CN109627427A - A kind of preparation method of low viscosity epoxy resin and super levelling powdery paints - Google Patents

A kind of preparation method of low viscosity epoxy resin and super levelling powdery paints Download PDF

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Publication number
CN109627427A
CN109627427A CN201811374079.9A CN201811374079A CN109627427A CN 109627427 A CN109627427 A CN 109627427A CN 201811374079 A CN201811374079 A CN 201811374079A CN 109627427 A CN109627427 A CN 109627427A
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China
Prior art keywords
epoxy resin
low viscosity
viscosity epoxy
preparation
powdery paints
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Pending
Application number
CN201811374079.9A
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Chinese (zh)
Inventor
张海瑞
孙彬
丁树国
徐煜慧
赵金祥
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Tianjin Xiangsheng New Materials Co Ltd
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Tianjin Xiangsheng New Materials Co Ltd
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Priority to CN201811374079.9A priority Critical patent/CN109627427A/en
Publication of CN109627427A publication Critical patent/CN109627427A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/62Alcohols or phenols
    • C08G59/621Phenols
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03Powdery paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03Powdery paints
    • C09D5/033Powdery paints characterised by the additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention relates to a kind of preparation methods of low viscosity epoxy resin, steps are as follows: 150-180 part by weight of liquid epoxy resin is added, 120-130 DEG C is warming up in mechanical stirring, 65-90 parts by weight of bisphenol A is added, after epoxy resin and bisphenol-A complete miscibility, temperature is controlled in 130 ± 2 DEG C of addition quaternary ammonium salt catalyst, at 150-160 DEG C after reaction 2-3 hours, reaction product is poured out, it is cooling to get low viscosity epoxy resin.The low viscosity epoxy resin of the method for the present invention preparation is remarkably improved levelability, glossiness and the richness of powdery paints, has very strong decorative performance and practical value.Production process is simple, does not generate the three wastes, meets national requirements for environmental protection, is conducive to realize industrialization.

Description

A kind of preparation method of low viscosity epoxy resin and super levelling powdery paints
Technical field
The invention belongs to technical field of coatings, are related to super levelling powdery paints, especially a kind of low viscosity epoxy resin Preparation method and its super levelling powdery paints.
Background technique
Attention with people and policy to environmental protection, traditional oil paint paint industry turn to more ring more and more Protect powdery paints.Powdery paints is a kind of powdered form coating of solid point 100%, is free of solvent and toxic and volatile substances, is A kind of coating of energy conservation and environmental protection, function admirable.It is preferable to be formed by coating compactness, adhesive force, impact strength and toughness. But powdery paints, since resin viscosity used is larger, its levelling of the film of formation and gloss are difficult to match in excellence or beauty with paint, limit Much applications of the industry more demanding to decorative performance.
By retrieval, patent publication us CN201410188126.6 discloses a kind of household electrical appliance with super levelability Powdery paints and its production method, it is the production method using common E-12 type epoxy resin addition flow improver additive.Specially Sharp open source literature 201110138155.8 discloses a kind of super leveling mirror surface powder coating, it be using modified polyurethane resin and Phenol aldehyde modified crosslinking agent preparation.
By comparison, there is essential difference in present patent application and above-mentioned patent publication us.
Summary of the invention
Place that the purpose of the present invention is to overcome the deficiency in the prior art, provides a kind of preparation method of low viscosity epoxy resin And super levelling powdery paints, it is demanding that low viscosity epoxy resin made from this method is mainly used in the gentle luster performance of convection current Decorative powder coatings is remarkably improved levelability, glossiness and the richness of powdery paints, have very strong decorative performance and Practical value.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of low viscosity epoxy resin, steps are as follows:
150-180 part by weight of liquid epoxy resin is added, 120-130 DEG C is warming up in mechanical stirring, 65-90 weight is added Part bisphenol-A is measured, after epoxy resin and bisphenol-A complete miscibility, temperature is controlled at 130 ± 2 DEG C, quaternary ammonium salt catalysis is added After reaction 2-3 hours, reaction product is poured out at 150-160 DEG C for agent, cooling to get low viscosity epoxy resin.
Moreover, the liquid epoxies is bisphenol f type epoxy resin, epoxide equivalent 160-180g/eq, viscosity is 700-1200cps@25℃。
Moreover, the parts by weight of the quaternary ammonium salt catalyst addition are 0.07-0.2 parts.
Moreover, the equal relative molecular mass of the number of the low viscosity epoxy resin is 2500-4500, epoxide equivalent 780- 950g/eq。
The super levelling powder of low viscosity epoxy resin made from preparation method using low viscosity epoxy resin as described above Last coating, constituent and its parts by weight are as follows:
Moreover, the polyester resin is terminal carboxyl polyester resin, acid value 47-51mgKOH/g, viscosity 2500- 3000mPa.s@200℃。
Moreover, the pigments and fillers are made of bloom barium sulfate, rutile type titanium white and inorganic pigment.
Moreover, the auxiliary agent is the mixture of levelling agent, anti-interference agent and degasser.
Low viscosity epoxy resin made from the preparation method of low viscosity epoxy resin as described above is applied in super levelling powder Application in material preparation aspect.
Moreover, the low viscosity epoxy resin can significantly improve the levelability of super levelling powdery paints, glossiness and rich Full scale.
The advantages of present invention obtains and good effect are as follows:
1, low viscosity epoxy resin made from the method for the present invention has the characteristics that intermediate molecular weight, low viscosity, party's legal system The low viscosity epoxy resin obtained can be applied in the demanding decorative powder coatings of the gentle luster performance of convection current, can significantly mention Levelability, glossiness and the richness of high powdery paints have very strong decorative performance and practical value.
2, the method for the present invention prepare low viscosity epoxy resin production process it is simple, do not generate the three wastes, meet national environmental protection It is required that being conducive to realize industrialization.
3, low viscosity epoxy resin viscosity made from the method for the present invention is lower, molecular weight is higher, is remarkably improved powder painting The levelability and glossiness of material, while the mechanical performance of powdery paints coating is also improved, there is very strong use value.
4, this super levelling powdery paints when film is relatively thin (50-60) μm, still can get excellent levelability, glossiness and Richness had not only reduced cost but also had improved performance, had very strong application prospect.
Specific embodiment
The embodiment of the present invention is described in detail below, it should be noted that the present embodiment is narrative, is not limited , this does not limit the scope of protection of the present invention.
Raw material used in the present invention is unless otherwise specified conventional commercial product;Used in the present invention Method is unless otherwise specified the conventional method of this field.
Embodiment 1
A kind of preparation method of low viscosity epoxy resin, steps are as follows:
160 part by weight of liquid epoxy resin are added in three-necked flask, is warming up to 120-130 DEG C in mechanical stirring, adds Enter 72 parts by weight of bisphenol A, after epoxy resin and bisphenol-A complete miscibility, temperature is controlled at 130 ± 2 DEG C, quaternary ammonium salt is added Reaction product is poured out three-necked flask after 150-160 DEG C is reacted 3 hours by catalyst, cooling to get low viscosity epoxy resin.
The super levelling powder of low viscosity epoxy resin made from preparation method using low viscosity epoxy resin as described above Last coating, constituent and its parts by weight are as follows:
Embodiment 2
A kind of preparation method of low viscosity epoxy resin, steps are as follows:
170 part by weight of liquid epoxy resin are added in three-necked flask, is warming up to 120-130 DEG C in mechanical stirring, adds Enter 80 parts by weight of bisphenol A, after epoxy resin and bisphenol-A complete miscibility, temperature is controlled at 130 ± 2 DEG C, quaternary ammonium salt is added Reaction product is poured out three-necked flask after reacting 2.5 hours at 150-160 DEG C by catalyst, cooling to get low viscosity epoxy tree Rouge.
More preferably, the liquid epoxies is bisphenol f type epoxy resin, epoxide equivalent (160-180) g/eq, viscosity (700-1200)cps@25℃。
Super levelling powdery paints, constituent made from preparation method using low viscosity epoxy resin as described above And its parts by weight are as follows:
More preferably, the polyester resin is end carboxyl end group type polyester resin, acid value 47-51mgKOH/g, viscosity (2500- 3000)mPa.s@200℃。
More preferably, the pigments and fillers are made of bloom barium sulfate, rutile type titanium white and inorganic pigment.
More preferably, other auxiliary agents are the mixture of levelling agent, anti-interference agent and degasser.
Embodiment 3
A kind of preparation method of low viscosity epoxy resin, steps are as follows:
165 part by weight of liquid epoxy resin are added in three-necked flask, is warming up to 120-130 DEG C in mechanical stirring, adds Enter 83 parts by weight of bisphenol A, after epoxy resin and bisphenol-A complete miscibility, temperature is controlled in 130 ± 2 DEG C of addition quaternary ammonium salts Reaction product is poured out three-necked flask after reacting 2.5 hours at 150-160 DEG C by catalyst, cooling to get low viscosity epoxy tree Rouge.
More preferably, the liquid epoxies is bisphenol f type epoxy resin, epoxide equivalent (160-180) g/eq, viscosity (700-1200)cps@25℃。
More preferably, the parts by weight of the quaternary ammonium salt catalyst addition are 0.07-0.2 parts;
The equal relative molecular mass of the number of the low viscosity epoxy resin is 2500-4500, and epoxide equivalent is (780-950) g/ eq。
Super levelling powdery paints, constituent made from preparation method using low viscosity epoxy resin as described above And its parts by weight are as follows:
More preferably, the polyester resin is end carboxyl end group type polyester resin, acid value 47-51mgKOH/g, viscosity (2500- 3000)mPa.s@200℃。
More preferably, the pigments and fillers are made of bloom barium sulfate, rutile type titanium white and inorganic pigment.
More preferably, the auxiliary agent is the mixture of levelling agent, anti-interference agent and degasser.
Low viscosity epoxy resin made from the preparation method of low viscosity epoxy resin of the present invention is in super levelling powdery paints Application.
More preferably, the low viscosity epoxy resin can significantly improve levelability, glossiness and the richness of powdery paints.
The related test results of powdery paints of the present invention:
1, powdery paints of the present invention has passed through SGS certification, Halogen certification, ROHS certification etc., toxicity and heavy metal analysis Meet sanitary standard.
2, the technical target of the product and detection method of powdery paints of the present invention:
1) gloss: >=94% (60 °)
2) appearance: the defects of without orange peel, pin hole
3) water resistance: tap water impregnates one month without the bad phenomenons such as blistering softening that fall off that fade;
4) acid resistance: the immersion of 3% hydrochloric acid solution 240 hours without exception;
5) alkali resistance: the immersion of 5% sodium hydroxide solution 168 hours without exception;
6) adhesive force: standard GB9286, tool use cross-cut tester, brush, adhesive tape, magnifying glass;Testing result: 0-2 grades;
7) impact resistance: 50kg.cm flawless.
The above result shows that both using super levelling powdery paints made from low viscosity epoxy resin made from the method for the present invention With excellent levelability, glossiness and richness, and there is excellent chemical moral character and mechanical performance, coating can be substantially reduced Cost has very strong application prospect.
Although disclosing the embodiment of the present invention for the purpose of illustration, it will be appreciated by those skilled in the art that: not Be detached from the present invention and spirit and scope of the appended claims in, various substitutions, changes and modifications be all it is possible, therefore, this The range of invention is not limited to the embodiment disclosure of that.

Claims (10)

1. a kind of preparation method of low viscosity epoxy resin, it is characterised in that: steps are as follows:
150-180 part by weight of liquid epoxy resin is added, 120-130 DEG C is warming up in mechanical stirring, 65-90 parts by weight are added Temperature is controlled at 130 ± 2 DEG C after epoxy resin and bisphenol-A complete miscibility, quaternary ammonium salt catalyst is added by bisphenol-A, 150-160 DEG C after reaction 2-3 hours, reaction product is poured out, cooling to get low viscosity epoxy resin.
2. the preparation method of low viscosity epoxy resin according to claim 1, it is characterised in that: the liquid epoxies For bisphenol f type epoxy resin, epoxide equivalent 160-180g/eq, viscosity is 25 DEG C of 700-1200cps@.
3. the preparation method of low viscosity epoxy resin according to claim 1, it is characterised in that: the quaternary ammonium salt catalysis The parts by weight of agent addition are 0.07-0.2 parts.
4. the preparation method of low viscosity epoxy resin according to any one of claims 1 to 3, it is characterised in that: described low The equal relative molecular mass of the number of viscosity epoxy is 2500-4500, epoxide equivalent 780-950g/eq.
5. utilizing the low viscosity epoxy as made from the preparation method of the described in any item low viscosity epoxy resins of Claims 1-4 The super levelling powdery paints of resin, it is characterised in that: its constituent and its parts by weight are as follows:
6. low viscosity epoxy resin made from the preparation method according to claim 5 using low viscosity epoxy resin is super Levelling powdery paints, it is characterised in that: the polyester resin is terminal carboxyl polyester resin, and acid value 47-51mgKOH/g, viscosity is 2500-3000mPa.s@200℃。
7. low viscosity epoxy resin made from the preparation method according to claim 5 using low viscosity epoxy resin is super Levelling powdery paints, it is characterised in that: the pigments and fillers are made of bloom barium sulfate, rutile type titanium white and inorganic pigment.
8. according to low viscosity ring made from the described in any item preparation methods using low viscosity epoxy resin of claim 5 to 7 The super levelling powdery paints of oxygen resin, it is characterised in that: the auxiliary agent is the mixture of levelling agent, anti-interference agent and degasser.
9. the low viscosity epoxy resin as made from the preparation method of the described in any item low viscosity epoxy resins of Claims 1-4 Application in terms of the super levelling powdery paints preparation.
10. low viscosity epoxy resin made from the preparation method of low viscosity epoxy resin according to claim 9 is in super stream Application in flat powdery paints preparation aspect, it is characterised in that: the low viscosity epoxy resin can significantly improve super levelling powder Levelability, glossiness and the richness of last coating.
CN201811374079.9A 2018-11-19 2018-11-19 A kind of preparation method of low viscosity epoxy resin and super levelling powdery paints Pending CN109627427A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115894862A (en) * 2022-12-16 2023-04-04 江苏扬农锦湖化工有限公司 Low-viscosity TOFA modified epoxy resin and preparation method thereof

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86100991A (en) * 1985-02-08 1986-08-20 采煤化学公司 With Resins, epoxy and carboxy(l)polyester is the preparation method of the powder coating of main component
US4722981A (en) * 1986-02-14 1988-02-02 The Dow Chemical Company Epoxy resins of controlled conversion and a process for their preparation
CN1175265A (en) * 1995-02-10 1998-03-04 陶氏化学公司 Epoxy resin composition capable of cure at low temperature
CN1498910A (en) * 2002-11-11 2004-05-26 西北工业大学 Resinoid phenols solidified agent and preparation method
CN102070974A (en) * 2010-12-07 2011-05-25 中国电器科学研究院 Powder coating for strengthening cross-contamination resistance and preparation method thereof
CN102504671A (en) * 2011-10-27 2012-06-20 西安大禾化工材料有限公司 Anticorrosion energy-saving type curing agent for rapidly curing epoxy powder coating at low temperature and preparation method thereof
CN106589319A (en) * 2016-11-22 2017-04-26 天津翔盛新材料有限公司 Four-functional-group super-flexible linear phenolic curing agent dedicated for heavy-duty anticorrosive powder coating, and synthetic method and application thereof
CN106750187A (en) * 2016-11-22 2017-05-31 天津翔盛新材料有限公司 A kind of heavy corrosion protection epoxy powder high tenacity phenols curing agent and preparation method and application
CN107298926A (en) * 2017-08-16 2017-10-27 吴丹 A kind of coating curing agent

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86100991A (en) * 1985-02-08 1986-08-20 采煤化学公司 With Resins, epoxy and carboxy(l)polyester is the preparation method of the powder coating of main component
US4722981A (en) * 1986-02-14 1988-02-02 The Dow Chemical Company Epoxy resins of controlled conversion and a process for their preparation
CN1175265A (en) * 1995-02-10 1998-03-04 陶氏化学公司 Epoxy resin composition capable of cure at low temperature
CN1498910A (en) * 2002-11-11 2004-05-26 西北工业大学 Resinoid phenols solidified agent and preparation method
CN102070974A (en) * 2010-12-07 2011-05-25 中国电器科学研究院 Powder coating for strengthening cross-contamination resistance and preparation method thereof
CN102504671A (en) * 2011-10-27 2012-06-20 西安大禾化工材料有限公司 Anticorrosion energy-saving type curing agent for rapidly curing epoxy powder coating at low temperature and preparation method thereof
CN106589319A (en) * 2016-11-22 2017-04-26 天津翔盛新材料有限公司 Four-functional-group super-flexible linear phenolic curing agent dedicated for heavy-duty anticorrosive powder coating, and synthetic method and application thereof
CN106750187A (en) * 2016-11-22 2017-05-31 天津翔盛新材料有限公司 A kind of heavy corrosion protection epoxy powder high tenacity phenols curing agent and preparation method and application
CN107298926A (en) * 2017-08-16 2017-10-27 吴丹 A kind of coating curing agent

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115894862A (en) * 2022-12-16 2023-04-04 江苏扬农锦湖化工有限公司 Low-viscosity TOFA modified epoxy resin and preparation method thereof

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Application publication date: 20190416