CN111607298A - Preparation method of spherical polypropylene powder coating - Google Patents
Preparation method of spherical polypropylene powder coating Download PDFInfo
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- CN111607298A CN111607298A CN202010556963.5A CN202010556963A CN111607298A CN 111607298 A CN111607298 A CN 111607298A CN 202010556963 A CN202010556963 A CN 202010556963A CN 111607298 A CN111607298 A CN 111607298A
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- polypropylene
- powder coating
- antioxidant
- solvent
- polypropylene powder
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 85
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 85
- -1 polypropylene Polymers 0.000 title claims abstract description 75
- 239000000843 powder Substances 0.000 title claims abstract description 67
- 238000000576 coating method Methods 0.000 title claims abstract description 57
- 239000011248 coating agent Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 45
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 30
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 27
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000008569 process Effects 0.000 claims abstract description 24
- 239000008096 xylene Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 11
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 11
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 11
- 229920005629 polypropylene homopolymer Polymers 0.000 claims abstract description 10
- 125000003944 tolyl group Chemical group 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 15
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical group O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 15
- 150000002978 peroxides Chemical class 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 11
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 11
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000000605 extraction Methods 0.000 description 4
- 229920001169 thermoplastic Polymers 0.000 description 4
- 239000004416 thermosoftening plastic Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
Classifications
-
- 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
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D123/10—Homopolymers or copolymers of propene
- C09D123/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
-
- 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
- C09D5/031—Powdery paints characterised by particle size or shape
-
- 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
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/47—Levelling agents
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/48—Stabilisers against degradation by oxygen, light or heat
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/80—Processes for incorporating ingredients
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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)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a preparation method of spherical polypropylene powder coating, which comprises the steps of preparing raw materials of polypropylene, a solvent and an auxiliary agent by adopting a solvent precipitation process to obtain the spherical polypropylene powder coating; the raw material polypropylene is homo-polypropylene, co-polypropylene or a mixture of homo-polypropylene and co-polypropylene, the solvent is toluene, xylene or a mixture of toluene and xylene, and the auxiliary agent is an antioxidant, a leveling agent and a molecular weight regulator. The method adopts a solvent precipitation process to prepare the polypropylene powder coating, and can prepare the polypropylene powder coatings with different particle sizes by adjusting the proportioning, cooling speed, stirring and other processes, and the powder coating has the characteristics of narrow particle size distribution, high sphericity, good powder flowability and the like. In addition, the polypropylene powder coating prepared by the method has the characteristics of cleanness, high efficiency, high yield and easiness in automatic production due to no three-waste discharge because the whole process is closed.
Description
Technical Field
The invention relates to the technical field of paint preparation, in particular to a preparation method of a spherical polypropylene powder paint.
Background
The powder coating is a solid powder synthetic resin coating composed of solid resin, pigment, filler, auxiliary agent and the like. Unlike conventional solvent-based coatings and water-based coatings, the dispersion medium is not a solvent and water, but air. It has the characteristics of no solvent pollution, 100 percent film forming and low energy consumption. Powder coatings fall into two broad categories, thermoplastic and thermosetting. The appearance (luster and leveling property) of a coating film of the thermoplastic powder coating is poor, and the adhesion between the thermoplastic powder coating and metal is also poor, so the thermoplastic powder coating is rarely applied in the field of automobile coating.
In the prior art, the conventional method for preparing the polypropylene powder coating adopts a mechanical grinding process, although the processing process is simple, a large amount of liquid nitrogen is consumed, the particle shape is irregular, the powder flowability is poor, the powder is not easy to spread in the construction, and the surface leveling of the coating needs post-baking treatment. In addition, the particle size distribution of the mechanically pulverized powder is too wide, the recovery rate of the finished product is not high, and the coarse powder and the fine powder outside the finished product need to be granulated again, so that certain influence is caused on the performance of the product in the later period, and the workload and the production cost are increased. Especially for ultra-fine powders smaller than 30 microns, the mechanical milling process is ineffective.
Disclosure of Invention
The invention provides a preparation method of spherical polypropylene powder coating.
The invention provides the following scheme:
a preparation method of spherical polypropylene powder coating comprises the steps of preparing raw materials of polypropylene, a solvent and an auxiliary agent by adopting a solvent precipitation process to obtain the spherical polypropylene powder coating;
the raw material polypropylene is homo-polypropylene, co-polypropylene or a mixture of homo-polypropylene and co-polypropylene, the solvent is toluene, xylene or a mixture of toluene and xylene, and the auxiliary agent is an antioxidant, a leveling agent and a molecular weight regulator.
Preferably: the mass ratio of the raw material polypropylene to the solvent is 1:3-1: 8.
Preferably: the mass ratio of the raw material polypropylene to the solvent is 1: 4.
Preferably: the antioxidant is a mixture of an antioxidant 1010 and an antioxidant 168, the mass ratio of the antioxidant 1010 to the antioxidant 168 is 3:1-5:1, and the weight of the antioxidant is 0.5-3% of that of the raw material polypropylene.
Preferably: the mass ratio of the antioxidant 1010 to the antioxidant 168 is 4: 1.
Preferably: the leveling agent is an acrylate leveling agent, and the weight of the leveling agent is 0.5-2% of that of the raw material polypropylene.
Preferably: the molecular weight regulator comprises peroxide and a performance improver, and the mass ratio of the peroxide to the performance improver is 1:5-1: 10.
Preferably: the peroxide is dicumyl peroxide, and the weight of the dicumyl peroxide is 0.1-0.5% of the weight of the raw material polypropylene.
Preferably: the performance improver is maleic anhydride, and the weight of the maleic anhydride is 1-5% of the weight of the raw material polypropylene.
Preferably: the solvent precipitation process comprises a high-pressure reaction process and a drying process, wherein the peroxide is added in the high-pressure reaction process; and (3) after the material obtained by the high-pressure reaction process enters a drying process, aging is carried out at the temperature of 80 ℃ for 24 hours, and then the maleic anhydride is added.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
according to the invention, the preparation method of the spherical polypropylene powder coating can be realized, and in one implementation mode, the method can comprise the steps of preparing the raw materials of polypropylene, a solvent and an auxiliary agent by adopting a solvent precipitation process to obtain the spherical polypropylene powder coating; the raw material polypropylene is homo-polypropylene, co-polypropylene or a mixture of homo-polypropylene and co-polypropylene, the solvent is toluene, xylene or a mixture of toluene and xylene, and the auxiliary agent is an antioxidant, a leveling agent and a molecular weight regulator. The method adopts a solvent precipitation process to prepare the polypropylene powder coating, and can prepare the polypropylene powder coatings with different particle sizes by adjusting the proportioning, cooling speed, stirring and other processes, and the powder coating has the characteristics of narrow particle size distribution, high sphericity, good powder flowability and the like. In addition, the polypropylene powder coating prepared by the method has the characteristics of cleanness, high efficiency, high yield and easiness in automatic production due to no three-waste discharge because the whole process is closed.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
The embodiment of the invention provides a preparation method of spherical polypropylene powder coating, which comprises the steps of preparing raw materials of polypropylene, solvent and auxiliary agent by adopting a solvent precipitation process to obtain the spherical polypropylene powder coating;
the raw material polypropylene is homo-polypropylene, co-polypropylene or a mixture of homo-polypropylene and co-polypropylene, the solvent is toluene, xylene or a mixture of toluene and xylene, and the auxiliary agent is an antioxidant, a leveling agent and a molecular weight regulator.
Further, the mass ratio of the raw material polypropylene to the solvent is 1:3-1: 8. Still further, the mass ratio of the raw material polypropylene to the solvent is 1: 4.
The antioxidant is a mixture of an antioxidant 1010 and an antioxidant 168, the mass ratio of the antioxidant 1010 to the antioxidant 168 is 3:1-5:1, and the weight of the antioxidant is 0.5-3% of that of the raw material polypropylene. The mass ratio of the antioxidant 1010 to the antioxidant 168 is 4: 1.
The leveling agent is an acrylate leveling agent, and the weight of the leveling agent is 0.5-2% of that of the raw material polypropylene.
The molecular weight regulator comprises peroxide and a performance improver, and the mass ratio of the peroxide to the performance improver is 1:5-1: 10. The peroxide is dicumyl peroxide, and the weight of the dicumyl peroxide is 0.1-0.5% of the weight of the raw material polypropylene. The performance improver is maleic anhydride, and the weight of the maleic anhydride is 1-5% of the weight of the raw material polypropylene.
The solvent precipitation process comprises a high-pressure reaction process and a drying process, wherein the peroxide is added in the high-pressure reaction process; and (3) after the material obtained by the high-pressure reaction process enters a drying process, aging is carried out at the temperature of 80 ℃ for 24 hours, and then the maleic anhydride is added. The peroxide and the maleic anhydride are added simultaneously in the method provided by the application, so that the peroxide and the maleic anhydride can be prevented from being mixed in the preparation process, and adhesion is prevented from being formed at normal temperature. After the materials enter a double-cone vacuum dryer (drying process) from a high-pressure reaction kettle (high-pressure reaction process), the materials need to be aged for 24 hours at the water temperature of 80 ℃ to ensure that the spherical polypropylene particles formed in the early stage are further stable to form compact and uniform spherical particles.
The embodiments provided in the present application are described in detail below with reference to specific examples, and the raw materials used in the following examples are all commercially available raw materials, and the sources of the raw materials are not limited in the present application.
Example 1:
300 kg of homopolymerized polypropylene, 2000 l of dimethylbenzene, 0.3 kg of dicumyl peroxide, 3 kg of flatting agent, 3 kg of antioxidant 1010 and 1 kg of antioxidant 168 are put into a 3000 l high-pressure reaction kettle, sealed, subjected to nitrogen-vacuum replacement twice and then filled with nitrogen to 0.2 MPa. Heating, controlling the rotating speed to 30 revolutions per minute, and when the material temperature reaches 150 ℃, beginning to preserve heat for 2 hours. And then stopping heating, keeping the rotating speed unchanged, slowly opening an air extraction valve, recovering xylene steam through a condenser, and gradually reducing the pressure in the kettle to the normal pressure.
Putting the material which is cooled to the normal pressure into a 5000L double-cone vacuum dryer through a pipeline, setting the water temperature to be 80 ℃, aging for 24 hours, starting a vacuum pump, distilling xylene to remove most of xylene, condensing the xylene through a condenser and recycling the xylene, adding 3 kg of maleic anhydride after most of the xylene (more than 1700L) is removed, setting the water temperature to be 90 ℃, simultaneously starting a motor of the double-cone vacuum dryer, controlling the rotating speed of the double-cone vacuum dryer to be 3-5 r/min, further removing the xylene, finishing drying when the temperature of an air extraction opening of the double-cone vacuum dryer is close to the room temperature and no more air is extracted, starting a cooling system of the double-cone vacuum dryer, and bringing the material in the dryer to the room temperature.
And sieving the dried material to obtain the polypropylene powder coating.
The performance of the obtained polypropylene powder coating is detected, and the product indexes are shown in table 1.
TABLE 1
Coarse powder with particle size less than 100 meshes | 0.5 kg |
100- | 309 kg |
Fine powder of more than 250 meshes | 1.0 kg |
Yield of finished product | 99.5% |
Angle of repose | 30° |
Bulk densityDegree of rotation | 600 g/l |
Solvent recovery | 1995L |
It can be known from table 1 that the powder coating obtained in example 1 has no odor of irritant maleic anhydride and dicumyl peroxide, and the melt index is obviously reduced and the toughness and adhesion are obviously improved along with the extension of the heat preservation time in the process of the re-melt index test, which indicates that the molecular weight regulator participates in the reaction and plays a role in further improving the performance of polypropylene.
Coating performance: the coating is flat, the adhesion is high, the coating is not cracked when being bent, and the impact coating is not cracked.
Example 2:
200 kg of homopolymerized polypropylene, 100 kg of copolymerized polypropylene, 1500 l of dimethylbenzene, 500 l of methylbenzene, 0.01 kg of dicumyl peroxide, 4 kg of flatting agent, 5 kg of antioxidant 1010 and 1 kg of antioxidant 168 are put into a 3000 l high-pressure reaction kettle, sealed, subjected to nitrogen-vacuum replacement twice and then filled with nitrogen to 0.2 MPa. Heating, controlling the rotating speed to 25 revolutions per minute, and when the material temperature reaches 150 ℃, beginning to preserve heat for 2 hours. Then slowly opening an air extraction valve, recovering the steam through a condenser, and gradually reducing the pressure in the kettle to the normal pressure.
Putting the material which is reduced to the normal pressure into a 5000L double-cone vacuum dryer through a pipeline, setting the water temperature to be 80 ℃, aging for 24 hours, starting a vacuum pump, distilling xylene to remove most of xylene, condensing the xylene through a condenser and recycling the xylene, adding 3 kg of maleic anhydride to set the water temperature to be 90 ℃ after most of solvent (more than 1700L) is removed, simultaneously starting a motor of the double-cone vacuum dryer, controlling the rotating speed of the double-cone vacuum dryer to be 3-5 r/min, further removing the xylene, finishing drying when the temperature of an air extraction opening of the double-cone vacuum dryer is close to the room temperature and no gas is extracted, starting a cooling system of the double-cone vacuum dryer, and turning the material in the dryer to the room temperature.
And sieving the dried material to obtain the polypropylene powder coating.
The performance of the obtained polypropylene powder coating is detected, and the product indexes are shown in table 2.
TABLE 2
Coarse powder with particle size less than 100 meshes | 0.3 kg |
100- | 309 kg |
Fine powder of more than 250 meshes | 0.8 kg |
Yield of finished product | 99.6% |
Angle of repose | 30° |
Bulk density | 590 g/l |
Solvent recovery | 1998L |
As can be seen from Table 2, the powder coating obtained in example 2 did not have the odor of irritating maleic anhydride and dicumyl peroxide, and the melt index was significantly decreased and the toughness and adhesion were significantly improved with the increase of the holding time in the re-melt index test process, indicating that the molecular weight regulator participated in the reaction and further improved the polypropylene performance.
Coating performance: the coating is flat, the adhesion is high, the coating is not cracked when being bent, and the impact coating is not cracked.
In summary, the preparation method of the spherical polypropylene powder coating provided by the application has the following characteristics:
1. the particle shape is similar to a sphere, and the polypropylene powder has excellent powder flow property, particularly outstanding powder flow property when being used as polypropylene ultrafine powder.
2. Compared with mechanical crushing, the powder prepared by the precipitation method has high melting and leveling speeds, can be instantly melted and leveled, and saves a complicated process of further leveling treatment by high-temperature baking after plastic dipping.
3. The particle size of the powder is controllable, and the particle size of the polypropylene powder can be controlled by adjusting the processes such as feeding ratio, cooling speed, rotating speed and the like, so that the application in different fields is met.
4. High product yield, low production cost, labor saving and easy automatic production.
5. The production is environment-friendly, the whole process has no three-waste discharge, and the method accords with the current environmental protection policy.
6. The method can be used for preparing superfine polypropylene powder, and preparing polypropylene superfine powder which cannot be prepared by mechanical crushing, thereby expanding the application field of polypropylene powder.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of spherical polypropylene powder coating is characterized in that the method comprises the steps of preparing raw materials of polypropylene, solvent and auxiliary agent by adopting a solvent precipitation process to obtain the spherical polypropylene powder coating;
the raw material polypropylene is homo-polypropylene, co-polypropylene or a mixture of homo-polypropylene and co-polypropylene, the solvent is toluene, xylene or a mixture of toluene and xylene, and the auxiliary agent is an antioxidant, a leveling agent and a molecular weight regulator.
2. The method for preparing spherical polypropylene powder coating according to claim 1, wherein the mass ratio of the raw material polypropylene to the solvent is 1:3 to 1: 8.
3. The method for preparing spherical polypropylene powder coating according to claim 2, wherein the mass ratio of the raw material polypropylene to the solvent is 1: 4.
4. The preparation method of the spherical polypropylene powder coating as claimed in claim 1, wherein the antioxidant is a mixture of an antioxidant 1010 and an antioxidant 168, the mass ratio of the antioxidant 1010 to the antioxidant 168 is 3:1-5:1, and the weight of the antioxidant is 0.5-3% of the weight of the raw material polypropylene.
5. The method for preparing spherical polypropylene powder coating according to claim 4, wherein the mass ratio of the antioxidant 1010 to the antioxidant 168 is 4: 1.
6. The method for preparing spherical polypropylene powder coating according to claim 1, wherein the leveling agent is acrylate leveling agent, and the weight of the leveling agent is 0.5-2% of the weight of the raw material polypropylene.
7. The method for preparing spherical polypropylene powder coating according to claim 1, wherein the molecular weight regulator comprises peroxide and a performance improver, and the mass ratio of the peroxide to the performance improver is 1:5-1: 10.
8. The method for preparing spherical polypropylene powder coating according to claim 7, wherein the peroxide is dicumyl peroxide, and the weight of the dicumyl peroxide is 0.1-0.5% of the weight of the raw polypropylene.
9. The method for preparing spherical polypropylene powder coating according to claim 7, wherein the performance improver is maleic anhydride, and the weight of the maleic anhydride is 1-5% of the weight of the raw material polypropylene.
10. The method for preparing spherical polypropylene powder coating according to claim 9, wherein the solvent precipitation process comprises a high pressure reaction step and a drying step, the peroxide is added in the high pressure reaction step; and (3) after the material obtained by the high-pressure reaction process enters a drying process, aging is carried out at the temperature of 80 ℃ for 24 hours, and then the maleic anhydride is added.
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