInfo
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Abstract
The invention provides a leveling agent for a powder coating, a preparation method thereof and a powder coating. The preparation method disclosed by the invention comprises the following steps: preparing a hyperbranched polymer from calixarene as a multi-branched supramolecular compound and polyisocyanate and applying the hyperbranched polymer as a novel leveling agent in a beta-hydroxyalkylamide/polyester powder coating, wherein the powder coating comprises the following components in parts by weight: 80-100 parts of terminal carboxyl polyester resin, 4-6 parts of beta-hydroxyalkylamide, 1.2-2.5 parts of leveling agent, 0.3-1.5 parts of degassing agent, 0.5-2.8 parts of brightener and 50-80 parts of pigment and filler. Compared with the prior art, the leveling agent disclosed by the invention has the advantages that the defect of the poor leveling property of the powder coating film is overcome; the decorative performance of the film is increased and the application field of the powder coating is enlarged; since leveling agents for powder coatings are mostly liquid products, the transport and addition are inconvenient, the product disclosed by the invention is in a solid powder form and brings convenience for the transport and addition use.
Description
Technical field
The invention belongs to paint field, be specifically related to a kind of powder coating, a kind of flow agent used for powder coating and preparation method thereof.
Background technology
Powder coating and application with its resource-saving, economize energy, nuisanceless, labor productivity is high and be convenient to realize the features such as automation paint, becomes current development one of coating variety rapidly.Become now generally acknowledged high, the good film performance of production efficiency, ecological environment-friendly type and the Eco-power 4E type coating products of meeting.
In thermosetting powder coating(s), flow agent is one of requisite auxiliary agent in powder coating composition.No matter be Gao Guang, have light, half light, sub-light or glossless powdered coating, in powder coating formula, all must add flow agent.Compared with liquid coating, the levelling of powder coating is more much more difficult than liquid coating, and the levelling property of powder coating film is also far short of what is expected than liquid coating film, and this and powder coating do not have much relations containing solvent.The film process of powder coating is also inter-adhesive the forming of flowing that relies on resin under molten state, and melt viscosity is high, has limited its unrestricted flow, and levelling effect is slightly poor, has slight orange peel to produce.Improve powder coating film levelling property, form the good film of outward appearance, be the emphasis that powder coating circle is paid close attention to always.
Powder coating is generally the levelling property that improves powder coating by adding flow agent, by the surface tension gradient of balance film, alleviates Bei Nade eddy effect, alleviates orange peel, promotes that film has better levelling property.But too much the interpolation of flow agent can affect the package stability of powder coating.
The flow agent that powder coating is conventional has Voncoat R 3310, acrylate copolymer, silicone modified polyacrylate and polyoxy silane etc., these flow agents are all generally thick liquid, also need to be in use distributed in resin, aerosil or some filler, this will increase cost to suitability for industrialized production.Flow agent used for powder coating research is at home also fewer, and in order to obtain the film of different planeness, the research of flow agent used for powder coating will be an important directions.
In prior art, the current domestic level of flow agent used for powder coating is lower, and film flow leveling does not reach expection requirement, and flow agent range of application is restricted, and coating film gloss degree does not reach related request; Great majority are viscous liquid, are inconvenient to add use; Flow agent system difference, consistency is bad, easily mutually produces and disturbs.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of flow agent used for powder coating and preparation method thereof.
The present invention also provides a kind of powder coating, has good levelling property and decorate properties.
One provided by the invention flow agent used for powder coating, structural formula is:
In formula, R is C
6h
4, C
7h
6, C
13h
10;
M is 4 or 6;
N is 4 or 6.
The preparation method of a kind of flow agent used for powder coating provided by the invention, comprises the following steps:
(1), get first part of p-t-butyl and be dissolved in chloroform, form saturated solution, add catalyzer;
(2), get polyisocyanates and be dissolved in chloroform, make the polyisocyanate solution of 0.4～0.6mol/L;
(3), under the condition of logical nitrogen, mechanical stirring and condensing reflux, the p-t-butyl solution that contains catalyzer prepared by step (1) is heated to 40～50 DEG C, polyisocyanate solution prepared by step (2) slowly adds in p-t-butyl solution, continues reaction 1～6h;
(4), continue reaction solution to be warming up to 55～65 DEG C, add second part of p-t-butyl, react to solution clarification, after evaporation, obtain faint yellow solid, after vacuum-drying, obtain product.
First part of described p-t-butyl: polyisocyanates: second part of p-t-butyl mol ratio is: 1:4～12:4.2～12.5.
Described p-t-butyl is to tert-butyl-calix [4], to any one in tert-butyl-calix [6].
The described catalyzer of step (1) can be any one in dibutyltin dilaurate, stannous octoate, triethylamine, trolamine or triethylenediamine.
Described catalyst levels be p-t-butyl total mass 0.01%～0.1%.
Described polyisocyanates can be any one in diphenylmethanediisocyanate (MDI), tolylene diisocyanate (TDI), how vulcabond (NDI) and phenylbenzene sec.-propyl vulcabond (DPDI).
Powder coating provided by the invention, the formula of this coating comprises the raw material of following weight part proportioning:
The acid number of described terminal carboxyl polyester resin is 25～40mgKOH/g, and second-order transition temperature is 55～65 DEG C.
Described beta-hydroxy alkylamide is any one in Primid XL 552 or Primid QM 1260.
Described air release agent is one or both the mixture in st-yrax or modification st-yrax.
Described brightening agent is 701 auxiliary agents.
Described color stuffing is one or more the mixture in titanium dioxide, barium sulfate, wollastonite, mica powder.
The preparation method of powder coating of the present invention is as follows:
(a), taking terminal carboxyl polyester resin, beta-hydroxy alkylamide, novel flow agent, air release agent, brightening agent and color stuffing by part by weight of the present invention is placed in compounding jar, fully mixing broken.
(b) material, after fragmentation is through melt extruder melting mixing, and the temperature in forcing machine I district is at 100～130 DEG C, and II district temperature is at 90～120 DEG C.Described melt extruder is twin screw or single screw extruder.
(c) material, after extruding through compressing tablet, cooling, pulverize and screening after packaging, the diameter of particle (equivalent grain size D50) that extrudate obtains after pulverizer is pulverized and sieved is 30～60 microns.
The high pressure static electricity method used for powder coating or the fluidized bed process that adopt the method for the invention to prepare are coated on metal base, and solidification value is 170～180 DEG C, and be 10～30 minutes set time, can adopt baking box or infrared being cured.
The present invention utilizes a kind of super molecular compound of higly branched chain---and calixarene and polyisocyanates have been prepared a kind of hyperbranched polymer, and be applied to use as novel flow agent in beta-hydroxy alkylamide/polyester powder coating, compare with prior art, the present invention has overcome the poor shortcoming of powder coating film levelling property; Increase the decorate properties of film, expanded the Application Areas of powder coating; Flow agent used for powder coating is mostly liquid product, transport, interpolation inconvenience, and product of the present invention is solid powdery, gives transport and adds use and brought convenience.
Embodiment
Embodiment 1
The preparation of flow agent for a kind of powder coating:
(1) take 1 part tert-butyl-calix [6] aromatic hydrocarbons is dissolved in chloroform, form saturated solution, add 0.0007 part of triethylamine;
(2) pipette 6 parts of 2,4 toluene diisocyanates with liquid-transfering gun and be dissolved in chloroform, make the polyisocyanate solution of 0.6mol/L;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, by what contain triethylamine, tert-butyl-calix [6] aromatic hydrocarbons solution is heated to 45 DEG C, 2,4 toluene diisocyanate solution in constant pressure funnel was slowly dripped off in 2 hours, continue reaction 2h;
(4) continue reaction solution to be warming up to 55 DEG C, add 6 parts to tert-butyl-calix [6] aromatic hydrocarbons, react to solution clarification, solution, after Rotary Evaporators is spin-dried for, obtains faint yellow solid, after vacuum-drying, obtains novel flow agent I.
Embodiment 2
The preparation of flow agent for a kind of powder coating:
(1) take 1 part tert-butyl-calix [6] aromatic hydrocarbons is dissolved in chloroform, form saturated solution, add 0.003 part of triethylamine;
(2) pipette 8 parts of 2,4 toluene diisocyanates with liquid-transfering gun and be dissolved in chloroform, make 0.5mol/L polyisocyanate solution;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, by what contain triethylamine, tert-butyl-calix [6] aromatic hydrocarbons solution is heated to 40 DEG C, 2,4 toluene diisocyanate solution in constant pressure funnel was slowly dripped off in 2 hours, continue reaction 3h;
(4) continue reaction solution to be warming up to 55 DEG C, add 10 parts to tert-butyl-calix [4] aromatic hydrocarbons, react to solution clarification, solution, after Rotary Evaporators is spin-dried for, obtains faint yellow solid, after vacuum-drying, obtains novel flow agent II.
Embodiment 3
The preparation of flow agent for a kind of powder coating:
(1) take 1 part tert-butyl-calix [6] aromatic hydrocarbons is dissolved in chloroform, form saturated solution, add 0.004 part of triethylamine;
(2) pipette 6 part 2 with liquid-transfering gun, 6-tolylene diisocyanate is dissolved in chloroform, makes 0.4mol/L polyisocyanate solution;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, by what contain triethylamine, tert-butyl-calix [6] aromatic hydrocarbons solution is heated to 45 DEG C, by 2 in constant pressure funnel, 6-tolylene diisocyanate solution slowly dripped off in 2 hours, continued reaction 2h;
(4) continue reaction solution to be warming up to 54 DEG C, add 7 parts to tert-butyl-calix [6] aromatic hydrocarbons, react to solution clarification, solution, after Rotary Evaporators is spin-dried for, obtains faint yellow solid, after vacuum-drying, obtains novel flow agent III.
Embodiment 4
The preparation of flow agent for a kind of powder coating:
(1) take 1 part tert-butyl-calix [4] aromatic hydrocarbons is dissolved in chloroform, form saturated solution, add 0.005 part of triethylamine;
(2) pipette 4 parts of 2,4 toluene diisocyanates with liquid-transfering gun and be dissolved in chloroform, make 0.55mol/L polyisocyanate solution;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, by what contain triethylamine, tert-butyl-calix [4] aromatic hydrocarbons solution is heated to 50 DEG C, 2,4 toluene diisocyanate solution in constant pressure funnel was slowly dripped off in 2 hours, continue reaction 4h;
(4) continue reaction solution to be warming up to 58 DEG C, add 5 parts to tert-butyl-calix [6] aromatic hydrocarbons, react to solution clarification, solution, after Rotary Evaporators is spin-dried for, obtains faint yellow solid, after vacuum-drying, obtains novel flow agent IV.
Embodiment 5
The preparation of flow agent for a kind of powder coating:
(1) take 1 part tert-butyl-calix [6] aromatic hydrocarbons is dissolved in chloroform, form saturated solution, add 0.003 part of triethylamine;
(2) pipette 6 parts of diphenylmethanediisocyanates with liquid-transfering gun and be dissolved in chloroform, make the polyisocyanate solution of 0.5mol/L;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, by what contain triethylamine, tert-butyl-calix [6] aromatic hydrocarbons solution is heated to 45 DEG C, diphenylmethanediisocyanate solution in constant pressure funnel was slowly dripped off in 2 hours, continue reaction 2h;
(4) continue reaction solution to be warming up to 55 DEG C, add 6 parts to tert-butyl-calix [6] aromatic hydrocarbons, react to solution clarification, solution, after Rotary Evaporators is spin-dried for, obtains faint yellow solid, after vacuum-drying, obtains novel flow agent V.
Embodiment 6
A kind of powder coating, the formula of described powder coating is as shown in table 1 below;
Embodiment 7
A kind of powder coating, the formula of described powder coating is as shown in table 1 below;
Embodiment 8
A kind of powder coating, the formula of described powder coating is as shown in table 1 below;
Embodiment 9
A kind of powder coating, the formula of described powder coating is as shown in table 1 below;
Embodiment 10
A kind of powder coating, the formula of described powder coating is as shown in table 1 below;
Comparative example 1
A kind of powder coating, the formula of described powder coating is as shown in table 1 below;
Comparative example 2
A kind of powder coating, the formula of described powder coating is as shown in table 1 below;
The preparation method of the powder coating of embodiment 6～10, comparative example 1～2 is as follows:
(a) take terminal carboxyl polyester resin, beta-hydroxy alkylamide, flow agent, air release agent, brightening agent and color stuffing by the described part by weight of upper table and be placed in compounding jar, fully mix and fragmentation.
(b) material after fragmentation is through melt extruder melting mixing, and the temperature in forcing machine I district is at 100～130 DEG C, and II district temperature is at 90～120 DEG C.Described melt extruder is twin screw or single screw extruder.
(c) material after extruding through compressing tablet, cooling, pulverize and screening after packaging, the diameter of particle (equivalent grain size D50) that extrudate obtains after pulverizer is pulverized and sieved is 30～60 microns.
The preparation of sample: the powder coating and their application respectively embodiment 6～10 and comparative example 1,2 being made by the method for electrostatic spraying is in long 145mm, wide 70mm, the iron plate of thick 1mm is upper, solidifies 10min under 180 DEG C of conditions.
Sample testing step: film coated surface degree of roughness is by naked-eye observation, and carry out PCI classification; Horizontal flow detects with reference to standard GB/T/T6554-2003.
From comparison of test results, the novel flow agent that adds the present invention to synthesize in powder coating formula, can improve significantly the levelling property of film, and reach domestic and international peer-level, has improved the decorate properties of powder coating.
Table 1 embodiment 6-10, comparative example 1-2 powder coating formula
Claims (10)
1. a flow agent used for powder coating, is characterized in that, described flow agent structural formula is:
In formula, R is C
6h
4, C
7h
6, C
13h
10;
M is 4 or 6;
N is 4 or 6.
2. the preparation method of a kind of flow agent used for powder coating claimed in claim 1, is characterized in that, described preparation method comprises the following steps:
(1), get first part of p-t-butyl and be dissolved in chloroform, form saturated solution, add catalyzer;
(2), get polyisocyanates and be dissolved in chloroform, make the polyisocyanate solution of 0.4～0.6mol/L;
(3), under the condition of logical nitrogen, mechanical stirring and condensing reflux, the p-t-butyl solution that contains catalyzer prepared by step (1) is heated to 40～50 DEG C, polyisocyanate solution prepared by step (2) slowly adds in p-t-butyl solution, continues reaction 1～6h;
(4), continue reaction solution to be warming up to 55～65 DEG C, add second part of p-t-butyl, react to solution clarification, after evaporation, obtain faint yellow solid, after vacuum-drying, obtain product.
3. preparation method according to claim 2, is characterized in that, first part of described p-t-butyl: polyisocyanates: second part of p-t-butyl mol ratio is: 1:4～12:4.2～12.5.
4. preparation method according to claim 2, is characterized in that, described p-t-butyl is to tert-butyl-calix [4], to any one in tert-butyl-calix [6].
5. preparation method according to claim 2, it is characterized in that, the described catalyzer of step (1) can be any one in dibutyltin dilaurate, stannous octoate, triethylamine, trolamine or triethylenediamine, 0.01%～0.1% of the total mass that described catalyst levels is p-t-butyl.
6. preparation method according to claim 2, it is characterized in that, the described polyisocyanates of step (2) can be any one in diphenylmethanediisocyanate, tolylene diisocyanate, how vulcabond and phenylbenzene sec.-propyl vulcabond.
7. a powder coating, is characterized in that, the formula of this coating comprises the flow agent described in claim 2-6 any one.
8. powder coating according to claim 7, is characterized in that, the formula of described coating comprises the raw material of following weight part proportioning:
9. powder coating according to claim 8, is characterized in that, described beta-hydroxy alkylamide is any one in Primid XL 552 or Primid QM 1260.
10. powder coating according to claim 8 or claim 9, is characterized in that, the acid number of described terminal carboxyl polyester resin is 25～40mgKOH/g, and second-order transition temperature is 55～65 DEG C; Described air release agent is one or both the mixture in st-yrax or modification st-yrax; Described brightening agent is 701 auxiliary agents; Described color stuffing is one or more the mixture in titanium dioxide, barium sulfate, wollastonite, mica powder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530811A (en) * | 2015-01-09 | 2015-04-22 | 黄文辉 | Aluminum profile red powder coating even reinforcing agent and preparation method thereof |
| CN104530812A (en) * | 2015-01-09 | 2015-04-22 | 黄文辉 | Aluminum profile powder coating even reinforcing agent and preparation method thereof |
| CN105419586A (en) * | 2015-12-30 | 2016-03-23 | 老虎粉末涂料制造（太仓）有限公司 | Park grade thermosetting negative ion powdery paint, preparation method and applications thereof |
| CN105505144A (en) * | 2015-12-30 | 2016-04-20 | 老虎粉末涂料制造（太仓）有限公司 | Forest-grade thermoset negative ion powder coating as well as preparation method and application thereof |
| CN105602414A (en) * | 2015-12-30 | 2016-05-25 | 老虎粉末涂料制造（太仓）有限公司 | Thermoset negative ion powder coating and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530811A (en) * | 2015-01-09 | 2015-04-22 | 黄文辉 | Aluminum profile red powder coating even reinforcing agent and preparation method thereof |
| CN104530812A (en) * | 2015-01-09 | 2015-04-22 | 黄文辉 | Aluminum profile powder coating even reinforcing agent and preparation method thereof |
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| CN104530812B (en) * | 2015-01-09 | 2016-08-24 | 宁夏鸿裕机械科技有限公司 | A kind of uniform reinforcing agent of aluminium section bar powder coating and preparation method thereof |
| CN105419586A (en) * | 2015-12-30 | 2016-03-23 | 老虎粉末涂料制造（太仓）有限公司 | Park grade thermosetting negative ion powdery paint, preparation method and applications thereof |
| CN105505144A (en) * | 2015-12-30 | 2016-04-20 | 老虎粉末涂料制造（太仓）有限公司 | Forest-grade thermoset negative ion powder coating as well as preparation method and application thereof |
| CN105602414A (en) * | 2015-12-30 | 2016-05-25 | 老虎粉末涂料制造（太仓）有限公司 | Thermoset negative ion powder coating and preparation method and application thereof |
| CN105419586B (en) * | 2015-12-30 | 2018-11-09 | 老虎表面技术新材料（苏州）有限公司 | Thermosetting property anion powder coating of park grade and preparation method thereof |
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| CN104017417B (en) | 2015-10-21 |
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Effective date of registration: 20170621 Address after: 511400, No. 22, Zhenxing South Road, Shek Tung Street, Dalong street, Panyu District, Guangdong, Guangzhou two, China Patentee after: Guangzhou guest decoration materials Co., Ltd. Address before: 241000 Yijiang,, Wuhu, Anhwei Normal University Patentee before: Anhui Normal University |
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