CN110373070A - A kind of high-intensitive heating anti-corrosion Graphene powder powder material and its preparation method and application - Google Patents
A kind of high-intensitive heating anti-corrosion Graphene powder powder material and its preparation method and application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
- C09D5/038—Anticorrosion agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of preparation methods of high-intensitive heating anti-corrosion Graphene powder powder material, include the following steps: the preparation of (1) modified graphene nanometer powder；(2) the modified graphene powder of step (1) preparation and fluorocarbon resin, styrax, dimethicone, di-2-ethylhexylphosphine oxide hexamethylene alkanamine are added in stirring container, are heated to 80-100 DEG C and are uniformly mixed；(3) nano-silicon nitride is added in the mixture obtained by step (2), continues to be stirred 30-60min, is then fed into double screw extruder and squeezes out, tabletting crushes, and grinding is sieved to get the high-strength anti-corrosion graphene powder coating.Preparation method of the present invention is simple, easily-controlled reaction conditions, low production cost, and prepared graphene powder coating has good intensity and corrosion resistance, easy to industrialized production.
Description
Technical field
The invention belongs to the preparation technical fields of grapheme material, and in particular to a kind of high-intensitive heating anti-corrosion Graphene powder
Powder material and its preparation method and application.
Background technique
Graphene is most hard, most thin nanometer new material known to the current mankind, is that one kind is connected by carbon atom with sp2 hydridization
The hexangle type of formation is in the flat film of honeycomb lattice, and 2004 by Univ Manchester UK physics professor AndreGeim
It is successfully separated out from graphite for the first time.Graphene has very excellent performance: (1) high mechanical strength-graphene thickness is only
Become 0.335nm, Young's modulus is up to 1TPa, and breaking strength is up to 130GPa；(2) high conductivity-graphene resistivity only 10-6
Ω cm, its electron mobility is more than 15000cm2/Vs under room temperature；(3) high-termal conductivity-single-layer graphene thermal coefficient is high
Up to 5300W/mK, it is higher than carbon nanotube (3000~3500W/mK) and diamond (1000~2200W/mK)；(4) high full
It is 6 (100-600A/ squares of the order of magnitude higher than copper with A/ square centimeters of the electric current degree of current density-graphene tolerable 1~200,000,000
Centimetre).The above-mentioned excellent properties of graphene make graphene using more and more extensive.
Two-dimension nano materials of the graphene as novel lamellar structure, are added in material so as to improve material
Performance has also obtained extensive research.Patent of invention CN104789028A discloses a kind of anticorrosion material comprising graphene fragment
Material, content is composed of the following components by mass percentage: film forming agent 20~80%, solvent 10~30%, and graphene fragment 0.1~
20%, pigment 1~10%, filler 1~20%.Material made from the invention has the characteristics that simple process and at low cost, and anti-
The good advantage of corrosive effect.It is anti-that Chinese patent CN103265881A discloses a kind of high temperature resistant comprising poly- aryl organic siliconresin
Rotten material is made of following component according to weight ratio: 40~50 parts of poly- aryl organic siliconresin, P-hydroxybenzoic acid glycidol
It is 20~30 parts of ester, 5~10 parts of acrylic resin, 10~15 parts of mica powder, 10~15 parts of graphene, 5~10 parts of ethyl acetate, dilute
Release 10~20 parts of agent；Diluent is butanol or dimethylbenzene.Manufactured anti-corrosion material can reach 400~500 DEG C with tolerable temperature, together
When have good anti-corrosion effect.However, some comprehensive performances of the grapheme material of above-mentioned prior art research are ideal not enough,
Some cause the stability of material and brushing performance also not good enough since the dispersibility of graphene is insufficient, need further progress
Improve.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of high-intensitive heating anti-corrosion graphene powder materials
The Graphene powder powder material one side of material and preparation method thereof, this quilt of present invention institute has very excellent intensity and anticorrosion energy
Power, on the other hand its stability and coating performance are also very excellent.
To achieve the goals above, the technical scheme adopted by the invention is as follows:
A kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, includes the following steps:
(1) preparation of modified graphene nanometer powder；
(2) by the modified graphene powder and fluorocarbon resin, styrax, dimethicone, di-2-ethylhexylphosphine oxide of step (1) preparation
Hexamethylene alkanamine is added in stirring container, is heated to 80-100 DEG C and is uniformly mixed；
(3) nano-silicon nitride is added in the mixture obtained by step (2), continues to be stirred 30-60min, followed by send
Enter in double screw extruder and squeeze out, tabletting crushes, grinding, and screening is to get the high-intensitive heating anti-corrosion graphene powder material
Material.
Preferably, in step (1) modified graphene the preparation method comprises the following steps: the graphene oxide of preparation is added to deionization
It in water, is uniformly dispersed, hydrazine hydrate is then added, react 3h at 70 DEG C, add dicyclohexylcarbodiimide and 3- aminopropan
Ethyl triethoxy silicane alkane, ultrasonic wave are uniformly dispersed, and are stirred to react 16h at 100 DEG C, obtain modified graphene nanometer powder.
Preferably, in parts by weight, the modified graphene powder in step (2) is 0.5-1 parts, fluorocarbon resin 50-80
Part, 1-2 parts of styrax, 2-4 parts of dimethicone, 3-7 parts of di-2-ethylhexylphosphine oxide hexamethylene alkanamine.
Preferably, in parts by weight, the additional amount of nano-silicon nitride is 2-6 parts in step (3).
Preferably, the time of ultrasonic wave dispersion is 1-5 hours.
In addition, the high-intensitive heating anti-corrosion graphene powder material that the preparation method is prepared is also claimed in the present invention
Material.
High-intensitive heating anti-corrosion Graphene powder powder material of the present invention can be coated on architectural shape surface, communication apparatus table
Face, track turnout surface or LED illumination lamp decoration surface.
Compared with prior art, the invention has the benefit that
(1) present invention is first modified graphene, is dispersed not with preventing graphene to be added directly into film-forming resin
, improved graphene can be grafted to obtain on fluorocarbon resin, so that graphene is fully dispersed in fluorocarbon resin；Separately
Outside, the present invention is by dispersing nano-silicon nitride in fluorocarbon resin, can increase the mechanical property of fluorocarbon resin material and resistance to
Corrosive nature；
(2) preparation method of the present invention is simple, easily-controlled reaction conditions, and low production cost is easy to industrialized production.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, includes the following steps:
(1) preparation of modified graphene nanometer powder: 55 parts of deionization is added to by 12 parts of graphene oxide of preparation
In water, be uniformly dispersed, then be added 4 parts of hydrazine hydrates, react 3h at 70 DEG C, add 0.6 part of dicyclohexylcarbodiimide and
15 parts of 3-aminopropyltriethoxysilane, ultrasonic wave disperse 3h, are stirred to react 16h at 100 DEG C, obtain modified graphene and receive
Rice flour end；
(2) by 0.8 part of the modified graphene powder and 70 parts of fluorocarbon resin, 1.5 parts of styrax, diformazan of step (1) preparation
In 5 parts of 3 parts of base silicone oil, di-2-ethylhexylphosphine oxide hexamethylene alkanamine addition stirring containers, it is heated to 90 DEG C and is uniformly mixed；
(3) 4 parts of nano-silicon nitride are added in the mixture obtained by step (2), continue to be stirred 45min, followed by send
Enter in double screw extruder and squeeze out, tabletting crushes, grinding, and screening is to get the high-intensitive heating anti-corrosion graphene powder material
Material.
Embodiment 2
A kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, includes the following steps:
(1) preparation of modified graphene nanometer powder: 55 parts of deionization is added to by 12 parts of graphene oxide of preparation
In water, be uniformly dispersed, then be added 4 parts of hydrazine hydrates, react 3h at 70 DEG C, add 0.6 part of dicyclohexylcarbodiimide and
15 parts of 3-aminopropyltriethoxysilane, ultrasonic wave disperse 3h, are stirred to react 16h at 100 DEG C, obtain modified graphene and receive
Rice flour end；
(2) by 0.6 part of the modified graphene powder and 60 parts of fluorocarbon resin, 1.2 parts of styrax, diformazan of step (1) preparation
In 4 parts of 2.4 parts of base silicone oil, di-2-ethylhexylphosphine oxide hexamethylene alkanamine addition stirring containers, it is heated to 90 DEG C and is uniformly mixed；
(3) 3 parts of nano-silicon nitride are added in the mixture obtained by step (2), continue to be stirred 50min, followed by send
Enter in double screw extruder and squeeze out, tabletting crushes, grinding, and screening is to get the high-intensitive heating anti-corrosion graphene powder material
Material.
Embodiment 3
A kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, includes the following steps:
(1) preparation of modified graphene nanometer powder: 55 parts of deionization is added to by 12 parts of graphene oxide of preparation
In water, be uniformly dispersed, then be added 4 parts of hydrazine hydrates, react 3h at 70 DEG C, add 0.6 part of dicyclohexylcarbodiimide and
15 parts of 3-aminopropyltriethoxysilane, ultrasonic wave disperse 3h, are stirred to react 16h at 100 DEG C, obtain modified graphene and receive
Rice flour end；
(2) by 1 part of the modified graphene powder and 80 parts of fluorocarbon resin, 2 parts of styrax, dimethyl-silicon of step (1) preparation
In 7 parts of 4 parts of oil, di-2-ethylhexylphosphine oxide hexamethylene alkanamine addition stirring containers, it is heated to 100 DEG C and is uniformly mixed；
(3) 6 parts of nano-silicon nitride are added in the mixture obtained by step (2), continue to be stirred 60min, followed by send
Enter in double screw extruder and squeeze out, tabletting crushes, grinding, and screening is to get the high-intensitive heating anti-corrosion graphene powder material
Material.
Embodiment 4
A kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, includes the following steps:
(1) preparation of modified graphene nanometer powder: 55 parts of deionization is added to by 12 parts of graphene oxide of preparation
In water, be uniformly dispersed, then be added 4 parts of hydrazine hydrates, react 3h at 70 DEG C, add 0.6 part of dicyclohexylcarbodiimide and
15 parts of 3-aminopropyltriethoxysilane, ultrasonic wave disperse 3h, are stirred to react 16h at 100 DEG C, obtain modified graphene and receive
Rice flour end；
(2) by 0.5 part of the modified graphene powder and 50 parts of fluorocarbon resin, 1 part of styrax, dimethyl of step (1) preparation
In 3 parts of 2 parts of silicone oil, di-2-ethylhexylphosphine oxide hexamethylene alkanamine addition stirring containers, it is heated to 100 DEG C and is uniformly mixed；
(3) 2 parts of nano-silicon nitride are added in the mixture obtained by step (2), continue to be stirred 40min, followed by send
Enter in double screw extruder and squeeze out, tabletting crushes, grinding, and screening is to get the high-intensitive heating anti-corrosion graphene powder material
Material.
Embodiment 5
A kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, includes the following steps:
(1) preparation of modified graphene nanometer powder: 55 parts of deionization is added to by 12 parts of graphene oxide of preparation
In water, be uniformly dispersed, then be added 4 parts of hydrazine hydrates, react 3h at 70 DEG C, add 0.6 part of dicyclohexylcarbodiimide and
15 parts of 3-aminopropyltriethoxysilane, ultrasonic wave disperse 3h, are stirred to react 16h at 100 DEG C, obtain modified graphene and receive
Rice flour end；
(2) by 0.9 part of the modified graphene powder and 60 parts of fluorocarbon resin, 1.8 parts of styrax, diformazan of step (1) preparation
In 6 parts of 3.2 parts of base silicone oil, di-2-ethylhexylphosphine oxide hexamethylene alkanamine addition stirring containers, it is heated to 90 DEG C and is uniformly mixed；
(3) 5 parts of nano-silicon nitride are added in the mixture obtained by step (2), continue to be stirred 50min, followed by send
Enter in double screw extruder and squeeze out, tabletting crushes, grinding, and screening is to get the high-intensitive heating anti-corrosion graphene powder material
Material.
Embodiment 6
A kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, includes the following steps:
(1) preparation of modified graphene nanometer powder: 55 parts of deionization is added to by 12 parts of graphene oxide of preparation
In water, be uniformly dispersed, then be added 4 parts of hydrazine hydrates, react 3h at 70 DEG C, add 0.6 part of dicyclohexylcarbodiimide and
15 parts of 3-aminopropyltriethoxysilane, ultrasonic wave disperse 3h, are stirred to react 16h at 100 DEG C, obtain modified graphene and receive
Rice flour end；
(2) by 0.7 part of the modified graphene powder and 65 parts of fluorocarbon resin, 2 parts of styrax, dimethyl of step (1) preparation
In 5 parts of 2 parts of silicone oil, di-2-ethylhexylphosphine oxide hexamethylene alkanamine addition stirring containers, it is heated to 100 DEG C and is uniformly mixed；
(3) 4 parts of nano-silicon nitride are added in the mixture obtained by step (2), continue to be stirred 50min, followed by send
Enter in double screw extruder and squeeze out, tabletting crushes, grinding, and screening is to get the high-intensitive heating anti-corrosion graphene powder material
Material.
Comparative example 1
A kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, includes the following steps:
(1) preparation of modified graphene nanometer powder: 55 parts of deionization is added to by 12 parts of graphene oxide of preparation
In water, be uniformly dispersed, then be added 4 parts of hydrazine hydrates, react 3h at 70 DEG C, add 0.6 part of dicyclohexylcarbodiimide and
15 parts of 3-aminopropyltriethoxysilane, ultrasonic wave disperse 3h, are stirred to react 16h at 100 DEG C, obtain modified graphene and receive
Rice flour end；
(2) by 0.8 part of the modified graphene powder and 70 parts of fluorocarbon resin, 1.5 parts of styrax, diformazan of step (1) preparation
In 5 parts of 3 parts of base silicone oil, di-2-ethylhexylphosphine oxide hexamethylene alkanamine addition stirring containers, it is heated to 90 DEG C and is uniformly mixed；
(3) mixture obtained by the step (2) is sent into double screw extruder and is squeezed out, tabletting, crushes, grinding, screening to get
The high-intensitive heating anti-corrosion Graphene powder powder material.
In order to illustrate the performance of the heating anti-corrosion Graphene powder powder material of high intensity prepared by the present invention, to embodiment 1-6
And the performance of the heating anti-corrosion Graphene powder powder material of high intensity prepared by comparative example 1 is determined, the result is as follows:
Illustrate: (1) above-mentioned appearance and color detection are range estimation；
(2) above-mentioned storage stability detection, using GB/T6753.3-1986 as examination criteria；
(3) above-mentioned impact strength detection, using GB/T1732-1993 as examination criteria；
(4) above-mentioned adhesive force detection, using GB/T1720-79 scratch as examination criteria；
(5) above-mentioned resistance to NaOH, resistance to H2SO4, resistance to NaCl detection, with GB/T9274-1988 examination criteria；
(6) above-mentioned oil resistivity detection, using GB/T9274-1988 as examination criteria；
(7) above-mentioned salt fog resistance detection, using GB/T1771-2007 as examination criteria.
Technical solution of the present invention and beneficial effect is described in detail in above-described specific embodiment, Ying Li
Solution is not intended to restrict the invention the foregoing is merely presently most preferred embodiment of the invention, all in principle model of the invention
Interior done any modification, supplementary, and equivalent replacement etc. are enclosed, should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of high-intensitive heating anti-corrosion Graphene powder powder material, which comprises the steps of:
(1) preparation of modified graphene nanometer powder；
(2) by the modified graphene powder and fluorocarbon resin, styrax, dimethicone, di-2-ethylhexylphosphine oxide hexamethylene of step (1) preparation
Alkanamine is added in stirring container, is heated to 80-100 DEG C and is uniformly mixed；
(3) nano-silicon nitride is added in the mixture obtained by step (2), continues to be stirred 30-60min, be then fed into double spiral shells
It squeezes out, tabletting, crushes in bar extruder, grinding, screening is to get the high-intensitive heating anti-corrosion Graphene powder powder material.
2. preparation method according to claim 1, which is characterized in that in step (1) modified graphene the preparation method comprises the following steps:
The graphene oxide of preparation is add to deionized water, is uniformly dispersed, hydrazine hydrate is then added, 3h is reacted at 70 DEG C, then
Dicyclohexylcarbodiimide is added and 3-aminopropyltriethoxysilane, ultrasonic wave are uniformly dispersed, is stirred to react at 100 DEG C
16h obtains modified graphene nanometer powder.
3. -2 described in any item preparation methods according to claim 1, which is characterized in that in parts by weight, changing in step (2)
Property graphene powder be 0.5-1 part, fluorocarbon resin be 50-80 parts, 1-2 parts of styrax, 2-4 parts of dimethicone, di-2-ethylhexylphosphine oxide
3-7 parts of hexamethylene alkanamine.
4. preparation method according to claim 1-3, which is characterized in that in parts by weight, nanometer in step (3)
The additional amount of silicon nitride is 2-6 parts.
5. according to the described in any item preparation methods of claim 2-4, which is characterized in that the time of ultrasonic wave dispersion is that 1-5 is small
When.
6. the high-intensitive heating anti-corrosion graphene powder material that a kind of any one of claim 1-5 preparation method is prepared
Material.
7. a kind of application of the heating anti-corrosion Graphene powder powder material of high intensity described in claim 6, which is characterized in that described high-strength
Degree heating anti-corrosion Graphene powder powder material can be coated on architectural shape surface, communication apparatus surface, track turnout surface or LED and shine
Bright lamp adorns surface.
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