CN112457748B - High-toughness low-temperature-resistant powder coating and preparation method thereof - Google Patents
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/26—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers modified by chemical after-treatment
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Abstract
The invention relates to the technical field of powder coatings, in particular to a high-toughness low-temperature-resistant powder coating and a preparation method thereof. The high-toughness low-temperature-resistant powder coating is prepared by mixing polypropylene degradation resin and polyester resin according to the mass ratio of 3:2-27, adding a curing agent, a brightener, a leveling agent, benzoin, titanium dioxide, barium sulfate and pigment, and extruding the mixture by an extruder; the polypropylene degradation resin is obtained by degrading polypropylene resin, and the molecular weight of the polypropylene degradation resin is 3000-5000. The high-toughness low-temperature-resistant powder coating improves the low-temperature performance of the polyester powder coating, and a coating film has good toughness, good impact resistance and high strength under a low-temperature condition, is suitable for being used in a low-temperature environment, and has low raw material cost; the invention also provides a preparation method of the composition.
Description
Technical Field
The invention relates to the technical field of powder coatings, and particularly relates to a high-toughness low-temperature-resistant powder coating and a preparation method thereof.
Background
The powder coating is a solid powder synthetic resin coating composed of solid resin, pigment, filler, auxiliary agent and the like. Unlike conventional solvent-based coatings and water-based coatings, the dispersion medium is not a solvent and water, but air. The powder coating has 100 percent of solid content and no solvent, so no volatile matter is generated in the spraying construction process, and the powder coating has the characteristics of no solvent pollution, 100 percent of film forming and low energy consumption and is an environment-friendly coating.
The powder coating includes two main types of thermoplastic powder coating and thermosetting powder coating.
The thermoplastic powder coating is composed of thermoplastic resin, pigment, filler, plasticizer, stabilizer and other components, is formed by electrostatic spraying, heating and melting, and is solidified into a film when cooled. Most of the raw materials used are polymers which are common in the market, and the requirements of service performance can be met under most conditions. However, the thermoplastic powder coating has certain defects of high melting temperature, low coloring level, poor adhesion with metal surfaces, low surface hardness and poor weather resistance, and is generally used as an anticorrosive coating of pipelines but not used as a protective coating of industrial equipment.
The thermosetting powder coating is characterized in that thermosetting resin is used as a film forming substance, a curing agent for crosslinking reaction is added, and the film forming material is heated to form reticular crosslinked macromolecules, so that the coating is hard, the coating cannot be softened like a thermoplastic coating at a higher temperature and can only be decomposed. However, the coating film of the thermosetting powder coating has poor toughness, poor impact resistance and poor low-temperature performance, and is not suitable for application in a low-temperature environment.
Patent CN2014100250172 discloses a degradable thermosetting powder coating and a preparation method thereof, wherein 25-55 parts of thermosetting resin, 4-20 parts of curing agent, 15-50 parts of degrading agent, 0.1-5 parts of flatting agent and 5-20 parts of pigment and filler are mixed, then melt-extruded, pressed into tablets and crushed, ground into powder and screened in grades to obtain a finished product. On the premise of meeting the basic performance of the thermosetting powder coating, the invention realizes the good degradation function of the thermosetting powder coating and avoids the pollution to the environment.
Patent CN2014103676849 discloses a preparation method of low-temperature thermosetting powder coating, which comprises uniformly mixing raw materials of epoxy resin E-12, polyester resin P-0583, leveling agent 388, barium sulfate, accelerant, catalytic assistant and benzoin, melting and dispersing, rolling into sheets, cooling, crushing the sheet powder, grinding into powder, and screening in grades to obtain a finished product; the invention mainly reduces the curing temperature of the thermosetting powder, reduces the production cost and expands the coating range.
None of the above patents solves the problems of poor toughness and poor impact resistance of the coating film of the thermosetting powder coating, and the low temperature properties of the coating film are not improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the high-toughness low-temperature-resistant powder coating, the low-temperature performance of the polyester powder coating is improved, and a coating film has good toughness, good impact resistance and high strength under the low-temperature condition, is suitable for being used in a low-temperature environment, and has low raw material cost; the invention also provides a preparation method of the composition.
The high-toughness low-temperature-resistant powder coating is prepared by mixing polypropylene degradation resin and polyester resin according to the mass ratio of 3:2-27, adding a curing agent, a brightener, a leveling agent, benzoin, titanium dioxide, barium sulfate and pigment, and extruding the mixture by an extruder;
the polypropylene degradation resin is obtained by degrading polypropylene resin, and the molecular weight of the polypropylene degradation resin is 3000-5000.
Preferably, the mass ratio of the polypropylene degradation resin to the polyester resin is 3:3 to 7.
The dosage of the curing agent is 7-8% of the mass of the polyester resin.
The weight percentage of the total mass of the polypropylene degradation resin and the polyester resin is as follows:
the amount of the brightener is 0.5-1%;
the using amount of the flatting agent is 1-2%;
the dosage of benzoin is 0.5-1%;
the amount of titanium dioxide is 4-6%;
the dosage of barium sulfate is 50-60%;
the pigment consumption is 1-2%.
The curing agent is TGIC curing agent, namely tris epoxy propyl isocyanurate.
The brightener is acrylate copolymer or methacrylate copolymer, preferably brightener C701 produced by Hubei Laisi company. The brightener can improve the wettability of resin to pigment and filler, reduce the surface tension of powder coating in the melting process, avoid the defects of coating such as pinholes, shrinkage cavities and the like, play a role in helping leveling and obviously improve the appearance of the coating.
The leveling agent is silicon dioxide modified polyacrylate, preferably leveling agent H88 produced by Hubei Laisi company. The leveling agent can reduce the melt viscosity of the powder coating, increase the fluidity of the coating in a molten state, and eliminate surface defects such as orange peel, shrinkage cavity, pinholes and the like, so that the coating can obtain better flatness.
The molecular weight of the polypropylene resin is generally between 10 and 50 ten thousand, the viscosity of the polypropylene resin is very high, the polypropylene resin cannot be ground into fine powder of 200 meshes, and the high molecular weight polypropylene resin is not compatible with polyester resin and cannot be directly used for preparing powder coating. Before the polypropylene resin and the polyester resin are mixed, the polypropylene resin needs to be subjected to degradation treatment so as to reduce the molecular weight of the polypropylene resin to 3000-5000.
The degradation treatment process of the polypropylene resin is as follows:
under the action of a catalyst, initiating polypropylene resin to generate a free radical reaction, controlling the degradation half-life period to be 1h, the degradation temperature to be 137 ℃, the reaction end temperature to be 200 ℃, and the degradation time to be 3h (including the temperature rise time); after degradation, heating to 270 ℃ and preserving heat for 1h, then quickly cooling and discharging to obtain the polypropylene degradation resin with the molecular weight of 3000-plus 5000.
The catalyst is peroxide bis (tert-butyl peroxide) diisopropylbenzene, and the addition amount is 0.2-0.5% of the mass of the polypropylene resin.
Wherein the macromolecular polypropylene resin generates bond breakage in the degradation process, thereby reducing the molecular weight; then heating to 270 ℃ and preserving the temperature for 1h, belonging to the thermal cracking process, and extracting volatile matters such as tert-butyl alcohol and the like generated by the decomposition of the catalyst; after 1 hour, the temperature needs to be rapidly reduced for discharging, and if the product stays in the kettle for too long time, an exothermic reaction is generated, so that the quality of the product is reduced, and the using effect is influenced.
The preparation method of the high-toughness low-temperature-resistant powder coating comprises the following steps:
firstly, degrading polypropylene resin to obtain polypropylene degraded resin with the molecular weight of 3000-; and adding the polypropylene degradation resin, the polyester resin, the curing agent, the brightener, the flatting agent, the benzoin, the titanium dioxide, the barium sulfate and the pigment into a mixer, mixing at normal temperature, extruding by an extruder, tabletting by a tablet press, grinding, and sieving by a 200-mesh sieve to obtain the high-toughness low-temperature-resistant powder coating.
The extruder had a first stage temperature of 125 ℃ and a second stage temperature of 130 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) The polypropylene resin is subjected to degradation treatment and is mixed with the polyester resin for use, so that the prepared powder coating has good toughness and low-temperature performance, can successfully pass an impact resistance test at the temperature of-20 ℃, and has better toughness and low-temperature performance than the traditional polyester powder coating;
(2) the invention adopts the polypropylene resin with lower cost to replace a part of polyester resin, reduces the cost of raw materials, and compared with the prior polyester powder coating, the cost of the raw materials is reduced by more than 30 percent.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the present invention is not limited thereto, and modifications of the technical solutions of the present invention by those skilled in the art should be within the scope of the present invention.
The raw materials and the amounts thereof of examples 1 to 3 and comparative examples 1 to 3 are shown in Table 1, and the amounts of the raw materials are in kg.
Wherein the polyester resin is polyester resin 4868 for Anhui sword;
the curing agent adopts TGIC curing agent;
the brightener C701 produced by Hubei Laisi company is adopted as the brightener;
the leveling agent is leveling agent H88 produced by Hubei Laisi company;
the polypropylene degradable resin is obtained by adopting commercially available polypropylene resin through the following degradation treatments:
Under the action of a catalyst peroxide bis (tert-butyl peroxide) diisopropylbenzene, the addition amount of the catalyst is 0.3 percent of the mass of the polypropylene resin, the polypropylene resin is initiated to generate a free radical reaction, the degradation half-life period is controlled to be 1h, the degradation temperature is 137 ℃, the reaction end temperature is 200 ℃, and the degradation time is 3h (including the temperature rise time); after degradation, heating to 270 ℃ and preserving heat for 1h, then quickly cooling and discharging to obtain the polypropylene degradation resin with the molecular weight of 3000-5000.
Table 1 raw materials and amounts thereof for examples 1 to 3 and comparative examples 1 to 3
| Starting materials | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Polyester resin | 210 | 150 | 120 | 270 | 300 | — | 280 |
| Polypropylene degradation resin | 90 | 150 | 180 | 30 | — | 300 | 20 |
| Curing agent | 15 | 11 | 8 | 20 | 21 | — | 21 |
| Brightener | 1.5 | 2 | 3 | 2 | 2 | 2 | 2 |
| Leveling agent | 5 | 5 | 6 | 5 | 5 | 5 | 5 |
| Benzoinum | 1.5 | 2 | 3 | 2 | 2 | 2 | 2 |
| Titanium white powder | 12 | 15 | 18 | 15 | 15 | 15 | 15 |
| Barium sulfate | 150 | 160 | 180 | 160 | 160 | 160 | 160 |
| Pigment (I) | 3 | 4 | 6 | 4 | 4 | 4 | 4 |
Example 1
Adding the polypropylene degradation resin, the polyester resin, the curing agent, the brightener, the flatting agent, the benzoin, the titanium dioxide, the barium sulfate and the pigment into a mixer according to the raw material proportion, mixing, extruding by an extruding machine, tabletting by a tabletting machine, grinding, and sieving by a 200-mesh sieve to obtain the high-toughness low-temperature-resistant powder coating.
And (3) spraying the prepared powder coating on a sample plate, and curing at 200 ℃ for 10min and then detecting.
Example 2
This example was prepared in the same manner as example 1.
Example 3
This example was prepared in the same manner as example 1.
Example 4
This example was prepared in the same manner as example 1.
Comparative example 1
The comparative example is different from example 2 only in that the raw materials do not contain the polypropylene degradation resin, the amount of the curing agent is increased, and the preparation method is the same as example 1.
Comparative example 2
This comparative example is different from example 2 only in that the polyester resin and the curing agent are not contained in the raw materials, and the preparation method is the same as that of example 1.
Comparative example 3
The comparative example is different from example 2 only in that the mass ratio of the polypropylene-degraded resin to the polyester resin is 14:1, the amount of the curing agent is increased, and the preparation method is the same as example 1.
The film-forming properties of the examples and comparative products were tested as follows:
(1) and (3) testing the impact resistance: GB/T1732-1993;
(2) cupping test: GB 9753-1988;
(3) adhesion force: GB/T9286-1998;
(4) bending: GB 6742-1986;
(5) accelerated weather resistance test: GB/T1865, GB/T9754, GB 1771-1991.
The test results are shown in table 2:
table 2 film forming property test results of examples and comparative examples
As can be seen from Table 2, the powder coating prepared by the invention has good mechanical property, adhesive force and weather resistance under normal temperature, and has good low-temperature resistance, and the changes of the impact resistance and the bending property are not large under the condition of-20 ℃. Compared with the example 2, the comparative examples 1 and 3 contain less polypropylene degradable resin or less polypropylene degradable resin, and the performances of the resin at normal temperature are not much different from those of the invention, but the impact resistance and bending performance of the resin at low temperature are obviously reduced, so the resin is not suitable for being used at low temperature and has higher cost. Compared with the example 2, the modified epoxy resin composition does not contain polyester resin, although the impact resistance and the bending property of the modified epoxy resin composition are not changed greatly under the normal temperature condition and the temperature of minus 20 ℃, the modified epoxy resin composition has various properties under the normal temperature condition which are lower than those of the modified epoxy resin composition, and the toughness and the adhesive force are poor and can not reach the national standard.
Claims (8)
1. A high-toughness low-temperature-resistant powder coating is characterized in that: mixing polypropylene degradation resin and polyester resin according to the mass ratio of 3:2-27, adding a curing agent, a brightener, a leveling agent, benzoin, titanium dioxide, barium sulfate and pigment, and extruding by an extruder to obtain the modified polypropylene;
the weight percentage of the total mass of the polypropylene degradation resin and the polyester resin is as follows:
the amount of the brightener is 0.5-1%;
the using amount of the flatting agent is 1-2%;
the dosage of benzoin is 0.5-1%;
the amount of titanium dioxide is 4-6%;
the dosage of barium sulfate is 50-60%;
the using amount of the pigment is 1-2%;
the polypropylene degradable resin is obtained by degrading polypropylene resin, and the molecular weight of the polypropylene degradable resin is 3000-5000;
the degradation treatment process of the polypropylene resin is as follows:
under the action of a catalyst, initiating polypropylene resin to generate a free radical reaction, controlling the degradation half-life period to be 1h, the degradation temperature to be 137 ℃, the reaction end temperature to be 200 ℃, and the degradation time to be 3h (including the temperature rise time); after degradation, heating to 270 ℃ and preserving heat for 1h, then quickly cooling and discharging to obtain the polypropylene degradation resin with the molecular weight of 3000-plus 5000.
2. The high toughness, low temperature resistant powder coating of claim 1, characterized in that; the catalyst is peroxide bis (tert-butyl peroxide) diisopropylbenzene, and the addition amount is 0.2-0.5% of the mass of the polypropylene resin.
3. The high toughness, low temperature resistant powder coating of claim 1, wherein: the mass ratio of the polypropylene degradation resin to the polyester resin is 3: 3-7.
4. The high toughness, low temperature resistant powder coating of claim 1, wherein: the dosage of the curing agent is 7-8% of the mass of the polyester resin.
5. The high toughness, low temperature resistant powder coating of claim 1, wherein: the curing agent is tris epoxy propyl isocyanurate.
6. The high toughness, low temperature resistant powder coating of claim 1, wherein: the brightener is acrylate copolymer or methacrylate copolymer.
7. The high toughness, low temperature resistant powder coating of claim 1, wherein: the leveling agent is silicon dioxide modified polyacrylate.
8. A high toughness, low temperature resistant powder coating as claimed in any one of claims 1 to 7, characterized by the steps of:
firstly, degrading polypropylene resin to obtain polypropylene degraded resin with the molecular weight of 3000-; and adding the polypropylene degradation resin, the polyester resin, the curing agent, the brightener, the flatting agent, the benzoin, the titanium dioxide, the barium sulfate and the pigment into a mixer, mixing at normal temperature, extruding by an extruder, tabletting by a tablet press, grinding, and sieving by a 200-mesh sieve to obtain the high-toughness low-temperature-resistant powder coating.
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| CN101338009A (en) * | 2007-07-03 | 2009-01-07 | 中国石化上海石油化工股份有限公司 | Method of preparing high fluidity punching proof acrylic resin |
| CN109081894A (en) * | 2018-07-20 | 2018-12-25 | 厦门科艾斯塑胶科技有限公司 | A kind of high fluidity toughener and preparation method thereof |
| CN109988485A (en) * | 2019-03-27 | 2019-07-09 | 广东好彩科技有限公司 | A kind of modified carbon fluoro powder coating |
| CN110183945A (en) * | 2019-05-30 | 2019-08-30 | 上海纳旭实业有限公司 | Low temperature impact heat insulating coat and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338009A (en) * | 2007-07-03 | 2009-01-07 | 中国石化上海石油化工股份有限公司 | Method of preparing high fluidity punching proof acrylic resin |
| CN109081894A (en) * | 2018-07-20 | 2018-12-25 | 厦门科艾斯塑胶科技有限公司 | A kind of high fluidity toughener and preparation method thereof |
| CN109988485A (en) * | 2019-03-27 | 2019-07-09 | 广东好彩科技有限公司 | A kind of modified carbon fluoro powder coating |
| CN110183945A (en) * | 2019-05-30 | 2019-08-30 | 上海纳旭实业有限公司 | Low temperature impact heat insulating coat and preparation method thereof |
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