CN116656095B - Pearlescent PET master batch and preparation method and application thereof - Google Patents
Pearlescent PET master batch and preparation method and application thereof Download PDFInfo
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- CN116656095B CN116656095B CN202310688547.4A CN202310688547A CN116656095B CN 116656095 B CN116656095 B CN 116656095B CN 202310688547 A CN202310688547 A CN 202310688547A CN 116656095 B CN116656095 B CN 116656095B
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- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 22
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 12
- 239000003549 soybean oil Substances 0.000 claims abstract description 12
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims abstract description 11
- -1 acrylic ester Chemical class 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 230000003678 scratch resistant effect Effects 0.000 claims abstract description 7
- 239000000314 lubricant Substances 0.000 claims abstract description 6
- 238000004040 coloring Methods 0.000 claims abstract description 5
- 230000009471 action Effects 0.000 claims abstract description 4
- 230000000379 polymerizing effect Effects 0.000 claims abstract description 3
- 238000004806 packaging method and process Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 9
- 239000003999 initiator Substances 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims description 2
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000011347 resin Substances 0.000 abstract description 4
- 229920005989 resin Polymers 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 71
- 239000005020 polyethylene terephthalate Substances 0.000 description 71
- 230000000052 comparative effect Effects 0.000 description 33
- 230000000694 effects Effects 0.000 description 25
- 238000003756 stirring Methods 0.000 description 13
- 239000000049 pigment Substances 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 6
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 6
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 4
- 239000004342 Benzoyl peroxide Substances 0.000 description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 235000019198 oils Nutrition 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004970 Chain extender Substances 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- UAUDZVJPLUQNMU-UHFFFAOYSA-N Erucasaeureamid Natural products CCCCCCCCC=CCCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 239000004595 color masterbatch Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 150000002924 oxiranes Chemical group 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/223—Packed additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2433/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2433/12—Homopolymers or copolymers of methyl methacrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a pearlescent PET master batch, a preparation method and application thereof, wherein the pearlescent PET master batch comprises the following raw materials in parts by weight: 75 to 85 parts of PET,8 to 15 parts of PMMA, 3 to 8 parts of toner, 0.2 to 3 parts of compatibilizer, 0.2 to 3 parts of scratch resistant agent and 0.1 to 0.5 part of lubricant; the compatibilizer is formed by polymerizing epoxidized soybean oil acrylic ester and glycidyl methacrylate. The pearlescent master batch has good dispersibility and tinting strength under the action of the reactive chain extension and compatibilizer, and is dust-free and environment-friendly in the processing and using processes. The product of the invention has simple manufacturing process, greatly reduced cost and wide application, and is a novel material with environmental protection and strong functionality. The pearlescent PET master batch manufactured by the process can be directly used for coloring materials in the fields of plastics, paint, coating and the like, and solves the problem of limitation of pearlescent powder in different resin materials.
Description
Technical Field
The invention relates to the technical field of pigments, in particular to a pearlescent PET master batch and a preparation method and application thereof.
Background
The pearl powder is one of the toner, in the production process of the toner, the final procedure is generally to prepare a finished product through filtration, drying and crushing, and the toner is subjected to high temperature in the drying process to easily cause secondary agglomeration of pigment molecules, so that the problems of difficult dispersion, quality reduction, complex processing technology and the like are caused in the subsequent use.
The pearlescent effect is due to TiO 2 Or other metal oxides are coated on the base material, and the light rays are reflected in multiple parallel to form pearl luster. In order to achieve good pearl effect, the addition amount of the pearl powder is large and accounts for about 20% -40% of the total amount of the pearl powder, the surface of the pearl powder is made of metal oxide, the pearl powder is incompatible with resin materials, the dispersibility and the dispersion stability are extremely poor, and the pearl powder needs to be subjected to surface modification, such as a coupling agent, a surfactant, organic silicon and the like, so that the defects of high cost, complex process, substrate limitation and the like of the pearl powder in use are overcome, and the application of the pearl powder in various resin materials is limited. Conventional beadsThe matrix material of the master batch is mainly PP, PE, and the PP and PE are coated with pearl powder, and the prepared finished product has punctiform pearl effect, but is limited by the PP and PE materials and can only be applied to the field of films. PET has good processability and glossiness, but has inferior coating force as PP and PE, and poor effect of adding pearl powder.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art, and solves the problems that the existing pearl powder has large addition amount, high cost, complex manufacturing process and processing process used in master batch subsequently, and no special reaction type chain extension auxiliary agent exists, thereby limiting the application of pearl effect in more matrix materials. The invention aims to provide a pearlescent PET master batch, and a preparation method and application thereof. On the premise of not adding pearl powder, the pearl PET master batch takes polyethylene terephthalate PET as a matrix material, utilizes the characteristics of incompatibility and different mobility of the polyethylene terephthalate PET and polymethyl methacrylate PMMA to generate a mirror surface at the interface between crystalline PET and amorphous PMMA to form planar pearl luster, and adds reactive chain extender Rong Chuji to effectively improve the stability and mechanical property of the composite material, and ensures that the pearl PET master batch has good dispersibility and coloring capability and keeps dust-free and environment-friendly in the processing and using processes.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a pearlescent PET master batch, which comprises the following preparation raw materials in parts by weight: 60 to 90 parts of PET, 5 to 18 parts of PMMA, 1 to 10 parts of toner, 0.01 to 6 parts of compatibilizer, 0.01 to 6 parts of scratch resistant agent and 0.01 to 1 part of lubricant; the compatibilizer is formed by polymerizing epoxidized soybean oil acrylic ester and glycidyl methacrylate.
In some embodiments of the present invention, the pearlescent PET masterbatch comprises the following preparation raw materials in parts by weight: 75 to 85 parts of PET,8 to 15 parts of PMMA, 3 to 8 parts of toner, 0.2 to 3 parts of compatibilizer, 0.2 to 3 parts of scratch resistant agent and 0.1 to 0.5 part of lubricant.
In some embodiments of the invention, the molar ratio of epoxidized soybean oil acrylate to glycidyl methacrylate is 1: (1-5).
In some embodiments of the invention, the toner comprises at least one of carbon black, iron oxide red, cobalt blue, chromium oxide green, chrome yellow, phthalocyanine blue.
In some embodiments of the invention, the scratch resistant agent comprises at least one of AST-50, SR-100, FSX 803.
In some embodiments of the invention, the lubricant comprises at least one of stearic acid, amide, zinc stearate, oleamide, erucamide, calcium stearate.
In a second aspect of the present invention, there is provided a method for preparing the pearlescent PET masterbatch, comprising the steps of:
and according to the composition of the pearlescent PET master batch, stirring and mixing the preparation raw materials uniformly, and blending, extruding, drawing and granulating in a double-screw extruder to obtain the pearlescent PET master batch.
In some embodiments of the present invention, the preparation method of the pearlescent PET masterbatch further comprises the preparation of the compatibilizer, including the following steps: under the inert atmosphere, the epoxidized soybean oil acrylic ester and the glycidyl methacrylate are subjected to polymerization reaction under the action of an initiator to prepare the compatibilizer.
In some embodiments of the invention, the polymerization reaction temperature is 50 ℃ to 200 ℃.
In some embodiments of the invention, the polymerization reaction time is 2 hours to 10 hours.
In some embodiments of the invention, the polymerization reaction comprises reacting at 50 ℃ to 100 ℃ for 1h to 5h, and then heating to 120 ℃ to 200 ℃ for continuing the reaction for 1h to 5h.
In some embodiments of the invention, the polymerization reaction comprises reacting at 80 ℃ to 90 ℃ for 2 hours to 4 hours, and then heating to 130 ℃ to 170 ℃ for 2 hours to 4 hours.
In some embodiments of the invention, the initiator comprises at least one of dicumyl peroxide (DCP), benzoyl Peroxide (BPO), potassium persulfate, ammonium persulfate.
In some embodiments of the invention, the ratio of the molar amount of the initiator to the sum of the molar amounts of the epoxidized soybean oil acrylate and glycidyl methacrylate is (0.1-2): 100; preferably (0.5 to 1.5): 100.
in some embodiments of the invention, the stirring speed of the stirring and evenly mixing is 800 r/min-1200 r/min; the time is 3 min-5 min.
In some embodiments of the invention, the twin screw extruder comprises a co-rotating twin screw extruder.
In some embodiments of the invention, the twin-screw extruder has a screw diameter d=40 mm to 62mm, an aspect ratio L/d= (20 to 48): 1, and a host rotation speed of 450Hz to 550Hz; the screw barrel temperature control is set as follows: 180-200 ℃ in zone 1, 200-220 ℃ in zone 2, 220-240 ℃ in zone 3-11, and 230-250 ℃ in die head temperature.
In some embodiments of the invention, the dicing comprises water-cooled dicing.
In some embodiments of the invention, the method for preparing the pearlescent PET master batch further comprises drying after granulating; the drying conditions comprise relative humidity of 45-50%, temperature of 15-25 ℃ and time of 10-15 h.
In a third aspect of the invention, a masterbatch is provided comprising the pearlescent PET masterbatch.
In a fourth aspect, the invention provides an application of the pearlescent PET master batch and/or the color master batch in coloring daily chemical packaging bottles.
In order to reduce scratches and pits generated by friction and collision of the daily-use packaging bottle body in the production, transportation and use processes, the scratch-resistant agent is added. The lubricant is added to improve the surface quality of the bottle body, so that the surface of the bottle body is smoother, the glossiness is better, and the pearl effect is better.
The beneficial effects of the invention are as follows: the invention does not add pearl powder at all, and the flow rates of PET and PMMA are stable and uniform during processing, and different flow rates enable the two materials to form a mirror surface, so that the invention has a planar pearl effect. The pearlescent master batch has good dispersibility and tinting strength under the action of the reactive chain extension and compatibilizer, and is dust-free and environment-friendly in the processing and using processes. The product of the invention has simple manufacturing process, greatly reduced cost and wide application, and is a novel material with environmental protection and strong functionality. The pearlescent PET master batch manufactured by the process can be directly used for coloring materials in the fields of plastics, paint, coating and the like, and solves the problem of limitation of pearlescent powder in different resin materials.
Drawings
FIG. 1 is a physical diagram of the product of example 1.
FIG. 2 is a FTIR spectrum of the product of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or apparatus used in the examples and comparative examples were either commercially available from conventional sources or may be obtained by prior art methods unless specifically indicated. Unless otherwise indicated, assays or testing methods are routine in the art.
In the following examples or comparative examples, the preparation method of the compatibilizer auxiliary comprises the following steps:
firstly, adding a certain amount of epoxidized soybean oil into a flask with a condenser tube and a dropping funnel, heating an oil bath to 85 ℃ and keeping stirring, wherein the molar ratio of the epoxidized soybean oil to the oil bath is 1:2 drops of the mixed solution of acrylic acid (triphenylphosphine and hydroquinone inhibitor which are catalysts containing 1% of the molar ratio of the acrylic acid) are added, the dropping speed is controlled, and the temperature is raised while dropping. After the mixed solution is added dropwise, the temperature of the oil is ensured to be increased to 110 ℃ and the constant temperature reaction is kept until the acid value of the system is 5mg KOH/g, so that epoxidized soybean oil acrylic ester is obtained; then, epoxy soybean oil Acrylate (AESO), glycidyl Methacrylate (GMA) were mixed in a molar ratio of 1:2, adding dicumyl peroxide (DCP) or Benzoyl Peroxide (BPO) with the total monomer mole number of 1% as an initiator, fully stirring to uniformly mix raw materials, putting the uniformly mixed raw material liquid into a reaction kettle, charging nitrogen, setting the temperature to be 80-90 ℃, setting the reaction time to be 3 hours, then heating to 150 ℃ for continuous reaction for 3 hours, taking out a product after the reaction, drying and crushing for standby, and obtaining the compatibilizer auxiliary agent.
Fig. 1 is a physical diagram of the obtained compatibilizer, and it can be seen that the obtained compatibilizer is a pale yellow solid.
FIG. 2 is a FTIR image of the chain extender prepared in example 1.
As can be seen from FIG. 2, 2929cm -1 And 2856cm -1 Respectively polyolefin chain segment-CH 2 Asymmetric stretching vibration and symmetric stretching vibration peak of 1462cm -1 is-CH 2 Bending vibration peak of 725cm -1 is-CH 2 - (n.gtoreq.4) in-plane rocking oscillation peak. Furthermore, 1738cm -1 Characteristic peak of-c=o-, 1171cm -1 is-CH 3 And the characteristic peaks of the epoxide groups, the above results prove that the chain-extending compatibilizing auxiliary is successfully prepared by initiating the polymerization reaction.
Example 1
The highlight multicolor pearlescent PET master batch of the embodiment comprises the following components in parts by weight: 84 parts of PET,9 parts of PMMA,4 parts of pigment blue 60,2 parts of Rong Chuji, 0.6 part of SR-100 and 0.4 part of stearic acid.
The preparation method of the pearlescent PET master batch in the embodiment comprises the following steps: firstly, weighing the raw materials in parts by weight; then the raw materials are put into a high-speed mixer for stirring, and the raw materials are stirred for 5min under the condition that the stirring speed is 1100r/min, so that the raw materials are uniformly mixed; and then the evenly mixed raw materials are put into a co-rotating double screw extruder for blending, extrusion, traction and granulating to obtain master batch primary products. Wherein, the screw diameter D=62 mm, the length-diameter ratio L/D=48 of the homodromous double-screw extruder, the rotating speed of the main machine is 490Hz, and the temperature control of the screw cylinder is set as follows: zone 1200 ℃, zone 2, zone 220 ℃, zone 3-11, zone 240 ℃, die head temperature 250 ℃, and the granulating mode is water-cooling granulating; and finally, drying the master batch primary product for 12 hours under the conditions of 45% of relative humidity and 25 ℃ to obtain a finished product of the highlight magic color pearlescent PET master batch.
The pearlescent PET master batch prepared in the embodiment has the pearlescent grade of 2 (obvious pearlescent effect), and the daily chemical packaging bottle prepared by using the master batch has the scratch resistance DeltaL of 1.1; the gloss GU60℃was 87.
Example 2
The highlight multicolor pearlescent PET master batch of the embodiment comprises the following components in parts by weight: 85 parts of PET,9 parts of PMMA,2.5 parts of pigment yellow 128,0.5 parts of Rong Chuji, 1.8 parts of FSX803 and 0.2 part of oleamide.
The preparation method of the pearlescent PET master batch in the embodiment comprises the following steps: firstly, weighing the raw materials in parts by weight; then the raw materials are put into a high-speed mixer for stirring, and the stirring speed is 1000r/min for 4min, so that the raw materials are uniformly mixed; and then the evenly mixed raw materials are put into a co-rotating double screw extruder for blending, extrusion, traction and granulating to obtain master batch primary products. Wherein, the screw diameter D=62 mm, the length-diameter ratio L/D=48 of the homodromous double-screw extruder, the rotating speed of the main machine is 490Hz, and the temperature control of the screw cylinder is set as follows: zone 1200 ℃, zone 2, zone 220 ℃, zone 3-11, zone 240 ℃, die head temperature 250 ℃, and the granulating mode is water-cooling granulating; and finally, drying the master batch primary product for 12 hours under the conditions of 45% of relative humidity and 25 ℃ to obtain a finished product of the highlight magic color pearlescent PET master batch.
The pearlescent PET master batch prepared in the embodiment has the pearlescent grade of 2 (obvious pearlescent effect), and the daily chemical packaging bottle prepared by using the master batch has the scratch resistance DeltaL of 0.7; the gloss GU60℃was 83.
Example 3
The highlight multicolor pearlescent PET master batch of the embodiment comprises the following components in parts by weight: 83 parts of PET,8 parts of PMMA,5 parts of pigment red 10,1 part of increase Rong Chuji, 2.5 parts of AST-50 and 0.5 part of oleamide.
The preparation method of the pearlescent PET master batch in the embodiment comprises the following steps: firstly, weighing the raw materials in parts by weight; then the raw materials are put into a high-speed mixer for stirring, and the raw materials are stirred for 4min under the condition that the stirring speed is 1100r/min, so that the raw materials are uniformly mixed; and then the evenly mixed raw materials are put into a co-rotating double screw extruder for blending, extrusion, traction and granulating to obtain master batch primary products. Wherein, the screw diameter D=62 mm, the length-diameter ratio L/D=48 of the homodromous double-screw extruder, the rotating speed of the main machine is 490Hz, and the temperature control of the screw cylinder is set as follows: zone 1200 ℃, zone 2, zone 220 ℃, zone 3-11, zone 240 ℃, die head temperature 250 ℃, and the granulating mode is water-cooling granulating; and finally, drying the master batch primary product for 12 hours under the conditions of 45% of relative humidity and 25 ℃ to obtain a finished product of the highlight magic color pearlescent PET master batch.
The pearlescent PET master batch prepared in the embodiment has the pearlescent grade of 2 (obvious pearlescent effect), and the daily chemical packaging bottle prepared by using the master batch has the scratch resistance DeltaL of 0.5; the gloss GU60℃was 86.
Comparative example 1
The PET master batch of the comparative example comprises the following components in parts by weight: 84 parts of PET,9 parts of PMMA,6 parts of pigment blue 60,0.6 parts of SR-100 and 0.4 part of stearic acid.
The preparation method of the PET master batch in the embodiment comprises the following steps: firstly, weighing the raw materials in parts by weight; then the raw materials are put into a high-speed mixer for stirring, and the raw materials are stirred for 5min under the condition that the stirring speed is 1100r/min, so that the raw materials are uniformly mixed; and then the evenly mixed raw materials are put into a co-rotating double screw extruder for blending, extrusion, traction and granulating to obtain master batch primary products. Wherein, the screw diameter D=62 mm, the length-diameter ratio L/D=48 of the homodromous double-screw extruder, the rotating speed of the main machine is 490Hz, and the temperature control of the screw cylinder is set as follows: zone 1200 ℃, zone 2, zone 220 ℃, zone 3-11, zone 240 ℃, die head temperature 250 ℃, and the granulating mode is water-cooling granulating; and finally, drying the master batch primary product for 12 hours under the conditions of 45% of relative humidity and 25 ℃ to obtain the pearlescent PET master batch finished product.
The pearl grade of the PET master batch prepared in the comparative example is 2 (obvious pearl effect), and the scratch resistance DeltaL of the daily chemical packaging bottle prepared by using the master batch is 1.1; the gloss GU60℃is 82.
Comparative example 2
The PET master batch of the comparative example comprises the following components in parts by weight: 95 parts of PET,2 parts of pigment red 10,1 part of increase Rong Chuji and 2 parts of AST-50.
The preparation method of the PET master batch of this comparative example is referred to comparative example 1.
The PET master batch prepared in the comparative example has a pearl grade of 0 (no pearl effect), and the daily chemical packaging bottle prepared by using the master batch has a scratch resistance DeltaL of 0.5; the gloss GU60℃was 79.
Comparative example 3
The PET master batch of the comparative example comprises the following components in parts by weight: 75 parts of PET,20 parts of PMMA,2.7 parts of pigment yellow 128,0.5 parts of Rong Chuji and 0.8 part of oleamide.
The preparation method of the PET master batch of this comparative example is referred to comparative example 1.
The PET master batch prepared in the comparative example has a pearl level of 1 (unobvious pearl effect), and the daily chemical packaging bottle prepared by using the master batch has a scratch resistance delta L of 2.3; the gloss GU60℃is 82.
Comparative example 4
The PET master batch of the comparative example comprises the following components in parts by weight: 85 parts of PET,9 parts of PMMA,2.5 parts of pigment yellow 128,2.0 parts of AESO,1.8 parts of FSX803 and 0.2 part of oleamide.
The preparation method of the PET master batch of this comparative example is referred to comparative example 1.
The PET master batch prepared in the comparative example has a pearl level of 1 (unobvious pearl effect), and the daily chemical packaging bottle prepared by using the master batch has a scratch resistance DeltaL of 0.7; the gloss GU60℃was 83.
Comparative example 5
The PET master batch of the comparative example comprises the following components in parts by weight: 85 parts of PET,9 parts of PMMA,2.5 parts of pigment yellow 128,2.0 parts of GMA,1.8 parts of FSX803 and 0.2 part of oleamide.
The preparation method of the PET master batch of this comparative example is referred to comparative example 1.
The PET master batch prepared in the comparative example has a pearl level of 1 (unobvious pearl effect), and the daily chemical packaging bottle prepared by using the master batch has a scratch resistance DeltaL of 0.7; the gloss GU60℃is 82.
Scratch resistance test in examples and comparative examples: according to the method GME60280, a scratch resistance tester and a color meter are adopted, a cross scratch test is utilized to scratch a grid on the surface of a material at fixed load and interval, the color change at a scratch is measured, the blushing degree represented by an DeltaL value is used for representing the scratch resistance of the material, and the larger the DeltaL value is, the worse the scratch resistance of the material is.
Gloss test: according to the standard GB/T8807, the high-precision gloss meter is adopted to test the gloss of each sample, the test master batch is pressed into sheets with certain thickness by a flat vulcanizing machine, the sample sheets are put into the gloss meter to test the gloss, and the medium gloss (general angle) is adopted: the test was performed at 60 ° and the results recorded.
Pearlescent property grade was rated on three scales of 0,1, 2, wherein: the level 0 indicates no pearl effect, the level 1 indicates no obvious pearl effect, and the level 2 indicates obvious pearl effect. The pearlescent performance grade test method specifically comprises the following steps: after detecting a template to be prepared by a professional in an indoor standard state, the template is visually inspected under natural light to check whether the template is defect-free, and is compared with a standard template. In addition, the gloss of the sample was measured, and the surface of the sample was irradiated with a beam of light, and the gloss of the sample was observed, thereby judging the pearlescent effect.
As can be seen from the test results, compared with comparative examples 2 and 3, the PET master batch prepared by adding a certain amount of PMMA with lower melting point than PET into the PET matrix reduces the crystallization temperature of PET, promotes the growth of PET crystal nuclei, accelerates the crystallization rate of PET crystal nuclei, and forms a mirror surface between crystalline opaque PET and transparent PMMA in a PET and PMMA blending system, thereby generating obvious planar pearl luster, and the adding amount of PMMA is optimal by 8% -9%.
As is clear from examples 1 to 3 and comparative example 1, the pearlescent effect and the glossiness of the master batch are improved after the compatibilizer is added, and the glossiness is positively correlated to the addition amount of the compatibilizer, namely, example 1 > example 3 > example 2 > comparative example 1.
As can be seen from comparative example 2: when PMMA is not added into the PET matrix, the PET is in a single transparent amorphous state, a mirror surface cannot be formed, and the master batch cannot achieve the pearl effect.
As can be seen from comparative example 3: when PMMA is excessively added into the PET matrix, PMMA becomes impurities, and blocks the movement of chain segments, so that crystal nuclei are not easy to generate, the crystallization rate is reduced, the formation of a mirror surface is not facilitated, the pearlescent effect of the master batch is poor, and the scratch resistance is poor because no scratch resistance agent is added.
As is clear from comparative example 4, when AESO alone is used as a compatibilizer, the effect of use is not achieved due to insufficient reactivity, and the pearlescent effect and the glossiness are inferior to those of example 2.
As is clear from comparative example 5, when GMA alone is used as a compatibilizer, the desired effect of compatibilization is not achieved due to its smaller molecular weight, and the gloss is inferior to that of example 2.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (9)
1. The pearlescent PET master batch is characterized in that: the preparation raw materials comprise the following components in parts by weight: 60-90 parts of PET, 5-18 parts of PMMA, 1-10 parts of toner, 0.01-6 parts of compatibilizer, 0.01-6 parts of scratch resistant agent and 0.01-1 part of lubricant; the compatibilizer is formed by polymerizing epoxidized soybean oil acrylic ester and glycidyl methacrylate; the molar ratio of the epoxidized soybean oil acrylic ester to the glycidyl methacrylate is 1: (1-5).
2. The pearlescent PET masterbatch of claim 1, wherein: the toner comprises at least one of carbon black, iron oxide red, cobalt blue, chromium oxide green, chrome yellow and phthalocyanine blue.
3. The pearlescent PET masterbatch of claim 1, wherein: the scratch resistant agent comprises at least one of AST-50, SR-100 and FSX 803.
4. A method for preparing the pearlescent PET masterbatch according to any one of claims 1 to 3, characterized in that: the method comprises the following steps:
according to the composition of the pearlescent PET master batch according to any one of claims 1-3, the preparation raw materials are stirred and mixed uniformly, and the pearlescent PET master batch is prepared by blending, extruding, drawing and granulating in a double-screw extruder.
5. The method for preparing pearlescent PET masterbatch according to claim 4, characterized in that: the preparation method of the pearlescent PET master batch also comprises the preparation of the compatibilizer auxiliary agent, and comprises the following steps: under the inert atmosphere, the epoxidized soybean oil acrylic ester and the glycidyl methacrylate are subjected to polymerization reaction under the action of an initiator to prepare the compatibilizer.
6. The method for preparing the pearlescent PET master batch according to claim 5, wherein the method comprises the following steps: the temperature of the polymerization reaction is 50-200 ℃.
7. The method for preparing the pearlescent PET master batch according to claim 5, wherein the method comprises the following steps: the polymerization reaction time is 2-10 h.
8. A masterbatch comprising the pearlescent PET masterbatch of any one of claims 1-3.
9. Use of the pearlescent PET masterbatch according to any one of claims 1 to 3 and/or the masterbatch according to claim 8 for coloring daily chemical packaging bottles.
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