CN111234446A - Preparation of coated iron oxide yellow color master batch - Google Patents

Preparation of coated iron oxide yellow color master batch Download PDF

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Publication number
CN111234446A
CN111234446A CN202010173301.XA CN202010173301A CN111234446A CN 111234446 A CN111234446 A CN 111234446A CN 202010173301 A CN202010173301 A CN 202010173301A CN 111234446 A CN111234446 A CN 111234446A
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iron oxide
oxide yellow
coated iron
preparation
coated
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徐海英
魏海
吴永光
徐军
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Shanghai Jinzhu Color Masterbatch Co ltd
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Shanghai Jinzhu Color Masterbatch Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/22Compounds of iron
    • C09C1/24Oxides of iron
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10Treatment with macromolecular organic compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2435/00Characterised 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 at least one being terminated by a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Derivatives of such polymers
    • C08J2435/06Copolymers with vinyl aromatic monomers
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2451/00Characterised 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
    • C08J2451/04Characterised 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 grafted on to rubbers
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2455/00Characterised by the use of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08J2423/00 - C08J2453/00
    • C08J2455/02Acrylonitrile-Butadiene-Styrene [ABS] polymers
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2272Ferric oxide (Fe2O3)
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/10Esters; Ether-esters
    • C08K5/101Esters; Ether-esters of monocarboxylic acids
    • C08K5/103Esters; Ether-esters of monocarboxylic acids with polyalcohols
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/13Phenols; Phenolates
    • C08K5/134Phenols containing ester groups
    • C08K5/1345Carboxylic esters of phenolcarboxylic acids
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K5/16Nitrogen-containing compounds
    • C08K5/20Carboxylic acid amides
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/34Heterocyclic compounds having nitrogen in the ring
    • C08K5/3412Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
    • C08K5/3432Six-membered rings
    • C08K5/3435Piperidines
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
    • C08K5/52Phosphorus bound to oxygen only
    • C08K5/524Esters of phosphorous acids, e.g. of H3PO3
    • C08K5/526Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients

Abstract

The invention relates to the technical field of high polymer materials, and in particular relates to preparation of a coated iron oxide yellow color master batch, which mainly comprises 30-65 parts of ABS resin, 5-15 parts of heat-resistant agent, 6-12 parts of toughening agent, 2-8 parts of antioxidant, 0.1-0.6 part of light stabilizer, 0.2-5 parts of lubricant and 0.4-10 parts of coated coloring agent.

Description

Preparation of coated iron oxide yellow color master batch
Technical Field
The invention relates to the technical field of high polymer materials, and particularly relates to preparation of a coated iron oxide yellow color master batch.
Background
With the development of society, the application of plastic products has penetrated into various fields of society. By using inorganic pigments of different colors, a plastic product can be given a rich and colorful appearance. However, the plastics as the high molecular organic material have poor compatibility with inorganic pigments, and if the inorganic pigments are not pretreated, the inorganic pigments are difficult to be uniformly dispersed in the plastics, thereby affecting the appearance quality and the service life of the product.
Yellow iron oxide, also known as iron oxyhydroxide, having hydroxyl functional groups on its surface, is not useful as a colorant in two ways: poor heat resistance and poor dispersibility. At present, the easily dispersible iron oxide yellow on the market is mainly obtained by physical method (mechanical grinding), but during grinding production, dust is easily generated, the environment is polluted, and the health of workers is harmed. The easily dispersible iron oxide yellow can also be obtained by chemical treatment. The invention discloses a method for preparing easily-dispersible iron oxide yellow by modifying the surface of ammonia process iron oxide yellow (CN 201410440986.4). The invention uses water as a medium, and adopts a stirring and beating mode to pretreat an ammonia process iron oxide yellow filter cake to obtain slurry with uniformly dispersed water phase, and then adds a super dispersant emulsion, and utilizes the hydroxyl group of the iron oxide yellow and the anchor group of the amino group of the super dispersant to form a hydrogen bond under a certain pH condition, and the solvation chain of the super dispersant coats the iron oxide yellow to modify the surface of the iron oxide yellow to obtain the easily-dispersible iron oxide yellow dispersed particles. Chinese application patent (CN 201710310972.4) discloses a heat-resistant easily-dispersible iron oxide yellow pigment and a preparation method thereof. Soluble calcium salt, sodium hexametaphosphate and sodium hydroxide are used as reaction raw materials, an ultrasonic dispersion technology is introduced in the coating process, calcium phosphate is coated on the surface of the iron oxide yellow pigment through reaction, and then organic treatment and modification are carried out on the surface of the iron oxide yellow pigment, so that the formed composite material improves the heat resistance and the dispersibility of the iron oxide yellow and can be used as a coloring agent in plastic processing and powder coating application. The Chinese application patent (CN 201810194542.5) adopts a high-temperature high-pressure powder depolymerization dispersion technology, the heat resistance of the iron oxide yellow is improved by a composite material formed by coating the iron oxide yellow with aluminum oxide and zinc oxide, the composite material can be used as a coloring agent and a preservative when being applied to plastic processing and powder coating, and the zinc oxide can inhibit the generation of a later-stage iron oxide yellow red phase to a certain extent so as to ensure that the color is purer.
From patent analysis, many existing patents are directed to improving the heat resistance and poor dispersion of iron oxide yellow by coating the iron oxide yellow with an inorganic material. The application of iron oxide yellow coated with organic materials in color masterbatches is rarely reported.
Disclosure of Invention
In order to overcome the defects of dispersibility and heat resistance of the iron oxide yellow in plastic processing, a polymer coating layer is formed on the surface of the iron oxide yellow, and the dispersibility and the heat resistance of the iron oxide yellow in the color master batch resin are improved through the polymer coating layer. The specific technical scheme is as follows:
the preparation method of the coated iron oxide yellow color master batch comprises the following components in percentage by weight:
ABS resin 30 to 65 portions of
Heat-resistant agent 5 to 15 portions of
Toughening agent 6 to 12 portions of
Antioxidant agent 2 to 8 portions of
Light stabilizers 0.1 to 0.6 portion
Lubricant agent 0.2 to 5 portions of
Coated colorant 0.4 to 10 portions of
Preferably, the heat-resistant agent prepared by the coated iron oxide yellow color master batch is one or two of styrene-maleic anhydride copolymer and styrene- (N-phenylmaleimide) -maleic anhydride copolymer;
preferably, the toughening agent prepared by the coated iron oxide yellow color master batch is one or more of methyl methacrylate-butadiene-styrene copolymer, styrene-butadiene-styrene copolymer and ethylene-methyl acrylate-glycidyl methacrylate copolymer;
preferably, the antioxidant prepared from the coated iron oxide yellow color master batch is one or more of hindered phenols, phosphites and thioesters;
preferably, the coated iron oxide yellow color master batch is used for preparing one or more of hindered amines and benzotriazoles of light stabilizers;
preferably, the lubricant prepared by the coated iron oxide yellow color master batch is one or a combination of more than one of stearic acid, ethylene bis stearamide and pentaerythritol stearate;
preferably, the coated colorant prepared from the coated iron oxide yellow color master batch is iron oxide yellow coated by acrylic emulsion;
preferably, the acrylic emulsion-coated iron oxide yellow is subjected to a grafting reaction with one or more of vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (6-methoxyethoxy) silane and gamma-methacryloxypropyltrimethoxysilane;
preferably, the acrylic emulsion is obtained by copolymerizing acrylate compounds under the action of an initiator, ultrapure water and an emulsifier.
Preferably, the mass ratio of the acrylate compound, the initiator, the ultrapure water and the emulsifier in the acrylic emulsion is 80-100: 1-15: 100-1000 parts of: 10 to 50.
Preferably, the acrylic ester compound in the acrylic emulsion is one or more of methyl methacrylate, ethyl methacrylate, lauryl methacrylate, n-butyl methacrylate and tert-butylaminoethyl methacrylate.
Preferably, the initiator of the acrylic emulsion is at least one of azobisisobutyronitrile, azobisisoheptonitrile, benzoyl peroxide and dilauroyl peroxide.
Preferably, the emulsifier of the acrylic emulsion is one or more of sodium dodecyl sulfate, span 60, span 80, tween 80 and tween 65.
Preferably, the preparation method of the coated iron oxide yellow color master batch comprises the following steps:
①, preparing ethanol and water solution with the volume of 5-20: 1, adding acetic acid to adjust the pH value to 4-5, adding a silane grafting agent under stirring, controlling the silane concentration to be 2-7%, and standing for 10-30 minutes to fully hydrolyze the silane.
② adding a certain amount of iron oxide yellow into the silane solution obtained in step ① while stirring, reacting for 1 hour at 40 ℃, filtering and washing with deionized water, and drying at 85 ℃.
③ putting emulsifier, ferric oxide yellow grafted with silane and ultrapure water into a flask, heating to 65-75 ℃, starting stirring to control the rotation speed to 800-900 r/min, stirring for at least 30 minutes to uniformly mix the priming material, adding an initiator into the reaction flask, after the temperature is stable, dropwise adding an acrylate compound into the reaction system by using a constant-pressure dropping funnel, controlling the dropwise adding time to be 1 hour, keeping the temperature for 1 hour after the dropwise adding is finished, cooling to 45 ℃, and filtering to obtain the coated ferric oxide yellow.
④ mixing ABS resin, heat-resistant agent and toughening agent in a high-speed mixer for 3-5 minutes, adding antioxidant, light stabilizer, lubricant and coated iron oxide yellow into the high-speed mixer for 3-5 minutes, adding the mixed particles into a double-screw extruder for melt extrusion, granulation, drying, cooling and packaging, wherein the rotation speed of the high-speed mixer is 200-600 r/min, and the rotation speed of the high-speed mixer is 700-1000 r/min.
Compared with the prior art, this patent, its advantage lies in:
① the ABS resin contains side phenyl, cyano and unsaturated double bond, it has better compatibility with many polymers, the iron oxide yellow coated by acrylic resin with different structures can be dispersed evenly in the ABS resin without grinding.
② has good heat resistance because the hydroxyl group of iron oxide yellow is converted into a silicon-oxygen bond by a chemical reaction with the polymer during storage, and thus color fading due to loss of the hydroxyl group does not occur at high temperature.
③ the color of the color master batch is long, because the iron oxide yellow coated by the polymer is connected with the coating layer by chemical bond, compared with the inorganic material which adopts ionic bond and Van der Waals force, the color master batch is more stable, thereby effectively avoiding the direct contact of external light, heat and oxygen and improving the long-term color of the color master batch.
The specific implementation mode is as follows:
example 1:
preparing ethanol and water solution with the volume of 5:1, adding acetic acid to adjust the pH value to 4-5, adding vinyl triethoxysilane while stirring, controlling the silane concentration to be 5%, and standing for 30 minutes to fully hydrolyze the silane.
30g of iron oxide yellow is added into the silane solution obtained in the step ① under the condition of stirring, reacted for 1 hour at 40 ℃, filtered and washed by deionized water, and then dried at 85 ℃.
Under the nitrogen atmosphere, 5g of Tween 80, 7g of span 80, 23g of vinyltriethoxysilane grafted iron oxide yellow and 100mL of ultrapure water are put into a flask, heated to 75-81 ℃, stirred at 800-1000 rpm, and stirred for at least 30 minutes to uniformly mix the priming materials. 0.55g of azobisisobutyronitrile was added to the reaction flask, and the temperature was stabilized. 57g of methyl methacrylate and 13g of lauryl methacrylate were added dropwise to the reaction system using a constant pressure dropping funnel. The dropping time is controlled to be 1 hour, and the temperature is kept for 1 hour after the dropping is finished. After the reaction time is over, the temperature is reduced to 45 ℃, and the coated iron oxide yellow with the particle size of 15.77 mu m is obtained by filtering with filter cloth.
42g of ABS resin, 13g of styrene-maleic anhydride copolymer and 6g of methyl methacrylate-butadiene-styrene copolymer are mixed in a high-speed mixer for 3-5 minutes, wherein the rotating speed of the high-speed mixer is 600-800 revolutions per minute. Then adding 4.2g of antioxidant 1010, 0.3g of light stabilizer UV770, 1g of ethylene bis stearamide and coated iron oxide yellow into a high-speed mixer, and mixing for 3-5 minutes, wherein the rotating speed of the high-speed mixer is 200-500 revolutions per minute; and adding the mixed particles into a double-screw extruder for melt extrusion, granulation, drying, cooling and packaging.
Example 2:
preparing ethanol and water solution with the volume of 5:1, adding acetic acid to adjust the pH value to 4-5, adding vinyl tri (6-methoxyethoxy) silane under stirring, controlling the silane concentration to be 6%, and standing for 30 minutes to fully hydrolyze the silane.
Under stirring, 35g of iron oxide yellow was added to the silane solution of step ①, reacted at 40 ℃ for 1 hour, washed with deionized water by suction filtration, and then dried at 85 ℃.
Under the nitrogen atmosphere, 10g of span 80, 15g of vinyl tris (6-methoxyethoxy) silane grafted iron oxide yellow and 80mL of ultrapure water are put into a flask, heated to 75-81 ℃, stirred at 800-1000 rpm for at least 30 minutes to uniformly mix the priming materials. 0.6g of azobisisobutyronitrile was added to the reaction flask, and the temperature was stabilized. 45g of methyl methacrylate was added dropwise to the reaction system using a constant pressure dropping funnel. The dropping time is controlled to be 1 hour, and the temperature is kept for 1 hour after the dropping is finished. After the reaction time is over, the temperature is reduced to 45 ℃, and the coated iron oxide yellow with the particle size of 12.66 mu m is obtained by filtering with filter cloth.
60g of ABS resin, 11g of styrene- (N-phenylmaleimide) -maleic anhydride and 7g of methyl methacrylate-butadiene-styrene copolymer are mixed in a high-speed mixer for 3 to 5 minutes, wherein the rotating speed of the high-speed mixer is 600 to 800 revolutions per minute. Then adding 8g of antioxidant 626, 0.4g of light stabilizer UV783, 0.4g of ethylene bis stearamide and 2.8g of coated iron oxide yellow into a high-speed mixer, and mixing for 3-5 minutes, wherein the rotating speed of the high-speed mixer is 200-500 revolutions per minute; and adding the mixed particles into a double-screw extruder for melt extrusion, granulation, drying, cooling and packaging.
Example 3:
preparing ethanol and water solution with the volume of 5:1, adding acetic acid to adjust the pH value to 4-5, adding gamma-methacryloxypropyl trimethoxy silane while stirring, controlling the silane concentration to be 5%, and standing for 20 minutes to fully hydrolyze the silane.
32g of iron oxide yellow is added into the silane solution obtained in the step ① under stirring, reacted for 1 hour at 40 ℃, filtered and washed by deionized water, and then dried at 85 ℃.
Under the nitrogen atmosphere, 6g of span 60, 7g of Tween 85, 17 g of gamma-methacryloxypropyltrimethoxysilane grafted iron oxide yellow and 100mL of ultrapure water are put into a flask, heated to 75-81 ℃, stirred at 800-1000 rpm, and stirred for at least 30 minutes to uniformly mix the priming materials. 0.5g of azobisisobutyronitrile was added to the reaction flask, and the temperature was stabilized. 50g of methyl methacrylate was added dropwise to the reaction system using a constant pressure dropping funnel. The dropping time is controlled to be 1 hour, and the temperature is kept for 1 hour after the dropping is finished. After the reaction time is over, the temperature is reduced to 45 ℃, and the coated iron oxide yellow with the particle size of 10.78 mu m is obtained by filtering with filter cloth.
44g of ABS resin, 6g of styrene-maleic anhydride copolymer and 7.3g of methyl methacrylate-butadiene-styrene copolymer are mixed in a high-speed mixer for 3-5 minutes, wherein the rotating speed of the high-speed mixer is 600-800 revolutions per minute. And then adding 7.5g of antioxidant 1010, 0.4g of benzotriazole light stabilizer, 4g of pentaerythritol stearate and 3g of coated iron oxide yellow into a high-speed mixer, mixing for 3-5 minutes, wherein the rotating speed of the high-speed mixer is 200-500 rpm, adding the mixed particles into a double-screw extruder, and carrying out melt extrusion, granulation, drying, cooling and packaging.
Comparative example 1:
42g of ABS resin, 13g of styrene-maleic anhydride copolymer and 6g of methyl methacrylate-butadiene-styrene copolymer are mixed in a high-speed mixer for 3-5 minutes, wherein the rotating speed of the high-speed mixer is 600-800 revolutions per minute. Then adding 4.2g of antioxidant 1010, 0.3g of light stabilizer UV770, 1g of ethylene bis stearamide and coated iron oxide yellow into a high-speed mixer, and mixing for 3-5 minutes, wherein the rotating speed of the high-speed mixer is 200-500 revolutions per minute; and adding the mixed particles into a double-screw extruder for melt extrusion, granulation, drying, cooling and packaging.
Comparative example 2
60g of ABS resin, 11g of styrene- (N-phenylmaleimide) -maleic anhydride and 7g of methyl methacrylate-butadiene-styrene copolymer are mixed in a high-speed mixer for 3 to 5 minutes, wherein the rotating speed of the high-speed mixer is 600 to 800 revolutions per minute. Then adding 8g of antioxidant 626, 0.4g of light stabilizer UV783, 0.4g of ethylene bis stearamide and 2.8g of coated iron oxide yellow into a high-speed mixer, and mixing for 3-5 minutes, wherein the rotating speed of the high-speed mixer is 200-500 revolutions per minute; and adding the mixed particles into a double-screw extruder for melt extrusion, granulation, drying, cooling and packaging.
Attached table 1, performance test data for each example:
Figure 101284DEST_PATH_IMAGE002
from the test results in the table above, it can be seen that the oil absorption of the masterbatch with the coated iron oxide yellow is greater than that of the masterbatch without the coated iron oxide yellow, indicating that the iron oxide yellow colorant is more dispersed in the ABS resin. After the storage for 1h at the temperature of 200 ℃, the color difference change of the color master batch of the coated iron oxide yellow is small, which shows that the heat resistance of the colorant is improved. In addition, after 720h of xenon lamp exposure photo-aging test, the color change index of the coated iron oxide yellow color master batch is smaller, which indicates that the color retention rate is higher and the color fading is not obvious.
The foregoing is only a preferred embodiment of the invention. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.

Claims (14)

1. The preparation method of the coated iron oxide yellow color master batch is characterized by comprising the following components in percentage by weight:
30-65 parts of ABS resin
5-15 parts of heat-resistant agent
6 to 12 portions of toughening agent
2 to 8 portions of antioxidant
0.1 to 0.6 portion of light stabilizer
0.2 to 5 portions of lubricant
0.4 to 10 portions of coated colorant.
2. The preparation of the coated iron oxide yellow color masterbatch according to claim 1, wherein: the heat-resistant agent is one or two of styrene-maleic anhydride copolymer and styrene- (N-phenylmaleimide) -maleic anhydride copolymer.
3. The preparation of the coated iron oxide yellow color masterbatch according to claim 1, wherein: the toughening agent is one or more of methyl methacrylate-butadiene-styrene copolymer, styrene-butadiene-styrene copolymer and ethylene-methyl acrylate-glycidyl methacrylate copolymer.
4. The preparation of the coated iron oxide yellow color masterbatch according to claim 1, wherein: the antioxidant is one or more of hindered phenols, phosphites and thioesters.
5. The preparation of the coated iron oxide yellow color masterbatch according to claim 1, wherein: one or more of hindered amine and benzotriazole of the light stabilizer.
6. The preparation of the coated iron oxide yellow color masterbatch according to claim 1, wherein: the lubricant is one or more of stearic acid, ethylene bis stearamide and pentaerythritol stearate.
7. The preparation of the coated iron oxide yellow color masterbatch according to claim 1, wherein: the coated coloring agent is iron oxide yellow coated by acrylic emulsion.
8. The acrylic emulsion-coated iron oxide yellow according to claim 7, wherein: the iron oxide yellow is subjected to grafting reaction with one or more of vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (6-methoxyethoxy) silane and gamma-methacryloxypropyltrimethoxysilane.
9. The acrylic emulsion-coated iron oxide yellow according to claim 8, wherein the acrylic emulsion is obtained by copolymerizing an acrylic ester compound, an initiator, ultrapure water and an emulsifier.
10. The acrylic emulsion according to claim 9, wherein the mass ratio of the acrylate compound to the initiator to the ultrapure water to the emulsifier is 80-100: 1-15: 100-1000 parts of: 10 to 50.
11. The acrylic emulsion according to claim 9, wherein the acrylic ester compound is one or more of methyl methacrylate, ethyl methacrylate, lauryl methacrylate, n-butyl methacrylate and t-butylaminoethyl methacrylate.
12. The acrylic emulsion according to claim 9, characterized in that: the initiator is at least one of azobisisobutyronitrile, azobisisoheptonitrile, benzoyl peroxide and dilauroyl peroxide.
13. The acrylic emulsion according to claim 9, characterized in that: the emulsifier is one or more of sodium dodecyl sulfate, span 60, span 80, Tween 80 and Tween 65.
14. The preparation method of the coated iron oxide yellow color master batch according to claims 1 to 13, wherein the preparation method comprises the following steps:
①, preparing ethanol and water solution with the volume of 5-20: 1, adding acetic acid to adjust the pH value to 4-5, adding a silane grafting agent under stirring, controlling the silane concentration to be 2-7%, and standing for 10-30 minutes to fully hydrolyze the silane;
② adding a certain amount of iron oxide yellow into the silane solution obtained in step ① under stirring, and reacting at 40 ℃ for 1 hour;
filtering and washing with deionized water, and drying at 85 deg.C;
③ putting the emulsifier, the ferric oxide yellow grafted with silane and ultrapure water into a flask, heating to 65-75 ℃, starting stirring, controlling the rotating speed at 800-900 r/min, and stirring for at least 30 minutes to uniformly mix the priming materials;
adding an initiator into a reaction bottle, and after the temperature is stable;
dripping the acrylate compound into the reaction system by using a constant-pressure dropping funnel;
controlling the dripping time to be 1 hour, and preserving the heat for 1 hour after the dripping is finished;
after the reaction time is over, cooling to 45 ℃, and filtering to obtain coated iron oxide yellow;
④ mixing ABS resin, heat-resistant agent and toughening agent in a high-speed mixer for 3-5 minutes, adding antioxidant, light stabilizer, lubricant and coated iron oxide yellow into the high-speed mixer for 3-5 minutes, adding the mixed particles into a double-screw extruder for melt extrusion, granulation, drying, cooling and packaging, wherein the rotation speed of the high-speed mixer is 200-600 r/min, and the rotation speed of the high-speed mixer is 700-1000 r/min.
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CN102883803A (en) * 2010-04-28 2013-01-16 宝洁公司 Delivery particles
CN105566834A (en) * 2014-11-10 2016-05-11 合肥杰事杰新材料股份有限公司 ABS composite material for low-odor low-volatilization scraping resistant automobile trim and preparation method
CN109722062A (en) * 2018-12-21 2019-05-07 英德科迪颜料技术有限公司 A kind of preparation method of core-shell structure transparent ferric oxide coated pigment

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JPH1036613A (en) * 1996-05-22 1998-02-10 Denki Kagaku Kogyo Kk Heat-resistant masterbatch resin, heat-resistant resin molding and its production
US20040214927A1 (en) * 2003-01-24 2004-10-28 Nitzsche Norman E. Compatible multi-functional color concentrate compositions
CN102883803A (en) * 2010-04-28 2013-01-16 宝洁公司 Delivery particles
CN105566834A (en) * 2014-11-10 2016-05-11 合肥杰事杰新材料股份有限公司 ABS composite material for low-odor low-volatilization scraping resistant automobile trim and preparation method
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114479515A (en) * 2022-01-16 2022-05-13 湖州师范学院 Method for optimizing heat resistance of coated iron oxide yellow pigment
CN114479515B (en) * 2022-01-16 2023-09-08 湖州师范学院 Method for optimizing heat resistance of wrapped iron oxide yellow pigment

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