CN104017417B - A kind of flow agent used for powder coating and preparation method thereof, a kind of powder coating - Google Patents
A kind of flow agent used for powder coating and preparation method thereof, a kind of powder coating Download PDFInfo
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- CN104017417B CN104017417B CN201410276869.9A CN201410276869A CN104017417B CN 104017417 B CN104017417 B CN 104017417B CN 201410276869 A CN201410276869 A CN 201410276869A CN 104017417 B CN104017417 B CN 104017417B
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Abstract
The invention provides a kind of flow agent used for powder coating and preparation method thereof, a kind of powder coating, the present invention utilizes a kind of super molecular compound of higly branched chain---and calixarene and polyisocyanates have prepared a kind of hyperbranched polymer, and be applied to use as novel flow agent in beta-hydroxy alkylamide/polyester powder coating, powder coating formulation is: terminal carboxyl polyester resin 80 ~ 100 parts, beta-hydroxy alkylamide 4 ~ 6 parts, flow agent 1.2 ~ 2.5 parts, air release agent 0.3 ~ 1.5 part, brightening agent 0.5 ~ 2.8 part and color stuffing 50 ~ 80 parts.Compare with prior art, instant invention overcomes the shortcoming that powder coating film levelling property is poor; Add the decorate properties of film, expand 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 add use to bring convenience.
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, become and develop one of coating variety rapidly at present.Become now generally acknowledged and met high, the excellent film performance of production efficiency, ecological environment-friendly type and Eco-power 4E type coating products.
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 formulation, 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 relies on the flowing of resin under molten state and inter-adhesively to form, and melt viscosity is high, limits its unrestricted flow, and levelling effect is slightly poor, has slight orange peel to produce.Improve powder coating film levelling property, form the film that outward appearance is good, be the emphasis that powder coating circle is paid close attention to always.
Powder coating is generally the levelling property improving powder coating by adding flow agent, by balancing the surface tension gradient of film, alleviating Bei Nade eddy effect, alleviating orange peel, promotes that film has better levelling property.But the interpolation of too much 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 in use to be 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 is different, and consistency is bad, easily mutually produces interference.
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.
Present invention also offers a kind of powder coating, there is 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 containing catalyzer step (1) prepared is heated to 40 ~ 50 DEG C, polyisocyanate solution prepared by step (2) is slowly added 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].
Catalyzer described in step (1) can be any one in dibutyltin dilaurate, stannous octoate, triethylamine, trolamine or triethylenediamine.
Described catalyst levels is 0.01% ~ 0.1% of the total mass of p-t-butyl.
Described polyisocyanates can be any one in diphenylmethanediisocyanate (MDI), tolylene diisocyanate (TDI), how vulcabond (NDI) and phenylbenzene isophorone (DPDI).
Powder coating provided by the invention, the formula of this coating comprises the raw material of following weight:
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 the mixture of one or more in titanium dioxide, barium sulfate, wollastonite, mica powder.
The preparation method of powder coating of the present invention is as follows:
(a), take 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 and be placed in compounding jar, fully mixing broken.
B the material after (), fragmentation is through melt extruder melting mixing, the temperature in forcing machine I district is at 100 ~ 130 DEG C, and II district's temperature is at 90 ~ 120 DEG C.Described melt extruder is twin screw or single screw extruder.
(c), extrude after material pack after compressing tablet, cooling, pulverizing and screening, the diameter of particle (equivalent grain size D50) that extrudate obtains after pulverizer is pulverized and sieved is 30 ~ 60 microns.
Adopt the high pressure static electricity method used for powder coating prepared of the method for the invention or fluidized bed process to be coated on metal base, solidification value is 170 ~ 180 DEG C, and set time is 10 ~ 30 minutes, can adopt baking box or to be infraredly cured.
The present invention utilizes a kind of super molecular compound of higly branched chain---and calixarene and polyisocyanates have 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, instant invention overcomes the shortcoming that powder coating film levelling property is poor; Add the decorate properties of film, expand 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 add use to bring convenience.
Embodiment
Embodiment 1
A kind of preparation of powder coating flow agent:
(1) taking 1 part is dissolved in chloroform to tert-butyl-calix [6] aromatic hydrocarbons, forms saturated solution, adds 0.0007 part of triethylamine;
(2) pipetting 6 parts of 2,4 toluene diisocyanates with liquid-transfering gun is dissolved in chloroform, makes the polyisocyanate solution of 0.6mol/L;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, containing triethylamine, 45 DEG C will be heated to tert-butyl-calix [6] arene solution, 2,4 toluene diisocyanate solution in constant pressure funnel was slowly dripped off in 2 hours, continues 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, namely obtains novel flow agent I.
Embodiment 2
A kind of preparation of powder coating flow agent:
(1) taking 1 part is dissolved in chloroform to tert-butyl-calix [6] aromatic hydrocarbons, forms saturated solution, adds 0.003 part of triethylamine;
(2) pipetting 8 parts of 2,4 toluene diisocyanates with liquid-transfering gun is dissolved in chloroform, makes 0.5mol/L polyisocyanate solution;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, containing triethylamine, 40 DEG C will be heated to tert-butyl-calix [6] arene solution, 2,4 toluene diisocyanate solution in constant pressure funnel was slowly dripped off in 2 hours, continues reaction 3h;
(4) continue reaction solution to be warming up to 55 DEG C, add 10 parts to tertiary butyl p tertButylcalixarene, react to solution clarification, solution, after Rotary Evaporators is spin-dried for, obtains faint yellow solid, after vacuum-drying, namely obtains novel flow agent II.
Embodiment 3
A kind of preparation of powder coating flow agent:
(1) taking 1 part is dissolved in chloroform to tert-butyl-calix [6] aromatic hydrocarbons, forms saturated solution, adds 0.004 part of triethylamine;
(2) pipetting 6 part of 2,6-tolylene diisocyanate with liquid-transfering gun is dissolved in chloroform, makes 0.4mol/L polyisocyanate solution;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, containing triethylamine, 45 DEG C will be heated to tert-butyl-calix [6] arene solution, 2,6-tolylene diisocyanate solution in constant pressure funnel were slowly dripped off in 2 hours, continues 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, namely obtains novel flow agent III.
Embodiment 4
A kind of preparation of powder coating flow agent:
(1) taking 1 part is dissolved in chloroform to tertiary butyl p tertButylcalixarene, forms saturated solution, adds 0.005 part of triethylamine;
(2) pipetting 4 parts of 2,4 toluene diisocyanates with liquid-transfering gun is dissolved in chloroform, makes 0.55mol/L polyisocyanate solution;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, containing triethylamine, 50 DEG C will be heated to tert-butyl-calix [4] arene solution, 2,4 toluene diisocyanate solution in constant pressure funnel was slowly dripped off in 2 hours, continues 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, namely obtains novel flow agent IV.
Embodiment 5
A kind of preparation of powder coating flow agent:
(1) taking 1 part is dissolved in chloroform to tert-butyl-calix [6] aromatic hydrocarbons, forms saturated solution, adds 0.003 part of triethylamine;
(2) pipetting 6 parts of diphenylmethanediisocyanates with liquid-transfering gun is dissolved in chloroform, makes the polyisocyanate solution of 0.5mol/L;
(3) under the condition of logical nitrogen, mechanical stirring and condensing reflux, containing triethylamine, 45 DEG C will be heated to tert-butyl-calix [6] arene solution, diphenylmethanediisocyanate solution in constant pressure funnel was slowly dripped off in 2 hours, continues 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, namely 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 () takes 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 is placed in compounding jar, fully mixing is also broken.
B the material after () fragmentation is through melt extruder melting mixing, the temperature in forcing machine I district is at 100 ~ 130 DEG C, and II district's temperature is at 90 ~ 120 DEG C.Described melt extruder is twin screw or single screw extruder.
(c) extrude after material pack after compressing tablet, cooling, pulverizing and screening, 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: powder coating and their application embodiment 6 ~ 10 and comparative example 1,2 obtained respectively by the method for electrostatic spraying is in long 145mm, and wide 70mm, on the iron plate of thick 1mm, solidifies 10min under 180 DEG C of conditions.
Sample testing step: film coated surface degree of roughness by naked-eye observation, and carries out PCI classification; Horizontal flow detects with reference to standard GB/T/T6554-2003.
From comparison of test results, in powder coating formulation, add the novel flow agent of the present invention's synthesis, the levelling property of film can be improved significantly, and reach domestic and international peer-level, improve the decorate properties of powder coating.
Table 1 embodiment 6-10, comparative example 1-2 powder coating formulation
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 according to claim 1, it 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 containing catalyzer step (1) prepared is heated to 40 ~ 50 DEG C, polyisocyanate solution prepared by step (2) is slowly added 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, catalyzer described in step (1) is any one in dibutyltin dilaurate, stannous octoate, triethylamine, trolamine or triethylenediamine, and described catalyst levels is 0.01% ~ 0.1% of the total mass of p-t-butyl.
6. preparation method according to claim 2, is characterized in that, the polyisocyanates described in step (2) is any one in diphenylmethanediisocyanate, tolylene diisocyanate.
7. a powder coating, is characterized in that, the formula of this coating comprises the flow agent prepared by 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:
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, it 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 the mixture of one or more in titanium dioxide, barium sulfate, wollastonite, mica powder.
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| CN104530811B (en) * | 2015-01-09 | 2016-08-24 | 宁夏康诚机电产品设计有限公司 | A kind of aluminium section bar red powder coating uniform reinforcing agent and preparation method thereof |
| 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 |
| CN105505144B (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 forest grade and preparation method 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 |
| CN105602414B (en) * | 2015-12-30 | 2018-11-09 | 老虎表面技术新材料（苏州）有限公司 | A kind of thermosetting property anion powder coating and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| EP0196895A2 (en) * | 1985-03-28 | 1986-10-08 | LOCTITE (IRELAND) Ltd. | Polymer bound calixarenes |
| CN102597048A (en) * | 2009-11-06 | 2012-07-18 | 国际商业机器公司 | Bilayer systems including a polydimethylglutarimide-based bottom layer and compositions thereof |
| CN102781582A (en) * | 2009-11-06 | 2012-11-14 | 加利福尼亚大学董事会 | Metal colloids with accessible metal surfaces |
| CN103725234A (en) * | 2013-12-03 | 2014-04-16 | 常州大学 | Calixarene modified attapulgite/urea resin composite adhesive and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003229567A1 (en) * | 2003-03-24 | 2004-10-18 | Centre National De La Recherche Scientifique | New calix arene compounds, their process of preparation and their use, particularly as enzymatic mimes |
| FR2939666B1 (en) * | 2008-12-17 | 2012-11-30 | Irsn | COSMETIC AND PHARMACEUTICAL FORMULATIONS OF CALIX MOLECULES [6] ARENES |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0196895A2 (en) * | 1985-03-28 | 1986-10-08 | LOCTITE (IRELAND) Ltd. | Polymer bound calixarenes |
| CN102597048A (en) * | 2009-11-06 | 2012-07-18 | 国际商业机器公司 | Bilayer systems including a polydimethylglutarimide-based bottom layer and compositions thereof |
| CN102781582A (en) * | 2009-11-06 | 2012-11-14 | 加利福尼亚大学董事会 | Metal colloids with accessible metal surfaces |
| CN103725234A (en) * | 2013-12-03 | 2014-04-16 | 常州大学 | Calixarene modified attapulgite/urea resin composite adhesive and preparation method thereof |
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Inventor after: Zhang Caogen Inventor before: Zhou Yunyou Inventor before: Wang Long Inventor before: Sun Junyong |
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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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