CN112724794A - Imidazolyl-modified epoxy resin paint and preparation method thereof - Google Patents

Imidazolyl-modified epoxy resin paint and preparation method thereof Download PDF

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Publication number
CN112724794A
CN112724794A CN202011580844.XA CN202011580844A CN112724794A CN 112724794 A CN112724794 A CN 112724794A CN 202011580844 A CN202011580844 A CN 202011580844A CN 112724794 A CN112724794 A CN 112724794A
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parts
epoxy resin
imidazolyl
modified epoxy
tert
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沈岳
伍宽平
吕宏飞
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Shanghai Handai Chemical Co ltd
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Shanghai Handai Chemical Co ltd
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    • 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
    • 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
    • C08G59/50Amines
    • C08G59/5046Amines heterocyclic
    • C08G59/5053Amines heterocyclic containing only nitrogen as a heteroatom
    • C08G59/5073Amines heterocyclic containing only nitrogen as a heteroatom having two nitrogen atoms in the ring
    • 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/327Aluminium phosphate

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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)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses an imidazolyl group modified epoxy resin paint and a preparation method thereof, wherein the method comprises the following steps: adding bisphenol F type epoxy resin into aluminum tripolyphosphate and 1, 3-propylene glycol dibutyrate under the pressure of 0.1-0.2MPa, heating to 55-60 ℃, and stirring for reaction; adding mica powder and tert-butyl dimethyl alkyl imidazole, heating to 62-65 deg.C, and heating while stirring; adding polyalcohol, and stirring for 1-4 hr. Tert-butyl dimethyl alkyl imidazole is used for modification, and imidazolyl is introduced into an epoxy resin curing system to form a net structure, so that the adhesive force is improved.

Description

Imidazolyl-modified epoxy resin paint and preparation method thereof
Technical Field
The invention belongs to the field of coatings, and particularly relates to an imidazolyl-modified epoxy resin paint and a preparation method thereof.
Background
The epoxy resin is a high molecular polymer, has a molecular formula of (C11H12O3) n, and is a general name of a polymer containing more than two epoxy groups in a molecule. It is a polycondensation product of epichlorohydrin and bisphenol A or a polyol. Because of the chemical activity of the epoxy group, the epoxy group can be opened by a plurality of compounds containing active hydrogen, and the epoxy group is cured and crosslinked to form a network structure, so that the epoxy group is a thermosetting resin.
Chinese patent application No. CN201210594347.4 discloses an epoxy resin coating, the composition components include the following components: epoxy resin, a curing agent, zinc phosphate, aluminum tripolyphosphate and composite ferrotitanium. The composite iron-titanium filled epoxy resin coating shows excellent corrosion resistance in a KCL solution with the temperature of 60 ℃, the pressure of 1.8MPa and the concentration of 5%. But the adhesive force is general and easy to fall off.
Disclosure of Invention
The invention provides an imidazole-based modified epoxy resin paint and a preparation method thereof, aiming at solving the problems of the prior art, and the imidazole-based modified epoxy resin paint has strong adhesive force and is not easy to peel off.
In order to solve the technical problems, the invention adopts the following technical scheme:
the imidazolyl group modified epoxy resin paint comprises the following raw materials in parts by weight: 70-90 parts of bisphenol F type epoxy resin, 3-5 parts of aluminum tripolyphosphate, 30-40 parts of 1, 3-propylene glycol dibutyrate, 30-80 parts of polyhydric alcohol, 1-4 parts of mica powder and 5-10 parts of tert-butyl dimethyl alkyl imidazole.
Preferably, the imidazolyl-modified epoxy resin paint comprises the following raw materials in parts by weight: 80 parts of bisphenol F type epoxy resin, 4 parts of aluminum tripolyphosphate, 35 parts of 1, 3-propylene glycol dibutyrate, 50 parts of polyhydric alcohol, 3 parts of mica powder and 8 parts of tert-butyl dimethyl alkyl imidazole.
Preferably, the imidazolyl-modified epoxy resin paint comprises the following raw materials in parts by weight: 70 parts of bisphenol F epoxy resin, 3 parts of aluminum tripolyphosphate, 30 parts of 1, 3-propylene glycol dibutyrate, 30 parts of polyhydric alcohol, 1 part of mica powder and 5 parts of tert-butyl dimethyl alkyl imidazole.
Preferably, the imidazolyl-modified epoxy resin paint comprises the following raw materials in parts by weight: 90 parts of bisphenol F epoxy resin, 5 parts of aluminum tripolyphosphate, 40 parts of 1, 3-propylene glycol dibutyrate, 80 parts of polyhydric alcohol, 4 parts of mica powder and 10 parts of tert-butyl dimethyl alkyl imidazole.
Preferably, the imidazolyl-modified epoxy resin paint comprises the following raw materials in parts by weight: 77 parts of bisphenol F epoxy resin, 5 parts of aluminum tripolyphosphate, 34 parts of 1, 3-propylene glycol dibutyrate, 40 parts of polyhydric alcohol, 2 parts of mica powder and 7 parts of tert-butyl dimethyl alkyl imidazole.
Preferably, the polyol is one or more of 1, 2-propanediol, 1, 3-propanediol or 1, 4-propanediol.
The preparation method of the imidazolyl group modified epoxy resin paint comprises the following steps: adding bisphenol F type epoxy resin into aluminum tripolyphosphate and 1, 3-propylene glycol dibutyrate under the pressure of 0.1-0.2MPa, heating to 55-60 ℃, and stirring for reaction; adding mica powder and tert-butyl dimethyl alkyl imidazole, heating to 62-65 deg.C, and heating while stirring; adding polyalcohol, and stirring for 1-4 hr.
The stirring speed was 700 and 800 rpm.
The invention has the following beneficial effects: tert-butyl dimethyl alkyl imidazole is used for modification, and imidazolyl is introduced into an epoxy resin curing system to form a net structure, so that the adhesive force is improved.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
The imidazolyl group modified epoxy resin paint comprises the following raw materials in parts by weight: 80 parts of bisphenol F type epoxy resin, 4 parts of aluminum tripolyphosphate, 35 parts of 1, 3-propylene glycol dibutyrate, 50 parts of polyhydric alcohol, 3 parts of mica powder and 8 parts of tert-butyl dimethyl alkyl imidazole.
The polyhydric alcohol is 1, 2-propylene glycol and 1, 3-propylene glycol in a mass ratio of 1: 1.
The preparation method of the imidazolyl group modified epoxy resin paint comprises the following steps: adding bisphenol F type epoxy resin into aluminum tripolyphosphate and 1, 3-propylene glycol dibutyrate under the pressure of 0.1-0.2MPa, heating to 55-60 ℃, and stirring at the speed of 750rpm for reaction; adding mica powder and tert-butyl dimethyl alkyl imidazole, heating to 62-65 deg.C, and heating while stirring; adding polyalcohol, and stirring for 3 hr.
Example 2
The imidazolyl group modified epoxy resin paint comprises the following raw materials in parts by weight: 70 parts of bisphenol F epoxy resin, 3 parts of aluminum tripolyphosphate, 30 parts of 1, 3-propylene glycol dibutyrate, 30 parts of polyhydric alcohol, 1 part of mica powder and 5 parts of tert-butyl dimethyl alkyl imidazole.
The polyalcohol is 1, 2-propylene glycol, a mixture of 1, 3-propylene glycol and 1, 4-propylene glycol in a mass ratio of 1:3: 5.
The preparation method of the imidazolyl group modified epoxy resin paint comprises the following steps: adding bisphenol F type epoxy resin into aluminum tripolyphosphate and 1, 3-propylene glycol dibutyrate under the pressure of 0.1-0.2MPa, heating to 55-60 ℃, and stirring for reaction at the stirring speed of 700 rpm; adding mica powder and tert-butyl dimethyl alkyl imidazole, heating to 62-65 deg.C, and heating while stirring; adding polyalcohol, and stirring for 1 hr.
Example 3
The imidazolyl group modified epoxy resin paint comprises the following raw materials in parts by weight: 90 parts of bisphenol F epoxy resin, 5 parts of aluminum tripolyphosphate, 40 parts of 1, 3-propylene glycol dibutyrate, 80 parts of polyhydric alcohol, 4 parts of mica powder and 10 parts of tert-butyl dimethyl alkyl imidazole.
The polyhydric alcohol is 1, 4-propylene glycol.
The preparation method of the imidazolyl group modified epoxy resin paint comprises the following steps: adding bisphenol F type epoxy resin into aluminum tripolyphosphate and 1, 3-propylene glycol dibutyrate under the pressure of 0.1-0.2MPa, heating to 55-60 ℃, and stirring for reaction at the stirring speed of 800 rpm; adding mica powder and tert-butyl dimethyl alkyl imidazole, heating to 62-65 deg.C, and heating while stirring; adding polyalcohol, and stirring for 4 hr.
Example 4
The imidazolyl group modified epoxy resin paint comprises the following raw materials in parts by weight: 77 parts of bisphenol F epoxy resin, 5 parts of aluminum tripolyphosphate, 34 parts of 1, 3-propylene glycol dibutyrate, 40 parts of polyhydric alcohol, 2 parts of mica powder and 7 parts of tert-butyl dimethyl alkyl imidazole.
The polyhydric alcohol is 1, 2-propylene glycol.
The preparation method of the imidazolyl group modified epoxy resin paint comprises the following steps: adding bisphenol F type epoxy resin into aluminum tripolyphosphate and 1, 3-propylene glycol dibutyrate under the pressure of 0.1-0.2MPa, heating to 55-60 ℃, and stirring for reaction at the stirring speed of 780 rpm; adding mica powder and tert-butyl dimethyl alkyl imidazole, heating to 62-65 deg.C, and heating while stirring; adding polyalcohol, and stirring for 2 hr.
Comparative example 1
The difference from example 1 is that: t-butyl dimethyl alkyl imidazole was not added.
Uniformly coating the paint film on a base material, wherein the drying temperature is 80 ℃, and the performance is measured:
Figure BDA0002864955210000031
Figure BDA0002864955210000041
as can be seen from the table, the invention has no peeling at the edge, smooth cut edge and very good adhesive force, because the tert-butyl dimethyl alkyl imidazole is used for modification, and the imidazolyl is introduced into an epoxy resin curing system to form a net structure, thereby improving the adhesive force.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, and any simple changes or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention are within the scope of the present invention.

Claims (8)

1. The imidazolyl group modified epoxy resin paint is characterized by comprising the following raw materials in parts by weight: 70-90 parts of bisphenol F type epoxy resin, 3-5 parts of aluminum tripolyphosphate, 30-40 parts of 1, 3-propylene glycol dibutyrate, 30-80 parts of polyhydric alcohol, 1-4 parts of mica powder and 5-10 parts of tert-butyl dimethyl alkyl imidazole.
2. The imidazolyl-modified epoxy resin paint of claim 1, which comprises the following raw materials in parts by weight: 80 parts of bisphenol F type epoxy resin, 4 parts of aluminum tripolyphosphate, 35 parts of 1, 3-propylene glycol dibutyrate, 50 parts of polyhydric alcohol, 3 parts of mica powder and 8 parts of tert-butyl dimethyl alkyl imidazole.
3. The imidazolyl-modified epoxy resin paint of claim 1, which comprises the following raw materials in parts by weight: 70 parts of bisphenol F epoxy resin, 3 parts of aluminum tripolyphosphate, 30 parts of 1, 3-propylene glycol dibutyrate, 30 parts of polyhydric alcohol, 1 part of mica powder and 5 parts of tert-butyl dimethyl alkyl imidazole.
4. The imidazolyl-modified epoxy resin paint of claim 1, which comprises the following raw materials in parts by weight: 90 parts of bisphenol F epoxy resin, 5 parts of aluminum tripolyphosphate, 40 parts of 1, 3-propylene glycol dibutyrate, 80 parts of polyhydric alcohol, 4 parts of mica powder and 10 parts of tert-butyl dimethyl alkyl imidazole.
5. The imidazolyl-modified epoxy resin paint of claim 1, which comprises the following raw materials in parts by weight: 77 parts of bisphenol F epoxy resin, 5 parts of aluminum tripolyphosphate, 34 parts of 1, 3-propylene glycol dibutyrate, 40 parts of polyhydric alcohol, 2 parts of mica powder and 7 parts of tert-butyl dimethyl alkyl imidazole.
6. The imidazolyl-modified epoxy resin lacquer according to claim 1 to 5, wherein the polyol is one or more of 1, 2-propanediol, 1, 3-propanediol or 1, 4-propanediol.
7. The preparation method of the imidazolyl-modified epoxy resin paint according to claim 1, comprising the steps of: adding bisphenol F type epoxy resin into aluminum tripolyphosphate and 1, 3-propylene glycol dibutyrate under the pressure of 0.1-0.2MPa, heating to 55-60 ℃, and stirring for reaction; adding mica powder and tert-butyl dimethyl alkyl imidazole, heating to 62-65 deg.C, and heating while stirring; adding polyalcohol, and stirring for 1-4 hr.
8. The method for preparing imidazolyl-modified epoxy resin paint as recited in claim 7, wherein the stirring speed is 700-800 rpm.
CN202011580844.XA 2020-12-28 2020-12-28 Imidazolyl-modified epoxy resin paint and preparation method thereof Pending CN112724794A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08245762A (en) * 1995-03-13 1996-09-24 Toshiba Chem Corp Epoxy resin composition and sealed semiconductor device
CN102056934A (en) * 2008-04-18 2011-05-11 陶氏环球技术公司 Silylimidazolium salt complexes
CN104004441A (en) * 2014-06-06 2014-08-27 南昌航空大学 Single-component epoxy primer and preparation method thereof
CN106699801A (en) * 2016-11-22 2017-05-24 山东硅科新材料有限公司 Synthetic process of silicon-based imidazole epoxy resin curing agent
CN106957585A (en) * 2017-02-28 2017-07-18 西安天元合成材料有限公司 A kind of anticorrosive paint

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08245762A (en) * 1995-03-13 1996-09-24 Toshiba Chem Corp Epoxy resin composition and sealed semiconductor device
CN102056934A (en) * 2008-04-18 2011-05-11 陶氏环球技术公司 Silylimidazolium salt complexes
CN104004441A (en) * 2014-06-06 2014-08-27 南昌航空大学 Single-component epoxy primer and preparation method thereof
CN106699801A (en) * 2016-11-22 2017-05-24 山东硅科新材料有限公司 Synthetic process of silicon-based imidazole epoxy resin curing agent
CN106957585A (en) * 2017-02-28 2017-07-18 西安天元合成材料有限公司 A kind of anticorrosive paint

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