CN110804285A - PET color master batch and preparation method thereof - Google Patents
PET color master batch and preparation method thereof Download PDFInfo
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- CN110804285A CN110804285A CN201911205987.XA CN201911205987A CN110804285A CN 110804285 A CN110804285 A CN 110804285A CN 201911205987 A CN201911205987 A CN 201911205987A CN 110804285 A CN110804285 A CN 110804285A
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- 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
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/04—Pigments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- 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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
Abstract
The invention relates to the technical field of color master batches, in particular to a PET color master batch and a preparation method thereof. The coating comprises the following components in parts by weight: 25-35 parts of carbon black, 60-70 parts of PET return material and 3-7 parts of toner. The PET color master batch is prepared from the carbon black, the PET return material and the toner, wherein the PET return material is a matrix of the PET color master batch and has strong affinity with the carbon black and the like, so that the carbon black, the PET return material and the like can be uniformly dispersed, and the PET color master batch has good compatibility with PET fibers; the color of the PET color master batch can be regulated and controlled by selecting the toner, so that the production requirements of different PET fibers are met. The PET color master batch prepared by the invention has the advantages of good coloring effect and coloring stability, uniform coloring, good appearance quality, stable color and no color difference.
Description
Technical Field
The invention relates to the technical field of color master batches, in particular to a PET color master batch and a preparation method thereof.
Background
PET (polyethylene terephthalate), i.e., polyethylene terephthalate, of the formula [ COC ]6H4COOCH2CH2O]nThe polyester is prepared by exchanging dimethyl terephthalate with glycol ester or esterifying terephthalic acid with glycol to synthesize dihydroxy ethyl terephthalate, and then performing polycondensation reaction. PET belongs to crystalline saturated polyester, is milk white or light yellow and highly crystalline polymer, and has smooth and glossy surface.
At present, there are two main ways of coloring polyester fibers (PET fibers), one is to dye after spinning, so-called "post-dyeing and finishing"; the other method is a dope dyeing method before spinning, namely adding pigment for dyeing before spinning. The former has complex process and higher cost; the latter process is relatively simple and low in cost. The color master batch coloring technology is a dope coloring technology before spinning. The colour master batch is composed of three basic elements of pigment or dye, carrier and additive, and is an aggregate made up by uniformly loading an excessive quantity of pigment in resin, its colouring power is higher than that of pigment itself, and when it is processed, a small quantity of colour master batch and uncoloured resin are mixed together so as to obtain the coloured resin or product with designed pigment concentration. The color master batch coloring method is simple and convenient to operate, accurate in metering, less in equipment pollution, easy to clean, convenient to use and easy to change colors.
However, the method still has some problems in practical application, such as uneven coloring, large color difference, and the like. Therefore, the invention aims to provide the PET color master batch which has good coloring effect and coloring stability, uniform coloring and no color difference.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a PET color masterbatch, which comprises the following components in parts by weight: 25-35 parts of carbon black, 60-70 parts of PET return material and 3-7 parts of toner.
As a preferable technical scheme, the paint comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
As a preferable technical scheme, the average particle size of the carbon black is 350-450 nm.
As a preferable technical scheme, the average particle size of the carbon black is 380-420 nm.
Preferably, the toner is at least one selected from phthalocyanine blue, violet B, B12, mesomarine blue and mesomarine ferric blue.
As a preferable technical proposal, the average particle size of the toner is 600-800 nm.
As a preferable technical scheme, the weight ratio of the carbon black, the PET return material and the toner is (5-8.5): (10-20): 1.
the second aspect of the invention provides a preparation method of PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
As a preferred technical scheme, the melt extrusion temperature is 220-230 ℃.
The third aspect of the invention provides an application of PET color master batch in PET fiber production.
Has the advantages that: the PET color master batch is prepared from the carbon black, the PET return material and the toner, wherein the PET return material is a matrix of the PET color master batch and has strong affinity with the carbon black and the like, so that the carbon black, the PET return material and the like can be uniformly dispersed, and the PET color master batch has good compatibility with PET fibers; the color of the PET color master batch can be regulated and controlled by selecting the toner, so that the production requirements of different PET fibers are met. The PET color master batch prepared by the invention has the advantages of good coloring effect and coloring stability, uniform coloring, good appearance quality, stable color and no color difference.
Detailed Description
The technical features in the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, but the scope of protection of the present invention is not limited thereto.
"preferred", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The first aspect of the invention provides a PET color master batch, which comprises the following components in parts by weight: 25-35 parts of carbon black, 60-70 parts of PET return material and 3-7 parts of toner.
In a preferred embodiment, the composition comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
Carbon black
Carbon black (carbon black), also known as carbon black, is an amorphous carbon. Light, loose and extremely fine black powder with very large surface area ranging from 10 to 3000m2The carbon-containing substance is a product obtained by incomplete combustion or thermal decomposition of a carbon-containing substance (coal, natural gas, heavy oil, fuel oil, etc.) under the condition of insufficient air.
In one embodiment, the carbon black has an average particle size of 350-450 nm.
In a preferred embodiment, the carbon black has an average particle size of 380-420 nm.
In a more preferred embodiment, the carbon black has an average particle size of 400 nm.
In one embodiment, the carbon black is type N330, available from ningburg chemical.
The applicant finds that when the PET color master batch is prepared by adopting the carbon black, the PET return material and the pigment, and the average particle size of the carbon black is controlled to be 350-450nm, and the average particle size of the toner is controlled to be 600-800nm, the prepared PET color master batch has better coloring effect and coloring stability. The applicant speculates that possible reasons are: under specific conditions, carbon black and toner have high kinetic energy, one part of the carbon black and the toner can be adsorbed on the surface of the PET returned material through physical action, the other part of the carbon black and the toner can be adsorbed and diffused into microcracks on the surface of the PET returned material and gaps between PET returned material chains, and meanwhile, the carbon black can penetrate into pores among toner particles, so that the attraction among the toner particles is reduced, and the coloring effect and the coloring stability of the PET color master batch are improved. However, since the carbon black has a small particle size, a large specific surface area, and a large surface free enthalpy, the carbon black is easily agglomerated, thereby affecting the coloring effect and the coloring stability.
In a preferred embodiment, the carbon black is a mixture of carbon black and modified carbon black.
In one embodiment, the weight ratio of carbon black to modified carbon black is 1: (0.8-1.2).
In a preferred embodiment, the weight ratio of the carbon black to the modified carbon black is 1: 1.
in one embodiment, the modified carbon black is prepared by the steps of:
1) mixing 3- (methacryloyloxy) propyl trimethoxy silane and ammonia water, dissolving in ethanol water solution, adding carbon black, performing ultrasonic treatment for 20-40min, stirring at 40-50 ℃ for reaction for 20-24h, washing with ethanol, and drying to obtain a mixture 1;
2) mixing the mixture 1 obtained in the step 1) with absolute ethyl alcohol, performing ultrasonic treatment for 20-40min, adding a 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution while stirring, adding an ammonium persulfate aqueous solution at 40-50 ℃, performing stirring reaction for 3-5h, washing with deionized water, and drying to obtain the modified carbon black.
In a preferred embodiment, the modified carbon black is prepared by the following steps:
1) mixing 3- (methacryloyloxy) propyl trimethoxy silane and ammonia water, dissolving in ethanol water solution, adding carbon black, performing ultrasonic treatment for 30min, stirring at 45 ℃ for reaction for 22h, washing with ethanol, and drying to obtain a mixture 1;
2) mixing the mixture 1 obtained in the step 1) with absolute ethyl alcohol, performing ultrasonic treatment for 30min, adding a 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution while stirring, adding an ammonium persulfate aqueous solution at 45 ℃, performing stirring reaction for 4h, washing with deionized water, and drying to obtain the modified carbon black.
In one embodiment, the weight ratio of 3- (methacryloyloxy) propyltrimethoxysilane, ammonia, ethanol aqueous solution and carbon black is 1: 0.16: 40: 2.
in one embodiment, the aqueous ethanol solution has a concentration of 90% by weight.
In one embodiment, the weight ratio of mixture 1, absolute ethanol, aqueous solution of sodium salt of 4-vinylbenzene methane sulfonate, and aqueous solution of ammonium persulfate is 1: 30: 25: 5.
in one embodiment, the aqueous solution of the sodium salt of 4-vinylbenzenemethanesulphonic acid has a concentration of 36% by weight.
In one embodiment, the aqueous ammonium persulfate solution has a concentration of 9% by mass.
The CAS number of the 3- (methacryloyloxy) propyltrimethoxysilane is 2530-85-0.
The CAS number of the 4-vinyl benzene methane sulfonic acid sodium salt is 10195-45-6.
The CAS number of the ammonium persulfate is 7727-54-0.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The applicant has unexpectedly found that when a mixture of carbon black and modified carbon black is used to prepare a PET color masterbatch together, the weight ratio of carbon black to modified carbon black is controlled to be 1: (0.8 to 1.2), the coloring effect and coloring stability of the prepared PET color master batch can be further improved. The applicant speculates that possible reasons are: the introduction of the modified carbon black provides sufficient electrostatic repulsive force and steric hindrance for carbon black particles, so that van der Waals adsorption among the carbon black particles is weakened; meanwhile, under specific conditions, the carbon black and the modified carbon black have good synergistic effect, and can be combined with PET return materials and the like in a system through various acting forces such as hydrophilic interaction, van der Waals force and the like, so that the coloring effect and the coloring stability of the PET color master batch are improved. And when the weight ratio of the carbon black to the modified carbon black is not 1: in the range of (0.8-1.2), the color master batch prepared has poor coloring effect.
PET feed back
The PET return material, also called PET reclaimed material, is a material formed by reprocessing PET waste material in production or used PET old material.
The PET regrind of the present invention is not particularly limited and may be obtained commercially, for example, PET regrind available commercially includes, but is not limited to, Yueagle Plastic materials, Inc. available in Dongguan.
The PET recycled material is a tool for bearing carbon black and toner, is a matrix of PET color master batch, can be used as a pre-dispersion and stable protection storage chamber for the carbon black and the toner, prevents the carbon black and the toner from agglomerating, and can uniformly disperse the carbon black and the toner into PET fibers after being melted during practical application to finish the coloring function.
Toner powder
Toner, i.e., pigment, dye, is a substance that can color an object.
In one embodiment, the toner is selected from at least one of phthalocyanine blue, violet B, B12, mediterranean blue, and mediterranean ferric blue.
In a preferred embodiment, the toner is phthalocyanine blue.
Phthalocyanine blue is also known as copper phthalocyanine, haliqin blue B, pigment blue, cyanine blue palace, Monas blue B, etc. Belonging to the phthalocyanine pigment series. Molecular formula C32H16CuN8。
In one embodiment, the toner has an average particle size of 600-800 nm.
In a preferred embodiment, the toner has an average particle diameter of 700 nm.
The phthalocyanine blue is purchased from Hangzhou Shurun textile auxiliary Co.
In one embodiment, the weight ratio of carbon black, PET regrind, toner is (5-8.5): (10-20): 1.
in a preferred embodiment, the weight ratio of the carbon black, the PET return material and the toner is 6: 13: 1.
the second aspect of the invention provides a preparation method of PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
In one embodiment, the melt extrusion temperature is 220-230 ℃.
In a preferred embodiment, the melt extrusion temperature is 225 ℃.
The third aspect of the invention provides an application of PET color master batch in PET fiber production.
Hereinafter, the present invention will be described in more detail by way of examples, but it should be understood that these examples are merely illustrative and not restrictive. In addition, the starting materials according to the invention are all commercially available, unless otherwise specified.
Examples
Practice ofExample 1
The embodiment 1 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black had an average particle diameter of 400 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 700 nm.
Embodiment 1 also provides a preparation method of the PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 2
The embodiment 2 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 25 parts of carbon black, 60 parts of PET recycled material and 3 parts of toner.
The carbon black had an average particle diameter of 350 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 600 nm.
Embodiment 2 also provides a preparation method of the PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 3
The embodiment 3 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 35 parts of carbon black, 70 parts of PET recycled material and 7 parts of toner.
The carbon black had an average particle diameter of 450 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 800 nm.
Embodiment 3 also provides a preparation method of the PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 4
The embodiment 4 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black has an average particle diameter of 200 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 700 nm.
Embodiment 4 also provides a preparation method of the PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 5
The embodiment 5 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black had an average particle diameter of 600 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 700 nm.
Embodiment 5 also provides a preparation method of the PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 6
Embodiment 6 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black had an average particle diameter of 400 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 500 nm.
Embodiment 6 also provides a preparation method of the PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 7
Embodiment 7 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black had an average particle diameter of 400 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 900 nm.
Embodiment 7 also provides a preparation method of the PET color master batch, which comprises the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 8
The embodiment 8 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black is a mixture of carbon black and modified carbon black.
The weight ratio of the carbon black to the modified carbon black is 1: 1.
the preparation method of the modified carbon black comprises the following steps:
1) mixing 3- (methacryloyloxy) propyl trimethoxy silane and ammonia water, dissolving in ethanol water solution, adding carbon black, performing ultrasonic treatment for 30min, stirring at 45 ℃ for reaction for 22h, washing with ethanol, and drying to obtain a mixture 1;
2) mixing the mixture 1 obtained in the step 1) with absolute ethyl alcohol, performing ultrasonic treatment for 30min, adding a 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution while stirring, adding an ammonium persulfate aqueous solution at 45 ℃, performing stirring reaction for 4h, washing with deionized water, and drying to obtain the modified carbon black.
The weight ratio of the 3- (methacryloyloxy) propyl trimethoxy silane to the ammonia water to the ethanol water solution to the carbon black is 1: 0.16: 40: 2.
the mass percentage concentration of the ethanol water solution is 90%.
The weight ratio of the mixture 1, the absolute ethyl alcohol, the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution and the ammonium persulfate aqueous solution is 1: 30: 25: 5.
the mass percentage concentration of the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution is 36%.
The mass percentage concentration of the ammonium persulfate aqueous solution is 9%.
The carbon black had an average particle diameter of 400 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 700 nm.
Embodiment 8 also provides a preparation method of the PET color master batch, comprising the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 9
Embodiment 9 of the present invention provides a PET color masterbatch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black is a mixture of carbon black and modified carbon black.
The weight ratio of the carbon black to the modified carbon black is 1: 0.8.
the preparation method of the modified carbon black comprises the following steps:
1) mixing 3- (methacryloyloxy) propyl trimethoxy silane and ammonia water, dissolving in ethanol water solution, adding carbon black, performing ultrasonic treatment for 30min, stirring at 45 ℃ for reaction for 22h, washing with ethanol, and drying to obtain a mixture 1;
2) mixing the mixture 1 obtained in the step 1) with absolute ethyl alcohol, performing ultrasonic treatment for 30min, adding a 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution while stirring, adding an ammonium persulfate aqueous solution at 45 ℃, performing stirring reaction for 4h, washing with deionized water, and drying to obtain the modified carbon black.
The weight ratio of the 3- (methacryloyloxy) propyl trimethoxy silane to the ammonia water to the ethanol water solution to the carbon black is 1: 0.16: 40: 2.
the mass percentage concentration of the ethanol water solution is 90%.
The weight ratio of the mixture 1, the absolute ethyl alcohol, the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution and the ammonium persulfate aqueous solution is 1: 30: 25: 5.
the mass percentage concentration of the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution is 36%.
The mass percentage concentration of the ammonium persulfate aqueous solution is 9%.
The carbon black had an average particle diameter of 400 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 700 nm.
Embodiment 9 also provides a preparation method of the PET color master batch, comprising the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 10
The embodiment 10 of the invention provides a PET color master batch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black is a mixture of carbon black and modified carbon black.
The weight ratio of the carbon black to the modified carbon black is 1: 1.2.
the preparation method of the modified carbon black comprises the following steps:
1) mixing 3- (methacryloyloxy) propyl trimethoxy silane and ammonia water, dissolving in ethanol water solution, adding carbon black, performing ultrasonic treatment for 30min, stirring at 45 ℃ for reaction for 22h, washing with ethanol, and drying to obtain a mixture 1;
2) mixing the mixture 1 obtained in the step 1) with absolute ethyl alcohol, performing ultrasonic treatment for 30min, adding a 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution while stirring, adding an ammonium persulfate aqueous solution at 45 ℃, performing stirring reaction for 4h, washing with deionized water, and drying to obtain the modified carbon black.
The weight ratio of the 3- (methacryloyloxy) propyl trimethoxy silane to the ammonia water to the ethanol water solution to the carbon black is 1: 0.16: 40: 2.
the mass percentage concentration of the ethanol water solution is 90%.
The weight ratio of the mixture 1, the absolute ethyl alcohol, the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution and the ammonium persulfate aqueous solution is 1: 30: 25: 5.
the mass percentage concentration of the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution is 36%.
The mass percentage concentration of the ammonium persulfate aqueous solution is 9%.
The carbon black had an average particle diameter of 400 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 700 nm.
Embodiment 10 also provides a preparation method of a PET color master batch, comprising the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 11
Embodiment 11 of the present invention provides a PET color masterbatch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black is a mixture of carbon black and modified carbon black.
The weight ratio of the carbon black to the modified carbon black is 1: 0.5.
the preparation method of the modified carbon black comprises the following steps:
1) mixing 3- (methacryloyloxy) propyl trimethoxy silane and ammonia water, dissolving in ethanol water solution, adding carbon black, performing ultrasonic treatment for 30min, stirring at 45 ℃ for reaction for 22h, washing with ethanol, and drying to obtain a mixture 1;
2) mixing the mixture 1 obtained in the step 1) with absolute ethyl alcohol, performing ultrasonic treatment for 30min, adding a 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution while stirring, adding an ammonium persulfate aqueous solution at 45 ℃, performing stirring reaction for 4h, washing with deionized water, and drying to obtain the modified carbon black.
The weight ratio of the 3- (methacryloyloxy) propyl trimethoxy silane to the ammonia water to the ethanol water solution to the carbon black is 1: 0.16: 40: 2.
the mass percentage concentration of the ethanol water solution is 90%.
The weight ratio of the mixture 1, the absolute ethyl alcohol, the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution and the ammonium persulfate aqueous solution is 1: 30: 25: 5.
the mass percentage concentration of the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution is 36%.
The mass percentage concentration of the ammonium persulfate aqueous solution is 9%.
The carbon black had an average particle diameter of 400 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 700 nm.
Embodiment 11 also provides a preparation method of a PET color master batch, comprising the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Example 12
Embodiment 12 of the present invention provides a PET color masterbatch, which comprises the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
The carbon black is a mixture of carbon black and modified carbon black.
The weight ratio of the carbon black to the modified carbon black is 1: 2.
the preparation method of the modified carbon black comprises the following steps:
1) mixing 3- (methacryloyloxy) propyl trimethoxy silane and ammonia water, dissolving in ethanol water solution, adding carbon black, performing ultrasonic treatment for 30min, stirring at 45 ℃ for reaction for 22h, washing with ethanol, and drying to obtain a mixture 1;
2) mixing the mixture 1 obtained in the step 1) with absolute ethyl alcohol, performing ultrasonic treatment for 30min, adding a 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution while stirring, adding an ammonium persulfate aqueous solution at 45 ℃, performing stirring reaction for 4h, washing with deionized water, and drying to obtain the modified carbon black.
The weight ratio of the 3- (methacryloyloxy) propyl trimethoxy silane to the ammonia water to the ethanol water solution to the carbon black is 1: 0.16: 40: 2.
the mass percentage concentration of the ethanol water solution is 90%.
The weight ratio of the mixture 1, the absolute ethyl alcohol, the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution and the ammonium persulfate aqueous solution is 1: 30: 25: 5.
the mass percentage concentration of the 4-vinyl benzene methane sulfonic acid sodium salt aqueous solution is 36%.
The mass percentage concentration of the ammonium persulfate aqueous solution is 9%.
The carbon black had an average particle diameter of 400 nm.
The carbon black was N330, available from Ningbo Tai, Zhejiang.
The PET recycle is purchased from Yuying plastics raw materials Co., Ltd, Dongguan city.
The toner is phthalocyanine blue.
The toner has an average particle diameter of 700 nm.
Embodiment 12 also provides a method for preparing a PET color masterbatch, comprising the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
The melt extrusion temperature was 225 ℃.
Performance evaluation
1. Coloring effect
The PET color master batches prepared in the examples 1 to 12 are taken to observe the coloring effect, and the judgment standards are as follows: good-uniform coloring and good appearance quality; better-more uniform coloring and better appearance quality; poor-uneven coloration, poor appearance quality.
2. Stability of coloring
The color stability of the PET color master batches prepared in examples 1 to 12 was observed after 3 months, and the evaluation criteria were as follows: good-stable color without color difference; better-more stable color and less color difference; poor-unstable color, large color difference.
The results are shown in the following table:
TABLE 1 Performance test results of PET color concentrates prepared in examples 1-12
| Coloring effect | Stability of coloring | |
| Example 1 | Is preferably used | Is preferably used |
| Example 2 | Is preferably used | Is preferably used |
| Example 3 | Is preferably used | Is preferably used |
| Example 4 | Difference (D) | Difference (D) |
| Example 5 | Difference (D) | Difference (D) |
| Example 6 | Difference (D) | Difference (D) |
| Example 7 | Difference (D) | Difference (D) |
| Example 8 | Good taste | Good taste |
| Example 9 | Good taste | Good taste |
| Example 10 | Good taste | Good taste |
| Example 11 | Is preferably used | Is preferably used |
| Example 12 | Difference (D) | Difference (D) |
According to experimental results, the PET color master batch prepared by the invention has the advantages of good coloring effect and coloring stability, uniform coloring, good appearance quality, stable color and no color difference.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. The use of some numerical ranges in the claims also includes sub-ranges within their range, and variations in these ranges are also to be construed as being covered by the appended claims where possible.
Claims (10)
1. The PET color master batch is characterized by comprising the following components in parts by weight: 25-35 parts of carbon black, 60-70 parts of PET return material and 3-7 parts of toner.
2. The PET color masterbatch according to claim 1, comprising the following components in parts by weight: 30 parts of carbon black, 65 parts of PET recycled material and 5 parts of toner.
3. The PET color masterbatch according to claim 1 or 2, wherein the average particle size of the carbon black is 350-450 nm.
4. The PET color masterbatch according to claim 3, wherein the carbon black has an average particle size of 380-420 nm.
5. The PET color masterbatch according to claim 1 or 2, wherein the toner is at least one selected from the group consisting of phthalocyanine blue, violet B, B12, mediterranean blue, and mediterranean iron blue.
6. The PET color masterbatch according to claim 5, wherein the average particle size of the toner is 600-800 nm.
7. The PET color masterbatch according to claim 1 or 2, wherein the weight ratio of the carbon black, the PET regrind and the toner is (5-8.5): (10-20): 1.
8. a process for the preparation of a PET masterbatch according to any one of claims 1 to 7, comprising the following steps: and mixing the carbon black, the PET return material and the toner, and then performing melt extrusion, stretching, water cooling and grain cutting to prepare the PET color master batch.
9. The method for preparing PET color masterbatch according to claim 8, wherein the melt extrusion temperature is 220-230 ℃.
10. Use of a PET masterbatch according to any one of claims 1 to 7 in the production of PET fibres.
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| WO2022201977A1 (en) * | 2021-03-25 | 2022-09-29 | 大日精化工業株式会社 | Master batch, resin composition and resin molded body |
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| WO2022201977A1 (en) * | 2021-03-25 | 2022-09-29 | 大日精化工業株式会社 | Master batch, resin composition and resin molded body |
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