CN110372847A - A kind of production technology of unglazed thermosetting powder coating special epoxy resin - Google Patents

A kind of production technology of unglazed thermosetting powder coating special epoxy resin Download PDF

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Publication number
CN110372847A
CN110372847A CN201910728453.9A CN201910728453A CN110372847A CN 110372847 A CN110372847 A CN 110372847A CN 201910728453 A CN201910728453 A CN 201910728453A CN 110372847 A CN110372847 A CN 110372847A
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CN
China
Prior art keywords
epoxy resin
unglazed
powder coating
thermosetting powder
parts
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910728453.9A
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Chinese (zh)
Inventor
洪昭雷
吴锡成
王建坤
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HUANGSHAN JINFENG INDUSTRIAL Co Ltd
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HUANGSHAN JINFENG INDUSTRIAL Co Ltd
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Priority to CN201910728453.9A priority Critical patent/CN110372847A/en
Publication of CN110372847A publication Critical patent/CN110372847A/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
    • 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
    • C09D167/00Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • 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

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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)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Epoxy Resins (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention provides a kind of production technology of unglazed thermosetting powder coating special epoxy resin, 100 parts of E-54 base epoxy resins are added in reaction kettle, the sodium hydroxide solution of 1.5 part of 1% concentration is added, the p-tert-butylphenol of 0.4 part of purity 99.5% is added, continue to stir and maintains 175-185 DEG C of duration of kettle temperature 0.5 hour, it opens 0.095MPa vacuum and sloughs moisture content, after 15 minutes, lay down vacuum, open bottom valve, blowing is cooling, broken to get the unglazed thermosetting powder coating special epoxy resin of product.The present invention is by producing a kind of unglazed thermosetting powder coating special epoxy resin, when the unglazed thermosetting powder coating of mixed type prepared with the polyester resin of acid value 42-45mgKOH/g in 4:6 ratio, 30 DEG C are stored 6 months, using effect is without significant change, the smooth exquisiteness of coating, gloss is less than or equal to 2.5 degree, and impact strength 50Kg.m passes through, and 70-80um coating is bent 2mm.

Description

A kind of production technology of unglazed thermosetting powder coating special epoxy resin
Technical field
The present invention relates to epoxy resin production technical field more particularly to a kind of dedicated epoxies of unglazed thermosetting powder coating The production technology of resin.
Background technique
Thermosetting property epoxy flat powder coating is the master for household antitheft door, hardware bin and instrument and meter protected decoration Want coating variety.Currently, thermosetting property epoxy flat powder coating generally uses conventional one-step method E-12 epoxy resin and delustering agent B68 is formulated, and the epoxy flat powder coating that this method is prepared, coating gloss can achieve 2 degree or so, but table substantially Face shows slightly coarse, and impact strength is lower than 40Kg.cm, is bent 3-4mm.Greatest drawback is powdery paints poor storage stability, 30 DEG C Storage just has caking phenomenon for one month, and 30 DEG C of storages are not available for three months substantially.
Therefore, a kind of production technology of unglazed thermosetting powder coating special epoxy resin is invented to solve the above problems very It is necessary to
Summary of the invention
The purpose of the present invention is to provide a kind of production technologies of unglazed thermosetting powder coating special epoxy resin, with solution Certainly above-mentioned technical problem.
The present invention using following technical scheme in order to solve the above technical problems, realized:
A kind of production technology of unglazed thermosetting powder coating special epoxy resin, it by following parts by weight raw material system At: 100 parts of epoxy resin, 43-45 parts of bis-phenol base propane, 1.5-1.7 parts of sodium hydroxide solution and p-tert-butylphenol 0.4-0.6 Part, production technology are as follows: 100 parts of epoxy resin are added in reaction kettle, opens and stirs and heat, are warming up to 80 DEG C, 43- is added 45 parts of bis-phenol base propane maintain agitating and heating to be warming up to 120 DEG C, and 1.5-1.7 parts of sodium hydroxide solutions are added, and continue stirring heating To 150 DEG C, stop heating, enable system automatic heating to 180-185 DEG C of the highest temperature, be again turned on heating, maintains kettle temperature 175-185 DEG C duration 1 hours, 0.4-0.6 parts of p-tert-butylphenols are added, continues to stir and maintains 175-185 DEG C of duration of kettle temperature 0.5 hour, It opens vacuum and sloughs moisture content, after 15 minutes, lay down vacuum, open bottom valve, blowing is cooling, broken to get the unglazed thermosetting property of product Powdery paints special epoxy resin.
Preferably, the epoxy resin is production model E-54 base epoxy resin.
Preferably, the bis-phenol base propane is polymeric carbon grade bis-phenol base propane.
Preferably, the sodium hydroxide solution is the sodium hydroxide solution of 1% concentration.
Preferably, the p-tert-butylphenol is the p-tert-butylphenol of purity 99.5%.
Preferably, blender is provided in the reaction kettle, stirring rate is 55-60 revs/min.
Preferably, the vacuum degree when reaction kettle sloughs moisture content is 0.095MPa.
The beneficial effects of the present invention are:
The present invention by producing a kind of unglazed thermosetting powder coating special epoxy resin, what which had Specific targets are as follows: 90-93 DEG C of softening point, epoxide equivalent 750-800, content of organic chloride 0.0015mol/100g, content of inorganic chlorine 0.0003mol/100g, fugitive constituent are less than or equal to 0.3%, and appearance light yellow clear solid is when poly- with acid value 42-45mgKOH/g In the unglazed thermosetting powder coating of mixed type that 4:6 ratio is prepared, 30 DEG C are stored 6 months ester resin, and using effect becomes without obvious Change, the smooth exquisiteness of coating, gloss is less than or equal to 2.5 degree, and impact strength 50Kg.m passes through, and 70-80um coating is bent 2mm.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below Specific embodiment is closed, the present invention is further explained, and however, the following embodiments are merely preferred embodiments of the present invention, and not all. Based on the implementation example in the implementation mode, those skilled in the art's obtained other realities without making creative work Example is applied, protection scope of the present invention is belonged to.Experimental method in following embodiments is unless otherwise specified conventional method, The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment one:
The present invention provides a kind of production technologies of unglazed thermosetting powder coating special epoxy resin, it is by following weight The raw material of number is made: 100 parts of E-54 base epoxy resin, 43 parts of polymeric carbon grade bis-phenol base propane, the sodium hydroxide of 1% concentration are molten 0.4 part of p-tert-butylphenol of 1.5 parts of liquid and purity 99.5%, production technology are as follows: add 100 parts of E-54 base epoxy resins Enter in reaction kettle, opens stirring rate and be 55-60 revs/min of stirring and heat, be warming up to 80 DEG C, 43 parts of polymeric carbon grade bis-phenols are added Base propane maintains agitating and heating to be warming up to 120 DEG C, and the sodium hydroxide solution of 1.5 part of 1% concentration is added, and continues stirring and is warming up to 150 DEG C, stop heating, enable system automatic heating to 180-185 DEG C of the highest temperature, be again turned on heating, maintains 175-185 DEG C of kettle temperature Duration 1 hour, the p-tert-butylphenol of 0.4 part of purity 99.5% is added, continue to stir and maintains 175-185 DEG C of duration of kettle temperature It 0.5 hour, opens 0.095MPa vacuum and sloughs moisture content, after 15 minutes, lay down vacuum, open bottom valve, blowing is cooling, broken, i.e., Obtain the unglazed thermosetting powder coating special epoxy resin of product.
The mixed type prepared with the polyester resin of the epoxy resin of the proportion and acid value 42-45mgKOH/g in 4:6 ratio without Light thermosetting powder coating, using electrostatic spraying or Typical spray method spraying household antitheft door, hardware bin or instrument and meter The coating of the epoxy powder coating of 70-80um thickness is prepared in protected decoration surface, carries out performance detection to the product, Performance test results are as shown in the table:
Embodiment two:
The present invention provides a kind of production technologies of unglazed thermosetting powder coating special epoxy resin, it is by following weight The raw material of number is made: 100 parts of E-54 base epoxy resin, 44 parts of polymeric carbon grade bis-phenol base propane, the sodium hydroxide of 1% concentration are molten 0.5 part of p-tert-butylphenol of 1.6 parts of liquid and purity 99.5%, production technology are as follows: add 100 parts of E-54 base epoxy resins Enter in reaction kettle, opens stirring rate and be 55-60 revs/min of stirring and heat, be warming up to 80 DEG C, 44 parts of polymeric carbon grade bis-phenols are added Base propane maintains agitating and heating to be warming up to 120 DEG C, and the sodium hydroxide solution of 1.6 part of 1% concentration is added, and continues stirring and is warming up to 150 DEG C, stop heating, enable system automatic heating to 180-185 DEG C of the highest temperature, be again turned on heating, maintains 175-185 DEG C of kettle temperature Duration 1 hour, the p-tert-butylphenol of 0.5 part of purity 99.5% is added, continue to stir and maintains 175-185 DEG C of duration of kettle temperature It 0.5 hour, opens 0.095MPa vacuum and sloughs moisture content, after 15 minutes, lay down vacuum, open bottom valve, blowing is cooling, broken, i.e., Obtain the unglazed thermosetting powder coating special epoxy resin of product.
The mixed type prepared with the polyester resin of the epoxy resin of the proportion and acid value 42-45mgKOH/g in 4:6 ratio without Light thermosetting powder coating, using electrostatic spraying or Typical spray method spraying household antitheft door, hardware bin or instrument and meter The coating of the epoxy powder coating of 70-80um thickness is prepared in protected decoration surface, carries out performance detection to the product, Performance test results are as shown in the table:
Embodiment three:
The present invention provides a kind of production technologies of unglazed thermosetting powder coating special epoxy resin, it is by following weight The raw material of number is made: 100 parts of E-54 base epoxy resin, 45 parts of polymeric carbon grade bis-phenol base propane, the sodium hydroxide of 1% concentration are molten 0.6 part of p-tert-butylphenol of 1.7 parts of liquid and purity 99.5%, production technology are as follows: add 100 parts of E-54 base epoxy resins Enter in reaction kettle, opens stirring rate and be 55-60 revs/min of stirring and heat, be warming up to 80 DEG C, 45 parts of polymeric carbon grade bis-phenols are added Base propane maintains agitating and heating to be warming up to 120 DEG C, and the sodium hydroxide solution of 1.7 part of 1% concentration is added, and continues stirring and is warming up to 150 DEG C, stop heating, enable system automatic heating to 180-185 DEG C of the highest temperature, be again turned on heating, maintains 175-185 DEG C of kettle temperature Duration 1 hour, the p-tert-butylphenol of 0.6 part of purity 99.5% is added, continue to stir and maintains 175-185 DEG C of duration of kettle temperature It 0.5 hour, opens 0.095MPa vacuum and sloughs moisture content, after 15 minutes, lay down vacuum, open bottom valve, blowing is cooling, broken, i.e., Obtain the unglazed thermosetting powder coating special epoxy resin of product.
The mixed type prepared with the polyester resin of the epoxy resin of the proportion and acid value 42-45mgKOH/g in 4:6 ratio without Light thermosetting powder coating, using electrostatic spraying or Typical spray method spraying household antitheft door, hardware bin or instrument and meter The coating of the epoxy powder coating of 70-80um thickness is prepared in protected decoration surface, carries out performance detection to the product, Performance test results are as shown in the table:
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry For personnel it should be appreciated that the present invention is not limited to the above embodiments, described in the above embodiment and specification is only the present invention Preference, be not intended to limit the invention, without departing from the spirit and scope of the present invention, the present invention also has various Changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by institute Attached claims and its equivalent thereof.

Claims (7)

1. a kind of production technology of unglazed thermosetting powder coating special epoxy resin, which is characterized in that it is by following parts by weight Several raw materials are made: 100 parts of epoxy resin, 43-45 parts of bis-phenol base propane, 1.5-1.7 parts of sodium hydroxide solution and to tert-butyl 0.4-0.6 parts of phenol, production technology are as follows: 100 parts of epoxy resin are added in reaction kettle, opens and stirs and heat, be warming up to 80 DEG C, 43-45 parts of bis-phenol base propane are added, agitating and heating is maintained to be warming up to 120 DEG C, 1.5-1.7 parts of sodium hydroxide solutions are added, Continue stirring and be warming up to 150 DEG C, stop heating, enable system automatic heating to 180-185 DEG C of the highest temperature, be again turned on heating, ties up It holds 175-185 DEG C of duration of kettle temperature 1 hour, 0.4-0.6 parts of p-tert-butylphenols is added, continues to stir and maintains kettle temperature 175-185 DEG C duration 0.5 hour, open vacuum and slough moisture content, after 15 minutes, lay down vacuum, open bottom valve, blowing is cooling, it is broken to get Product is unglazed thermosetting powder coating special epoxy resin.
2. a kind of production technology of unglazed thermosetting powder coating special epoxy resin according to claim 1, feature Be: the epoxy resin is production model E-54 base epoxy resin.
3. a kind of production technology of unglazed thermosetting powder coating special epoxy resin according to claim 1, feature Be: the bis-phenol base propane is polymeric carbon grade bis-phenol base propane.
4. a kind of production technology of unglazed thermosetting powder coating special epoxy resin according to claim 1, feature Be: the sodium hydroxide solution is the sodium hydroxide solution of 1% concentration.
5. a kind of production technology of unglazed thermosetting powder coating special epoxy resin according to claim 1, feature Be: the p-tert-butylphenol is the p-tert-butylphenol of purity 99.5%.
6. a kind of production technology of unglazed thermosetting powder coating special epoxy resin according to claim 1, feature It is: is provided with blender in the reaction kettle, stirring rate is 55-60 revs/min.
7. a kind of production technology of unglazed thermosetting powder coating special epoxy resin according to claim 1, feature Be: the vacuum degree when reaction kettle sloughs moisture content is 0.095MPa.
CN201910728453.9A 2019-08-08 2019-08-08 A kind of production technology of unglazed thermosetting powder coating special epoxy resin Pending CN110372847A (en)

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CN201910728453.9A CN110372847A (en) 2019-08-08 2019-08-08 A kind of production technology of unglazed thermosetting powder coating special epoxy resin

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Application Number Priority Date Filing Date Title
CN201910728453.9A CN110372847A (en) 2019-08-08 2019-08-08 A kind of production technology of unglazed thermosetting powder coating special epoxy resin

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5714264A (en) * 1995-10-18 1998-02-03 Basf Lacke & Farben, Ag Aqueous powder coating dispersion for packaging containers
CN101864057A (en) * 2010-05-10 2010-10-20 宏昌电子材料股份有限公司 Epoxy resin used for powder coating and preparation method thereof
CN103068941A (en) * 2010-06-23 2013-04-24 陶氏环球技术有限责任公司 Powder coatings compositions
CN109836584A (en) * 2017-11-29 2019-06-04 中国石油化工股份有限公司 A kind of modified bisphenol A type solid epoxy and its synthetic method and the application in low damp luminosity powdery paints

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5714264A (en) * 1995-10-18 1998-02-03 Basf Lacke & Farben, Ag Aqueous powder coating dispersion for packaging containers
CN101864057A (en) * 2010-05-10 2010-10-20 宏昌电子材料股份有限公司 Epoxy resin used for powder coating and preparation method thereof
CN103068941A (en) * 2010-06-23 2013-04-24 陶氏环球技术有限责任公司 Powder coatings compositions
CN109836584A (en) * 2017-11-29 2019-06-04 中国石油化工股份有限公司 A kind of modified bisphenol A type solid epoxy and its synthetic method and the application in low damp luminosity powdery paints

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Application publication date: 20191025

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