CN113061386A - Preparation process of nano composite epoxy powder coating with different dimensions - Google Patents
Preparation process of nano composite epoxy powder coating with different dimensions Download PDFInfo
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- CN113061386A CN113061386A CN202110483692.XA CN202110483692A CN113061386A CN 113061386 A CN113061386 A CN 113061386A CN 202110483692 A CN202110483692 A CN 202110483692A CN 113061386 A CN113061386 A CN 113061386A
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
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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 is suitable for the technical field of paint preparation, and provides a preparation process of a nano composite epoxy powder paint with different dimensions, which comprises the following steps: A. modifying the nano material by using a modifier or a dispersant, and ball-milling and mixing the modified nano material and epoxy resin according to a proportion to prepare a nano material pre-dispersion; B. weighing the predispersion, epoxy resin, curing agent, flatting agent, filler, pigment and auxiliary agent according to a designed formula, crushing the mixture, and then mixing and stirring; C. carrying out melt extrusion on the uniformly mixed powder; D. and cooling, tabletting and grinding the extruded polymer, then screening, and obtaining the required powder coating product, wherein the molybdenum number of the screened powder is 110-130. Therefore, the invention has the advantages of simple process, high production efficiency, good modification effect and low cost.
Description
Technical Field
The invention relates to the technical field of paint preparation, in particular to a preparation process of a nano composite epoxy powder paint with different dimensions.
Background
Corrosion is a ubiquitous phenomenon of metal structures, causing enormous economic loss and life threat to humans. Common corrosion protection methods to slow down the corrosion rate are coating protection, cathodic protection and the addition of corrosion inhibitors. Surface coatings are currently the most common method of protecting metal surfaces from corrosion, which generally isolates the metal surface from the corrosive medium. And the coating is the most commonly used corrosion resistant material in industry because of its excellent mechanical and chemical resistance. Solvent-based coatings are prone to atmospheric pollution due to the release of Volatile Organic Compounds (VOCs). With the emergence of powder coating, compared with liquid coating, powder coating has the advantages of environmental protection, resource saving and high efficiency. Epoxy powder coatings are the most effective coatings for protecting steel from corrosion and have been studied in corrosive media such as seawater, marine and industrial environments. The epoxy-based coating has excellent performance, good stability in a corrosive environment, good adhesion on a metal matrix, and good mechanical property and thermal property, but the cured body of the epoxy resin has high crosslinking density and has the defects of large internal stress, brittleness, poor impact resistance and poor cracking resistance, and the like.
With the development of nanotechnology, the application of nano materials in the coating is more and more, the unique physical and chemical properties of the nano materials and the small-size effect, the quantum size effect and the surface interface effect which are not possessed by the conventional materials greatly improve the water washing resistance, the adhesive force, the smoothness and the aging resistance of the coating product, and the surface toughness and the hardness of the coating are also greatly improved. However, the nanoparticles have large specific surface area, high surface activity, easy agglomeration among particles, and high viscosity of the epoxy resin, and it is difficult to uniformly disperse the nanoparticles in the epoxy resin matrix.
The surface modification methods of nanomaterials are classified into physical methods, chemical methods and mechanochemical methods 3, which are classified into various methods such as action effects and means for modification.
The physical method is a method of modifying the surface by physical means such as adsorption, coating, and coating. The surface adsorption is to adsorb the heterogeneous material on the surface of the nano-particles through Van der Waals force or electrostatic attraction so as to prevent the nano-materials from agglomerating; coating and cladding are to wrap inorganic or organic compounds on the surface of the nano material to weaken the agglomeration.
The chemical method is to modify the surface of the nanometer material by utilizing various surface modifiers or chemical reactions, the most used at present are surfactants and coupling agents, and the modification mechanism of both is that the modifiers are used for grafting various functional groups on the surface of the nanometer material, so that the surface has reactivity and the surface structure and the chemical state of the nanometer material are changed.
The mechanochemical method is that through mechanical methods of crushing, grinding, friction and the like, the lattice structure, crystal form and the like of the nano material are changed, the internal energy of a system is increased, the temperature is raised, particles are promoted to be melted and thermally decomposed to generate free radicals or ions, the surface activity of the nano material is enhanced, and the nano material and other substances are promoted to be subjected to chemical reaction or mutual adhesion, so that the purpose of surface modification is achieved.
When modification is carried out by a coating means, the defects of long reaction time, high energy consumption, complex operation and the like exist; the mechanical method is simple to operate and low in cost, but the distribution of the particle size is not uniform; when the coupling agent or the surfactant is used for chemical modification, the dispersion stability is poor and the agglomeration is easy to occur again, so that the uniform dispersion of the nano particles in the epoxy resin matrix is difficult to achieve by adopting a common mechanical blending method or a melt blending method, and the nano particles are easy to agglomerate under the action of intermolecular force, static electricity and the like in the blending use process of the inorganic nano material and the organic material, so that the due effect of the nano material is lost.
In view of the above, the prior art is obviously inconvenient and disadvantageous in practical use, and needs to be improved.
Disclosure of Invention
In view of the above-mentioned drawbacks, the present invention provides a process for preparing a nano composite epoxy powder coating with different dimensions, which can uniformly distribute modified nanoparticles in a nano composite epoxy resin powder by utilizing the synergistic effect of a ball milling method and a melt mixing method, thereby producing a high-performance powder coating on conventional production equipment.
In order to achieve the purpose, the invention provides a preparation process of a nano composite epoxy powder coating with different dimensions, which comprises the following steps:
A. modifying the nano material by using a modifier or a dispersant, and ball-milling and mixing the modified nano material and epoxy resin according to a proportion to prepare a pre-dispersion with the nano material accounting for 0.1-3%;
B. weighing the predispersion, the epoxy resin, the curing agent, the flatting agent, the filler, the pigment and the auxiliary agent according to a designed formula, crushing the mixture to the granularity of 0.1-2 mm, and then mixing and stirring for 5-10 minutes;
C. carrying out melt extrusion on the uniformly mixed powder, wherein the melting temperature is 90-100 ℃, the temperature of an extruder head is 100-110 ℃, and the average residence time of the material is less than 30 seconds;
D. and cooling and tabletting the extruded polymer, feeding the polymer into a flour mill with 5000-6000 rpm for grinding, and screening the powder to obtain the powder coating product with the molybdenum number of 110-130.
According to the preparation process of the different-dimension nano composite epoxy powder coating, the epoxy resin is bisphenol A type epoxy resin.
According to the preparation process of the nano composite epoxy powder coating with different dimensions, the nano material particles are zero-dimensional nano material nano silicon dioxide or nano zinc oxide orDiatomite, nano bentonite, one-dimensional carbon nano tube or two-dimensional MoS2Or graphene oxide.
According to the preparation process of the different-dimension nano composite epoxy powder coating, ball milling and mixing in the step A are carried out by adopting a ball mill, the mixing time of the ball mill is 2-4 h, and the rotating speed of the ball mill is 400-600 r/m.
According to the preparation process of the nano composite epoxy powder coating with different dimensions, the mixing time of the ball mill is 3 hours, and the rotating speed of the ball mill is 500 r/m.
According to the preparation process of the nano composite epoxy powder coating with different dimensions, the modifier is KH-550 silane coupling agent or polyvinylpyrrolidone PVP or dopamine hydrochloride PDA.
According to the preparation process of the different-dimension nano composite epoxy powder coating, a screw extruder is adopted for melt extrusion in the step C, the melting temperature is 95 ℃, and the temperature of an extruder head is 105 ℃.
According to the preparation process of the different-dimension nano composite epoxy powder coating, the number of the powder molybdenum in the step D is 120 molybdenum.
The invention provides a preparation process of a nano composite epoxy powder coating with different dimensions, which comprises the following steps:
A. modifying the nano material by using a modifier or a dispersant, and ball-milling and mixing the modified nano material and epoxy resin according to a proportion to prepare a pre-dispersion with the nano material accounting for 0.1-3%;
B. weighing the predispersion, the epoxy resin, the curing agent, the flatting agent, the filler, the pigment and the auxiliary agent according to a designed formula, crushing the mixture to the granularity of 0.1-2 mm, and then mixing and stirring for 5-10 minutes;
C. carrying out melt extrusion on the uniformly mixed powder, wherein the melting temperature is 90-100 ℃, the temperature of an extruder head is 100-110 ℃, and the average residence time of the material is less than 30 seconds;
D. and cooling and tabletting the extruded polymer, feeding the polymer into a flour mill with 5000-6000 rpm for grinding, and screening the powder to obtain the powder coating product with the molybdenum number of 110-130.
The invention has the beneficial effects that: the synergistic effect of ball milling mixing and melt mixing extrusion increases the interaction among molecules, obviously improves the compatibility of the nano particles and the polymer or the polymer matrix, can fully disperse the nano material into the powder coating, and prevents the nano material from agglomerating. The produced nano composite epoxy powder coating has the advantages of strong adhesive force, high impact resistance, uniform and flat appearance of a coating film, good glossiness, good salt spray resistance and the like. The process method can adopt the conventional ball mill and powder production equipment to produce the nano composite epoxy powder coating. The production method can be operated at normal temperature and normal pressure, and has the advantages of simple process, high production efficiency, good modification effect and low cost. The ball milling mixing and melting mixing extrusion technology are adopted to improve the dispersion of the nano particles in the epoxy resin; the high-performance nano modified powder coating can be produced without changing the conventional powder coating production equipment, and is beneficial to industrial actual production and application.
Detailed Description
The present invention will be described in further detail with the aim of making the objects, technical solutions and advantages thereof more apparent, and it should be understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.
The invention provides a preparation process of a nano composite epoxy powder coating with different dimensions, which comprises the following steps:
A. modifying the nano material by using a modifier or a dispersant, and ball-milling and mixing the modified nano material and epoxy resin according to a proportion to prepare a pre-dispersion with the nano material accounting for 0.1-3%;
B. weighing the predispersion, the epoxy resin, the curing agent, the flatting agent, the filler, the pigment and the auxiliary agent according to a designed formula, crushing the mixture to the granularity of 0.1-2 mm, and then mixing and stirring for 5-10 minutes;
C. carrying out melt extrusion on the uniformly mixed powder, wherein the melting temperature is 90-100 ℃, the temperature of an extruder head is 100-110 ℃, and the average residence time of the material is less than 30 seconds;
D. and cooling and tabletting the extruded polymer, feeding the polymer into a flour mill with 5000-6000 rpm for grinding, and screening the powder to obtain the powder coating product with the molybdenum number of 110-130.
Preferably, the epoxy resin of the present invention is a bisphenol a type epoxy resin.
In addition, the nano material particles are zero-dimensional nano material nano silicon dioxide or nano zinc oxide or diatomite or nano bentonite or one-dimensional carbon nano tube or two-dimensional MoS2Or graphene oxide.
Further, ball milling and mixing in the step A are carried out by adopting a ball mill, the mixing time of the ball mill is 2-4 h, and the rotating speed of the ball mill is 400-600 r/m.
More preferably, the mixing time of the ball mill of the present invention is 3 hours, and the rotation speed of the ball mill is 500 rpm.
In addition, the modifier is KH-550 silane coupling agent or polyvinylpyrrolidone PVP or dopamine PDA hydrochloride.
In addition, a screw extruder is adopted for melt extrusion in the step C, the melting temperature is 95 ℃, and the temperature of an extruder head is 105 ℃.
Preferably, the number of the molybdenum powder in step D of the present invention is 120.
The first implementation mode comprises the following steps:
A. KH-550 silane coupling agent is selected to be used for coupling nano SiO2Modifying, namely modifying 2g of modified nano SiO2Ball-milling and mixing the mixture with 98g of epoxy resin in a ball mill for 3 hours at the rotating speed of 500 r/min to prepare the nano SiO-containing material22 percent of nano silicon dioxide epoxy resin pre-dispersion.
B. Weighing the predispersion, epoxy resin, curing agent, flatting agent, filler, pigment and auxiliary agent according to a designed formula, crushing to the granularity of less than 2mm, and then stirring and mixing for 5 minutes in a mixer;
C. adding the uniformly mixed powder into a screw extruder for melt extrusion, wherein the temperature of a cavity of the extruder is 95 ℃, the temperature of an extruder head is 105 ℃, and the average residence time of the material is not more than 30 seconds;
D. and tabletting the extruded polymer by a cooling tabletting machine, feeding the polymer into a flour mill with 5000-6000 rpm for grinding, separating fine powder by using a cyclone separator, and vibrating and sieving the powder separated by the cyclone separator with 120 molybdenum to obtain the required powder coating product.
Example two:
A. polyvinylpyrrolidone PVP is selected to modify the one-dimensional nano material multi-walled carbon nano-tube, and 0.2g of modified nano SiO is added2Ball-milling and mixing the powder and 99.8g of epoxy resin E12 in a ball mill for 3 hours at the rotating speed of 500 r/m to prepare the nano SiO-containing powder20.2 percent of multiwalled carbon nanotube epoxy resin pre-dispersion.
B. Weighing the predispersion, epoxy resin, curing agent, flatting agent, filler, pigment and auxiliary agent according to a designed formula, crushing to the granularity of less than 2mm, and then stirring and mixing for 5 minutes in a mixer;
C. adding the uniformly mixed powder into a screw extruder for melt extrusion, wherein the temperature of a cavity of the extruder is 95 ℃, the temperature of an extruder head is 105 ℃, and the average residence time of the material is not more than 30 seconds;
D. and tabletting the extruded polymer by a cooling tabletting machine, feeding the polymer into a flour mill with 5000-6000 rpm for grinding, separating fine powder by using a cyclone separator, and vibrating and sieving the powder separated by the cyclone separator with 120 molybdenum to obtain the multi-walled carbon nanotube composite epoxy powder coating.
The third embodiment is as follows:
A. selecting dopamine hydrochloride PDA to react with two-dimensional nano material MoS2Performing modification treatment to obtain 0.5g of modified nano SiO2Ball-milling and mixing the powder and 99.5g of epoxy resin E12 in a ball mill for 3 hours at the rotating speed of 500 r/m to prepare the nano SiO-containing powder20.5% MoS by mass2An epoxy resin pre-dispersion.
B. Weighing the predispersion, epoxy resin, curing agent, flatting agent, filler, pigment and auxiliary agent according to a designed formula, crushing to the granularity of less than 2mm, and then stirring and mixing for 3 minutes in a mixer;
C. adding the uniformly mixed powder into a screw extruder for melt extrusion, wherein the temperature of a cavity of the extruder is 95 ℃, the temperature of an extruder head is 105 ℃, and the average residence time of the material is not more than 30 seconds;
D. and tabletting the extruded polymer by a cooling tabletting machine, feeding the polymer into a flour mill with 5000-6000 rpm for grinding, separating fine powder by using a cyclone separator, and vibrating and sieving the powder subjected to cyclone separation by using 120 molybdenum to obtain the MoS2 composite epoxy powder coating.
The nano composite epoxy powder coating with different dimensions can be prepared in the embodiments, the material cost ratio can be changed according to actual conditions, and the nano composite epoxy powder coating can be roll-coated on different products.
In summary, the invention provides a preparation process of a nano composite epoxy powder coating with different dimensions, which comprises the following steps:
A. modifying the nano material by using a modifier or a dispersant, and ball-milling and mixing the modified nano material and epoxy resin according to a proportion to prepare a pre-dispersion with the nano material accounting for 0.1-3%;
B. weighing the predispersion, the epoxy resin, the curing agent, the flatting agent, the filler, the pigment and the auxiliary agent according to a designed formula, crushing the mixture to the granularity of 0.1-2 mm, and then mixing and stirring for 5-10 minutes;
C. carrying out melt extrusion on the uniformly mixed powder, wherein the melting temperature is 90-100 ℃, the temperature of an extruder head is 100-110 ℃, and the average residence time of the material is less than 30 seconds;
D. and cooling and tabletting the extruded polymer, feeding the polymer into a flour mill with 5000-6000 rpm for grinding, and screening the powder to obtain the powder coating product with the molybdenum number of 110-130.
The invention has the beneficial effects that: the synergistic effect of ball milling mixing and melt mixing extrusion increases the interaction among molecules, obviously improves the compatibility of the nano particles and the polymer or the polymer matrix, can fully disperse the nano material into the powder coating, and prevents the nano material from agglomerating. The produced nano composite epoxy powder coating has the advantages of strong adhesive force, high impact resistance, uniform and flat appearance of a coating film, good glossiness, good salt spray resistance and the like. The process method can adopt the conventional ball mill and powder production equipment to produce the nano composite epoxy powder coating. The production method can be operated at normal temperature and normal pressure, and has the advantages of simple process, high production efficiency, good modification effect and low cost. The ball milling mixing and melting mixing extrusion technology are adopted to improve the dispersion of the nano particles in the epoxy resin; the high-performance nano modified powder coating can be produced without changing the conventional powder coating production equipment, and is beneficial to industrial actual production and application.
The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it should be understood that various changes and modifications can be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A preparation process of a nano composite epoxy powder coating with different dimensions is characterized by comprising the following steps:
A. modifying the nano material by using a modifier or a dispersant, and ball-milling and mixing the modified nano material and epoxy resin according to a proportion to prepare a pre-dispersion with the nano material accounting for 0.1-3%;
B. weighing the predispersion, the epoxy resin, the curing agent, the flatting agent, the filler, the pigment and the auxiliary agent according to a designed formula, crushing the mixture to the granularity of 0.1-2 mm, and then mixing and stirring for 5-10 minutes;
C. carrying out melt extrusion on the uniformly mixed powder, wherein the melting temperature is 90-100 ℃, the temperature of an extruder head is 100-110 ℃, and the average residence time of the material is less than 30 seconds;
D. and cooling and tabletting the extruded polymer, feeding the polymer into a flour mill with 5000-6000 rpm for grinding, and screening the powder to obtain the powder coating product with the molybdenum number of 110-130.
2. The process for preparing a nano composite epoxy powder coating with different dimensions as claimed in claim 1, wherein the epoxy resin is bisphenol a epoxy resin.
3. The process for preparing nano composite epoxy powder paint with different dimensions as claimed in claim 1, wherein the nano material particles are zero-dimensional nano material nano silica or nano zinc oxide or diatomite or nano bentonite or one-dimensional carbon nano tube or two-dimensional MoS2Or graphene oxide.
4. The preparation process of the different-dimension nano composite epoxy powder coating according to claim 1, wherein ball milling mixing in the step A is performed by a ball mill, the mixing time of the ball mill is 2-4 h, and the rotation speed of the ball mill is 400-600 rpm.
5. The process for preparing nano composite epoxy powder coating with different dimensions as claimed in claim 4, wherein the mixing time of the ball mill is 3h, and the rotation speed of the ball mill is 500 rpm.
6. The process for preparing nano composite epoxy powder coating with different dimensions as claimed in claim 1, wherein the modifier is KH-550 silane coupling agent or polyvinylpyrrolidone PVP or dopamine PDA hydrochloride.
7. The process for preparing nano composite epoxy powder coating with different dimensions as claimed in claim 1, wherein the melt extrusion in step C adopts a screw extruder, the melting temperature is 95 ℃, and the temperature of the extruder head is 105 ℃.
8. The process for preparing a nano composite epoxy powder coating with different dimensions as claimed in claim 1, wherein the number of the powder molybdenum in the step D is 120 molybdenum.
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Cited By (5)
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| CN113637383A (en) * | 2021-07-21 | 2021-11-12 | 潍坊东方钢管有限公司 | Preparation method of polydopamine modified molybdenum disulfide composite epoxy powder coating |
| CN113667373A (en) * | 2021-07-21 | 2021-11-19 | 潍坊东方钢管有限公司 | Preparation method of silane modified nano silicon dioxide composite epoxy resin powder coating |
| CN113736338A (en) * | 2021-07-21 | 2021-12-03 | 潍坊东方钢管有限公司 | Preparation method of pyrrolidone modified multi-walled carbon nanotube composite epoxy powder coating |
| CN115505318A (en) * | 2022-08-09 | 2022-12-23 | 潍坊东方钢管有限公司 | Processing method of composite epoxy powder coating and material conveying equipment |
| CN116410626A (en) * | 2021-12-29 | 2023-07-11 | 山东东岳未来氢能材料股份有限公司 | Antistatic agent for ETFE powder coating and antistatic ETFE powder coating |
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| CN115505318A (en) * | 2022-08-09 | 2022-12-23 | 潍坊东方钢管有限公司 | Processing method of composite epoxy powder coating and material conveying equipment |
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