CN117925086A - High-cohesiveness nylon 12 powder coating and preparation method and application thereof - Google Patents
High-cohesiveness nylon 12 powder coating and preparation method and application thereof Download PDFInfo
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- CN117925086A CN117925086A CN202410050140.3A CN202410050140A CN117925086A CN 117925086 A CN117925086 A CN 117925086A CN 202410050140 A CN202410050140 A CN 202410050140A CN 117925086 A CN117925086 A CN 117925086A
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- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 title claims abstract description 258
- 229920000299 Nylon 12 Polymers 0.000 title claims abstract description 226
- 239000000843 powder Substances 0.000 title claims abstract description 212
- 238000000576 coating method Methods 0.000 title claims abstract description 70
- 239000011248 coating agent Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 89
- 238000012216 screening Methods 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000853 adhesive Substances 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 61
- 239000000178 monomer Substances 0.000 claims description 52
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 36
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 28
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 26
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 26
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- 239000001361 adipic acid Substances 0.000 claims description 13
- 235000011037 adipic acid Nutrition 0.000 claims description 13
- 238000005507 spraying Methods 0.000 claims description 13
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 12
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 claims description 5
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000004985 diamines Chemical class 0.000 claims description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 4
- HQHCYKULIHKCEB-UHFFFAOYSA-N tetradecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCC(O)=O HQHCYKULIHKCEB-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 3
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims description 2
- 230000008595 infiltration Effects 0.000 claims description 2
- 238000001764 infiltration Methods 0.000 claims description 2
- 150000003951 lactams Chemical class 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229920005862 polyol Polymers 0.000 claims description 2
- 150000003077 polyols Chemical class 0.000 claims description 2
- DXNCZXXFRKPEPY-UHFFFAOYSA-N tridecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCC(O)=O DXNCZXXFRKPEPY-UHFFFAOYSA-N 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 description 35
- 238000000227 grinding Methods 0.000 description 27
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 24
- 238000012360 testing method Methods 0.000 description 17
- 239000004677 Nylon Substances 0.000 description 14
- 229920001778 nylon Polymers 0.000 description 14
- 238000001556 precipitation Methods 0.000 description 14
- 238000001291 vacuum drying Methods 0.000 description 13
- 239000005711 Benzoic acid Substances 0.000 description 12
- 235000010233 benzoic acid Nutrition 0.000 description 12
- 238000007599 discharging Methods 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 12
- 238000007142 ring opening reaction Methods 0.000 description 12
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 11
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 11
- 229920002292 Nylon 6 Polymers 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229920001169 thermoplastic Polymers 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- 239000004416 thermosoftening plastic Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004831 Hot glue Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000002966 varnish Substances 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
- C09D177/00—Coating compositions based on polyamides obtained by reactions forming a carboxylic amide link in the main chain; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/36—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino acids, polyamines and polycarboxylic acids
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyamides (AREA)
Abstract
The invention provides a high-cohesiveness nylon 12 powder coating, a preparation method and application thereof. The method comprises the following steps: optionally, mixing nylon 12 particles with a solvent, heating to dissolve, and cooling to a crystallization temperature to precipitate nylon 12 powder; adding laurolactam, comonomer, end-capping agent, catalyst and water into a polymerization reactor for polymerization to obtain copolymerized nylon 12 particles; and dissolving the copolymerized nylon 12 particles in a solvent to prepare a solution, adhering the solution to the surface of the nylon 12 powder, and separating, drying and screening to obtain the high-cohesiveness nylon 12 powder coating. Compared with the common nylon 12 powder coating, the powder coating prepared by the method has higher adhesive force, and meanwhile, the addition of the copolymerized nylon 12 can enable the surface of the product coating to be smoother.
Description
Technical Field
The invention belongs to the technical field of nylon materials, and particularly relates to a high-cohesiveness nylon 12 powder coating, a preparation method and application thereof.
Background
The powder coating is a novel coating, is directly coated in a form of fine powder, and a powder coating solid system can realize high utilization rate, thereby achieving maximum utilization of resources and belongs to an environment-friendly coating. Currently, powder coatings can be classified into thermoset and thermoplastic based on processing and film-forming characteristics.
The thermosetting powder coating consists of thermosetting resin, curing agent, pigment, assistant, etc. and is reacted with the curing agent to form the integral structure through crosslinking.
The thermoplastic powder coating takes thermoplastic resin as a main raw material, and is obtained by a precipitation method or a cryogenic grinding method; the film can be formed by heating, melting, leveling, cooling and solidifying without complex solidifying procedures, and has recoverability. Nylon powder coatings are one type of thermoplastic powder coating.
Nylon 12 has the advantages of good mechanical property, good wear resistance, good weather resistance and the like, so that the nylon 12 powder coating is widely applied to metal coating, and the coating prepared by the nylon 12 powder coating has excellent performances of detergent resistance, cold and hot water alternation resistance and the like, and simultaneously has smooth surface, excellent wear resistance and excellent stain resistance.
The nylon 12 powder coating is mainly applied to household appliances and automobiles, the use environments of the household appliances and automobiles are complex and variable, and the environment such as high humidity, high temperature, acid and alkali, oil salt and the like can be possibly contacted for a long time. The insufficient adhesive force can cause peeling, delamination, corrosion and the like of the product, and the product quality and the service life can be improved by improving the adhesive force of the product
To sum up, there is a need in the art of nylon 12 powder coatings to address the product deficiencies resulting from insufficient adhesion.
Disclosure of Invention
The invention aims to provide a preparation method of a high-cohesiveness nylon 12 powder coating, which has higher adhesive force compared with the common nylon 12 powder coating, and meanwhile, the addition of the copolymerized nylon 12 can enable the surface of a product coating to be smoother.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
A method for preparing a high-cohesiveness nylon 12 powder coating, comprising the steps of:
Optionally, S1: mixing nylon 12 particles with a solvent, heating to dissolve, and cooling to a crystallization temperature to precipitate nylon 12 powder;
s2: adding laurolactam, comonomer, end-capping agent, catalyst and water into a polymerization reactor for polymerization to obtain copolymerized nylon 12 particles;
S3: and dissolving the copolymerized nylon 12 particles in a solvent to prepare a solution, adhering the solution to the surface of the nylon 12 powder, and separating, drying and screening to obtain the high-cohesiveness nylon 12 powder coating.
The crystallization speed of the copolymerized nylon 12 is low, so that more time can be needed to fuse with the contact surface in the melting and cooling process, and the mechanism is similar to that of a nylon hot melt adhesive. The inventors have found in the study that the addition of copolymerized nylon 12 can reduce the crystallization rate during the powder coating process of nylon 12, resulting in improved adhesion. The addition of the copolymerized nylon 12 can reduce the crystal size and the crystal speed of the nylon 12 matrix powder, and is beneficial to improving the smoothness of the coated surface of the product.
In one embodiment of the invention, the relative viscosity of the nylon 12 of S1 ranges from 1.4 to 2.5, preferably from 1.6 to 2.1.
In one embodiment of the invention, the solvent of S1 is a polar alcoholic solvent, preferably one or more of ethanol, benzyl alcohol, hexafluoroisopropanol.
In one embodiment of the invention, the temperature at which S1 is raised is 140℃to 200 ℃.
In one embodiment of the invention, the S1 is dissolved to give a solution concentration of 1 to 60% by weight, preferably 10 to 40% by weight.
In one embodiment of the invention, the crystallization temperature of S1 is from 25℃to 139 ℃.
In one embodiment of the invention, the comonomer of S2 is a combination of lactam monomers, organic diacid monomers, organic diamine monomers; preferably a combination of a C6-C12 lactam monomer, a C2-C30 organic diacid monomer, and a C2-C30 organic diamine monomer; more preferably caprolactam, and one or more of hexamethylenediamine, pentamethylenediamine, decaenediamine, dodecaenediamine, and one or more of adipic acid, sebacic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid; preferably, the molar ratio of carboxyl groups to amino groups in the composition is 1:1. It is known in the art that the ratio of carboxyl mole number to amino mole number 1:1 in the composition is the most suitable reaction ratio, but small adjustments around this range do not significantly affect the actual effect.
In one embodiment of the invention, the proportion by mass of laurolactam in S2 in all comonomers is from 1% to 99%.
In one embodiment of the invention, the capping agent S2 is an organic carboxylic acid, preferably an organic mono-acid and/or an organic diacid; preferably, the end capping agent is added in an amount of 0.1 to 3wt% based on the total mass of the dodecalactam monomer and the comonomer.
In one embodiment of the invention, the catalyst of S2 is an oxygen-containing phosphorus catalyst, preferably one or more of phosphate-containing, phosphite-containing and hypophosphite-containing; preferably, the catalyst is added in an amount of 0.1 to 3wt% based on the total mass of dodecalactam monomer, comonomer and capping agent.
In one embodiment of the present invention, the water is added in an amount of 1 to 30wt% based on the total mass of the dodecalactam monomer added.
In one embodiment of the invention, the co-nylon 12 particles of S2 have a melting point in the range of 80-180 ℃. The degree of molecular chain regularity is broken through copolymerization, and the melting point of a copolymerization product is regulated and controlled by adjusting the types and the proportion of laurolactam and a comonomer.
In one embodiment of the invention, the solvent of S3 is a polar polyol, preferably one or more of benzyl alcohol, hexafluoroisopropanol, ethanol; preferably, the concentration of the copolymerized nylon 12 solution is 1-40wt%.
In one embodiment of the invention, the adhered copolymerized nylon 12 in S3 comprises 0.1 to 99.9wt%, preferably 1 to 10wt% of the total mass of the nylon 12 powder.
In one embodiment of the invention, the nylon 12 copolymer solution in S3 is used for adhering nylon 12 powder by one or more of dropwise stirring, atomizing spraying and powder infiltration, preferably atomizing spraying.
It is another object of the present invention to provide a high adhesion nylon 12 powder coating.
The high-cohesiveness nylon 12 powder coating is prepared by the preparation method, and is nylon 12 powder adhered with copolymerized nylon 12.
In one embodiment of the invention, the powder coating D50 particle size is 100-200 microns.
It is a further object of the present invention to provide the use of a high adhesion nylon 12 powder coating
The application of the high-cohesiveness nylon 12 powder coating is that the powder coating is obtained by adopting the preparation method or is the powder coating, and the nylon 12 powder coating is used for powder coating of conveying pipelines and containers, powder dip coating of kitchen and bathroom and industrial mechanical parts.
Compared with the prior art, the invention has the following positive effects:
(1) The adhesive has better adhesive force in use, can increase the quality and the service life of products, and meanwhile, the addition of the copolymerized nylon 12 can make the surface of the product coating smoother.
(2) The method can be applied to different scenes by adjusting the performance of the copolymer nylon 12 and matching with nylon 12 powder coating.
Drawings
FIG. 1 is a chart showing the basic nylon 12 powder of example 1, with a particle size of 150 microns;
FIG. 2 is a nylon 12 powder coating obtained in example 1.
Detailed Description
The following examples further illustrate the technical solutions provided by the present invention, but the present invention is not limited to the listed examples, but includes any other known modifications within the scope of the claims.
Main raw material information:
the relative viscosity data in the tables were obtained using ASTM D789-2006 test.
The adhesive force test method refers to the patent GB/T9286-1998 cross-cut test of paint films of colored paint and varnish, and the cross-cut distance is 2mm; an adhesive tape with an adhesion force of more than 10N/25mm was covered on the diced coating, pressed to expel air under the adhesive tape, and then the adhesive tape was pulled up rapidly at an angle perpendicular to the surface of the coating, rated according to GB/T9286.
The test equipment is a hundred-grid knife and is used for uniformly dividing square grids with certain specification and size, and the adhesion degree of the coating film to the substrate is evaluated by evaluating the integrity degree of the coating film in the square grids, and the adhesion degree is expressed as 'grade'. The method is mainly used for measuring the adhesive force of the organic coating by a cross-hatch method, is not only suitable for laboratories, but also can be used for construction sites under various conditions. The design and manufacture are according to ISO2409-1992 standard, and are applicable to GB/T9286-98, BS 3900E6/ASTM D3359.
Example 1
20Kg of nylon 12 (L2000) particles and 100kg of ethanol are added into a precipitation device to be heated to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment to grind for 1h, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 15:75:10, the water quantity is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.3% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 175 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. 8L of the solution is atomized and sprayed into 20kg of nylon 12 powder at the speed of 4L/h, then a too high mixer is used, the rotating speed is set to 150r/min, the dispersion treatment is carried out for 30min, and the mass of the copolymerized nylon accounts for 2% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 2
20Kg of nylon 12 (L2000) particles and 100kg of ethanol are added into a precipitation device to be heated to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 15:75:10, the water quantity is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.3% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 175 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. And atomizing and spraying 16L of the solution into 20kg of nylon 12 powder at a speed of 4L/h, setting the rotating speed to 150r/min by using an overhigh mixer, and carrying out dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 4% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 3
20Kg of nylon 12 (L2000) particles and 100kg of ethanol are added into a precipitation device to be heated to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 15:75:10, the water quantity is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.3% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 175 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. And atomizing and spraying 24L of the solution into 20kg of nylon 12 powder at a speed of 4L/h, setting the rotating speed to 150r/min by using an overhigh mixer, and carrying out dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 6% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 4
20Kg of nylon 12 (L2000) particles and 100kg of ethanol are added into a precipitation device to be heated to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 15:75:10, the water quantity is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.3% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 175 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. And (3) atomizing and spraying 32L of the solution into 20kg of nylon 12 powder at a speed of 4L/h, and then using an overhigh mixer to set the rotating speed to 150r/min, and performing dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 8% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 5
20Kg of nylon 12 (L2000) particles and 100kg of ethanol are added into a precipitation device to be heated to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 15:75:10, the water quantity is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.3% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 175 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. And atomizing and spraying 40L of the solution into 20kg of nylon 12 powder at a speed of 4L/h, setting the rotating speed to 150r/min by using an overhigh mixer, and carrying out dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 10% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 6
20Kg of nylon 12 (L1000) particles and 70kg of ethanol are added into a precipitation device to be heated to 140 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 60 ℃ to separate out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 190 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 15:75:10, the water quantity is 10wt% of the total mass of the monomer, the end capping agent benzoic acid is 1.0% of the total mass of the monomer, the catalyst sodium hypophosphite is 1.0% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 175 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a 10% concentration copolymer nylon 12 dilute solution. And atomizing and spraying 20L of the solution into 20kg of nylon 12 powder at a speed of 2L/h, and then using an overhigh mixer to set the rotating speed to 150r/min for dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 10% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at the temperature of 80 ℃, adding the dried nylon 12 powder into a screening device after drying, setting the upper limit of the size of a screen to be 300 microns, setting the lower limit of the size of the screen to be 50 microns, and obtaining the powder with the particle size D50 of 190 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 7
20Kg of nylon 12 (L3000) particles and 200kg of ethanol are added into a precipitation device to be heated to 190 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 138 ℃ to precipitate nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 110 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 15:75:10, the water quantity is 30wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.2% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.1% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 175 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a 2% concentration copolymer nylon 12 dilute solution. 100L of the solution is atomized and sprayed into 20kg of nylon 12 powder at the speed of 10L/h, then a too high mixer is used, the rotating speed is set to 150r/min, the dispersion treatment is carried out for 30min, and the mass of the copolymer nylon accounts for 10% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 110 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 8
20Kg of nylon 12 (L2000) particles and 100kg of ethanol are added into a precipitation device to be heated to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
A total of 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid are added into a polymerization reactor, the copolymerized nylon 12 is PA11/66/12 copolymer, and the copolymerization ratio PA11/66/12 is 10:80:10, the water amount is 30wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst phosphoric acid is 0.3% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 169 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in hexafluoroisopropanol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. And atomizing and spraying 40L of the solution into 20kg of nylon 12 powder at a speed of 4L/h, setting the rotating speed to 150r/min by using an overhigh mixer, and carrying out dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 10% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 9
20Kg of nylon 12 (L2000) particles and 100kg of ethanol are added into a precipitation device to be heated to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 10:25:65, the water amount is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.3% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 139 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. And atomizing and spraying 40L of the solution into 20kg of nylon 12 powder at a speed of 4L/h, setting the rotating speed to 150r/min by using an overhigh mixer, and carrying out dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 10% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Example 10
20Kg of nylon 12 (L2000) particles and 100kg of ethanol are added into a precipitation device to be heated to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 15:75:10, the water quantity is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.3% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 175 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. And (3) dripping 40L of the solution into 20kg of nylon 12 powder at a uniform speed of 1L/h, setting the rotating speed to 150r/min by using an overhigh mixer, and carrying out dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 10% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Comparative example 1
Prepared by the prior art.
20Kg of nylon 12 particles and 100kg of ethanol are added into a precipitation device, the temperature is raised to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Comparative example 2
In comparison with example 5, the difference is that a non-comonomer coating is used.
20Kg of nylon 12 particles and 100kg of ethanol are added into a precipitation device, the temperature is raised to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
10Kg of caprolactam is added into a polymerization reactor, the water amount is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4% of the total mass of the monomer, the catalyst sodium hypophosphite is 0.3% of the total mass of the monomer, the obtained nylon 6 has a melting point of 224 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the nylon 6 particles are obtained after discharging.
The copolymerized nylon 12 particles are dissolved in benzyl alcohol to prepare nylon 6 dilute solution with the concentration of 5 percent. And atomizing and spraying 40L of the solution into 20kg of nylon 12 powder at a speed of 4L/h, setting the rotating speed to 150r/min by using an overhigh mixer, and carrying out dispersion treatment for 30min, wherein the mass of nylon 6 accounts for 10% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
Comparative example 3
In comparison with example 5, the difference is that a comonomer coating is used which is outside the melting point range.
20Kg of nylon 12 particles and 100kg of ethanol are added into a precipitation device, the temperature is raised to 160 ℃, and the rotating speed of a stirring paddle is set to 100r/min until the nylon 12 is completely dissolved; then, stirring and slowly cooling to 130 ℃, and separating out nylon 12 particles to form spherulitic powder; vacuum drying the obtained powder at 80deg.C for 6 hr, and removing ethanol solvent; then adding the dried powder into grinding equipment, and grinding and dispersing the agglomerated powder; and finally, adding the ground powder into screening equipment, setting the upper limit of the size of a screen to be 300 microns and the lower limit of the size of the screen to be 50 microns, and obtaining the basic nylon 12 powder, wherein the particle size D50 of the powder is 150 microns.
Adding 10kg of laurolactam, caprolactam, hexamethylenediamine and adipic acid into a polymerization reactor, wherein the copolymerized nylon 12 is PA6/66/12 copolymer, and the mass ratio of PA6/66/12 is 20:75:5, the water quantity is 20wt% of the total mass of the monomer, the end capping agent benzoic acid is 0.4 wt% of the total mass of the monomer, the sodium hypophosphite catalyst is 0.3wt% of the total mass of the monomer, the obtained copolymerized nylon 12 has a melting point of 190 ℃, the temperature of the reactor is controlled to be 250 ℃ for ring-opening reaction for 5 hours, the pressure is slowly released to normal pressure, the temperature is slowly reduced to 200 ℃, and the copolymerized nylon 12 particles are obtained after discharging.
The copolymer nylon 12 particles are dissolved in benzyl alcohol to prepare a copolymer nylon 12 dilute solution with the concentration of 5 percent. And atomizing and spraying 40L of the solution into 20kg of nylon 12 powder at a speed of 4L/h, setting the rotating speed to 150r/min by using an overhigh mixer, and carrying out dispersion treatment for 30min, wherein the mass of the copolymerized nylon accounts for 10% of the total mass of the nylon 12 powder. And (3) drying the treated nylon 12 powder for 6 hours at 80 ℃ in vacuum, adding the dried nylon 12 powder into a screening device, setting the upper limit of the size of a screen to 300 microns, setting the lower limit of the size of the screen to 50 microns, and obtaining the powder with the particle size D50 of 150 microns. And then coating the sample plate, and performing a hundred-cell test.
The test results of comparative examples 1-3 and examples 1-5 are as follows:
In conclusion, the nylon 12 powder coating prepared by the method can effectively improve the adhesive force. Those skilled in the art will appreciate that certain modifications and adaptations of the invention are possible and can be made under the teaching of the present specification. Such modifications and adaptations are intended to be within the scope of the present invention as defined in the appended claims.
Claims (6)
1. A method for preparing a high-cohesiveness nylon 12 powder coating, which is characterized by comprising the following steps:
Optionally, S1: mixing nylon 12 particles with a solvent, heating to dissolve, and cooling to a crystallization temperature to precipitate nylon 12 powder;
s2: adding laurolactam, comonomer, end-capping agent, catalyst and water into a polymerization reactor for polymerization to obtain copolymerized nylon 12 particles;
S3: and dissolving the copolymerized nylon 12 particles in a solvent to prepare a solution, adhering the solution to the surface of the nylon 12 powder, and separating, drying and screening to obtain the high-cohesiveness nylon 12 powder coating.
2. The method of claim 1, wherein S1 the nylon 12 has a relative viscosity in the range of 1.4-2.5, preferably 1.6-2.1;
And/or the solvent in S1 is a polar alcohol solvent, preferably one or more of ethanol, benzyl alcohol and hexafluoroisopropanol;
and/or the temperature of S1 is 140-200 ℃;
and/or the concentration of the solution obtained by dissolving S1 is 1-60wt%, preferably 10-40wt%;
and/or, the crystallization temperature of S1 is 25-139 ℃.
3. The method of claim 1, wherein the comonomer S2 is a combination of lactam monomers, organic diacid monomers, and organic diamine monomers; preferably a combination of a C6-C12 lactam monomer, a C2-C30 organic diacid monomer, and a C2-C30 organic diamine monomer; more preferably caprolactam, and one or more of hexamethylenediamine, pentamethylenediamine, decaenediamine, dodecaenediamine, and one or more of adipic acid, sebacic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid;
Preferably, the number of moles of carboxyl groups to moles of amino groups in the composition is 1:1, a step of;
And/or, the mass ratio of laurolactam in S2 in all comonomers is 1% to 99%;
and/or, S2 the end capping agent is an organic carboxylic acid, preferably an organic mono-acid and/or an organic diacid;
Preferably, the end capping agent is added in an amount of 0.1 to 3wt% based on the total mass of the dodecalactam monomer and the comonomer;
And/or the catalyst in S2 is an oxygen-containing phosphorus catalyst, preferably one or more of phosphate radical, phosphite radical and hypophosphite radical;
Preferably, the catalyst is added in an amount of 0.1 to 3wt% based on the total mass of dodecalactam monomer, comonomer and capping agent;
and/or, the addition amount of the water in S2 is 1-30wt% based on the total mass of the dodecalactam monomer;
and/or controlling the melting point range of the copolymerized nylon 12 particles in the step S2 to be 80-180 ℃.
4. The preparation method according to claim 1, wherein the solvent of S3 is one or more of polar polyols, preferably benzyl alcohol, hexafluoroisopropanol, ethanol;
preferably, the concentration of the copolymerized nylon 12 solution is 1-40wt%;
And/or, the adhered copolymerized nylon 12 in the S3 accounts for 0.1-99.9wt% of the total mass of the nylon 12 powder, preferably 1-10wt%;
and/or the nylon 12 solution in S3 adheres to the nylon 12 powder by one or more of dripping stirring, atomizing spraying and powder infiltration, preferably atomizing spraying.
5. A high-cohesiveness nylon 12 powder coating, which is obtained by the preparation method according to any one of claims 1 to 4, characterized in that the powder coating is nylon 12 powder adhered with copolymerized nylon 12;
and/or the powder coating D50 particle size is 100-200 microns.
6. Use of a highly adhesive nylon 12 powder coating obtained by the method of any one of claims 1 to 4 or the powder coating of claim 5 for powder coating of conveying pipes, containers, kitchen and bathroom, industrial mechanical parts.
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