CN114479516A - Aqueous easily-dispersible azo organic pigment - Google Patents
Aqueous easily-dispersible azo organic pigment Download PDFInfo
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- CN114479516A CN114479516A CN202210132658.2A CN202210132658A CN114479516A CN 114479516 A CN114479516 A CN 114479516A CN 202210132658 A CN202210132658 A CN 202210132658A CN 114479516 A CN114479516 A CN 114479516A
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- 239000012860 organic pigment Substances 0.000 title claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 239000002245 particle Substances 0.000 claims abstract description 57
- 239000000203 mixture Substances 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000376 reactant Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001023 inorganic pigment Substances 0.000 claims abstract description 14
- 239000002952 polymeric resin Substances 0.000 claims abstract description 13
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 11
- 239000000049 pigment Substances 0.000 claims abstract description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 7
- 238000001125 extrusion Methods 0.000 claims abstract description 7
- 238000005491 wire drawing Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 36
- 238000004821 distillation Methods 0.000 claims description 22
- 238000000605 extraction Methods 0.000 claims description 10
- -1 polyethylene Polymers 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000004743 Polypropylene Substances 0.000 claims description 8
- 229920001155 polypropylene Polymers 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- XQRLCLUYWUNEEH-UHFFFAOYSA-N diphosphonic acid Chemical compound OP(=O)OP(O)=O XQRLCLUYWUNEEH-UHFFFAOYSA-N 0.000 claims description 4
- SCIGVHCNNXTQDB-UHFFFAOYSA-N decyl dihydrogen phosphate Chemical compound CCCCCCCCCCOP(O)(O)=O SCIGVHCNNXTQDB-UHFFFAOYSA-N 0.000 claims description 3
- KRIXEEBVZRZHOS-UHFFFAOYSA-N tetradecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCOP(O)(O)=O KRIXEEBVZRZHOS-UHFFFAOYSA-N 0.000 claims description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 claims description 2
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 claims description 2
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 claims description 2
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 13
- 229920005989 resin Polymers 0.000 abstract description 12
- 239000011347 resin Substances 0.000 abstract description 12
- 238000009775 high-speed stirring Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- 239000012736 aqueous medium Substances 0.000 abstract description 3
- 238000003810 ethyl acetate extraction Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 30
- 239000000243 solution Substances 0.000 description 14
- 239000000975 dye Substances 0.000 description 11
- 238000001746 injection moulding Methods 0.000 description 9
- 239000001054 red pigment Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229920013716 polyethylene resin Polymers 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical class [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/22—Compounds of iron
- C09C1/24—Oxides of iron
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a water-based easily-dispersible azo organic pigment, and relates to the technical field of organic pigments. An aqueous easily-dispersible azo organic pigment is prepared by the following steps: s1: stirring and mixing a sodium hydroxide solution and organic phosphoric acid to obtain a reaction solution A; s2: carrying out ethyl acetate extraction on the reaction liquid A to obtain a reactant B; s3: putting the reactant B, the polymer resin particles and the inorganic pigment powder into a solid stirrer in sequence for stirring to obtain a mixture C; s4: and putting the mixture C into an extruder for melt extrusion and wire drawing to obtain the finished pigment master batch. According to the invention, the high-molecular resin particles and the inorganic pigment are mixed by a high-speed stirring process, so that the inorganic pigment and the high-molecular resin particles in the prepared organic pigment master batch are uniformly dispersed, and meanwhile, the prepared master batch has larger particles and extremely low surface energy, so that the particles are not easy to agglomerate in an aqueous medium and have better dispersion stability.
Description
Technical Field
The invention relates to the technical field of organic pigments, in particular to a water-based easily-dispersible azo organic pigment.
Background
Pigments can be classified into inorganic dyes and organic pigments. And the inorganic dye refers to oxide of nonferrous metal, or some metal insoluble metal salt, mainly including various metal oxides, chromates, carbonates, sulfates, sulfides, etc. Inorganic dyes have strong weather resistance and light resistance, and the inorganic dyes can darken and deepen colors without fading due to the action of sunlight and the atmosphere. Also other pigments, through the action of sunlight and the atmosphere, cause a change in the chemical composition of the pigment and discoloration due to structural damage. Inorganic dyes are widely used in the fields of coatings, inks, plastics and rubbers because of their good color fastness.
The aqueous ink is a solid-liquid dispersion system in which a pigment is in a solid phase and water and a resin or the like are in a liquid phase. The traditional organic pigment has low polarity and poor hydrophilicity, and in addition, the pigment has high surface energy and capillary adhesion, is easy to agglomerate in an aqueous medium and has poor dispersion stability. During the printing process, the color performance of the printed matter, including tinting strength, glossiness and smoothness, is greatly influenced. The invention provides a water-based easily-dispersible azo organic pigment.
Disclosure of Invention
The present invention aims to provide an aqueous easily dispersible azo organic pigment to solve the problems set forth in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a water-based easily-dispersible azo organic pigment comprises the following steps:
s1: adding a sodium hydroxide solution into a closed container with stirring and temperature control functions, controlling the temperature of the sodium hydroxide solution to be 50-70 ℃ through a temperature control function, then adding organic phosphoric acid into the closed container, maintaining the temperature to be 50-70 ℃, stirring the mixture for 20-40 minutes, and obtaining a reaction solution A;
s2: carrying out ethyl acetate pair extraction on the reaction liquid A, extracting for three times to obtain an extraction liquid, placing the extraction liquid into a distillation container, and distilling to remove ethyl acetate to obtain a reactant B;
s3: putting the reactant B, the polymer resin particles and the inorganic pigment powder into a solid stirrer in sequence for stirring to obtain a mixture C;
s4: and putting the mixture C into an extruder for melt extrusion and wire drawing, and performing water cooling, particle cutting and drying on the strand silk to obtain the finished pigment master batch.
Further, the concentration of the sodium hydroxide solution in the step S1 is 1.5-2%, and the organic phosphoric acid is any one or more of 1, 12-dodecane diphosphonic acid, 1-decyl phosphoric acid and 1-tetradecyl phosphoric acid.
Further, the distillation mode in the step S2 adopts reduced pressure distillation, the distillation temperature is 70-75 ℃, and the distillation pressure is 10-15 KPa.
Furthermore, the stirring speed of the high-speed stirrer in the step S3 is set to 2000-3000r/min, and the stirring time is 40-60S.
Further, the polymer resin particles in the step S3 are any one or a mixture of more of polyethylene particles, polypropylene particles, poly-1-butene particles, poly-1-pentene particles, poly-1-hexene particles, poly-1-octene particles, and poly-4-methyl-1-pentene particles.
Further, the inorganic dye in the step S3 is an iron-or aluminum-containing inorganic dye, and the particle diameter of the inorganic dye is 0.1 to 0.5 μm.
Furthermore, the molar ratio of the sodium hydroxide in the sodium hydroxide solution in the step S1 to the organic phosphoric acid is 1-2: 1.
Furthermore, the mass ratio of the reactant B, the polymer resin particles and the inorganic dye powder in the step S3 is 2-7: 30-45: 100 respectively.
An aqueous easily dispersible azo organic pigment prepared according to the method.
Compared with the prior art, the invention has the beneficial effects that:
according to the water-based easily-dispersible azo organic pigment, the high-molecular resin particles and the inorganic pigment are mixed by a high-speed stirring process, so that the inorganic pigment and the high-molecular resin particles in the prepared organic pigment master batch are uniformly dispersed, and meanwhile, the prepared master batch particles are large and have extremely low surface energy, so that the inorganic pigment and the high-molecular resin particles are not easily agglomerated in a water-based medium and have good dispersion stability.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the embodiment provides a water-based easily dispersible azo organic pigment master batch, which is prepared by the following steps:
s1: adding 40L of sodium hydroxide solution into a closed dispersion kettle with the capacity of 60L and the functions of stirring and temperature control, controlling the temperature of the sodium hydroxide solution to be 60 ℃ through the function of temperature control, then adding 1725g of 1-decyl phosphoric acid into the closed dispersion kettle, maintaining the temperature to be 60 ℃, stirring the mixture for 30 minutes, and obtaining reaction liquid A;
s2: carrying out ethyl acetate pair extraction on the reaction liquid A, extracting for three times to obtain extract liquor, placing the extract liquor into a distillation container, distilling to remove ethyl acetate to obtain 1935g of a reactant B, wherein the distillation temperature is 75 ℃, and the distillation pressure is 12 KPa;
s3: putting 1935g of reactant B, 20kg of polyethylene resin particles and 50kg of iron oxide red powder (the average particle diameter of the iron oxide red powder is 0.3 micron) with the model Y101 into a high-speed stirrer in sequence for high-speed stirring, wherein the stirring speed of the high-speed stirrer is set to be 2500r/min, and the stirring time is 50s, so as to obtain a mixture C;
s4: and putting the mixture C into an extruder for melt extrusion and wire drawing, and performing water cooling, grain cutting and drying on the strand wires to obtain 69kg of finished iron oxide red pigment master batch.
Example two:
the embodiment provides a water-based easily dispersible azo organic pigment master batch, which is prepared by the following steps:
s1: adding 40L of sodium hydroxide solution into a closed dispersion kettle with the capacity of 60L and stirring and temperature control functions, controlling the temperature of the sodium hydroxide solution to be 60 ℃ through the temperature control function, subsequently adding 1315g of 1, 12-dodecane diphosphonic acid into the closed dispersion kettle, maintaining the temperature to be 60 ℃, stirring the mixture for 30 minutes, and obtaining reaction liquid A;
s2: carrying out ethyl acetate pair extraction on the reaction liquid A, extracting for three times to obtain extract liquor, placing the extract liquor into a distillation container, distilling to remove ethyl acetate to obtain 1632g of a reactant B, wherein the distillation temperature is 75 ℃, and the distillation pressure is 12 KPa;
s3: sequentially putting 1632g of reactant B, 20kg of polyethylene resin particles and 50kg of iron oxide red powder (the average particle diameter of the iron oxide red powder is 0.3 micron) with the model of Y101 into a high-speed stirrer for high-speed stirring, wherein the stirring speed of the high-speed stirrer is set to 2500r/min, and the stirring time is 50s, so as to obtain a mixture C;
s4: and putting the mixture C into an extruder for melt extrusion and wire drawing, and performing water cooling, grain cutting and drying on the strand wires to obtain 67kg of finished iron oxide red pigment master batch.
Example three:
the embodiment provides a water-based easily dispersible azo organic pigment master batch, which is prepared by the following steps:
s1: adding 45L of sodium hydroxide solution into a closed dispersion kettle with the capacity of 60L and stirring and temperature control functions, controlling the temperature of the sodium hydroxide solution to be 60 ℃ through the temperature control function, subsequently adding 1500g of 1, 12-dodecane diphosphonic acid into the closed dispersion kettle, maintaining the temperature to be 60 ℃, stirring the mixture for 30 minutes, and obtaining reaction liquid A;
s2: carrying out ethyl acetate pair extraction on the reaction liquid A, extracting for three times to obtain extract liquor, placing the extract liquor into a distillation container, distilling to remove ethyl acetate to obtain 1725g of a reactant B, wherein the distillation temperature is 75 ℃, and the distillation pressure is 12 KPa;
s3: 1725g of reactant B, 20kg of polyethylene resin particles and 50kg of iron oxide red powder Y101 (the average particle diameter of which is 0.3 μm) were put into a high-speed stirrer in this order and stirred at a high speed, wherein the stirring speed of the high-speed stirrer was set to 2500r/min and the stirring time was 50s, and a mixture C was obtained;
s4: and putting the mixture C into an extruder for melt extrusion and wire drawing, and performing water cooling, grain cutting and drying on the strand wires to obtain 68kg of finished iron oxide red pigment master batch.
Example four:
the embodiment provides a water-based easily dispersible azo organic pigment master batch, which is prepared by the following steps:
s1: adding 40L of sodium hydroxide solution into a closed dispersion kettle with the capacity of 60L and the functions of stirring and temperature control, controlling the temperature of the sodium hydroxide solution to be 60 ℃ through the function of temperature control, then adding 2085g of 1-tetradecyl phosphoric acid into the closed dispersion kettle, maintaining the temperature to be 60 ℃, stirring the mixture for 30 minutes, and obtaining reaction liquid A;
s2: carrying out ethyl acetate pair extraction on the reaction liquid A, extracting for three times to obtain extract liquor, placing the extract liquor into a distillation container, distilling to remove ethyl acetate to obtain 2201g of reactant B, wherein the distillation temperature is 75 ℃, and the distillation pressure is 12 KPa;
s3: 2201g of reactant B, 20kg of polyethylene resin particles and 50kg of iron oxide red powder (the average particle diameter of which is 0.3 micron) with the model Y101 are put into a high-speed stirrer in sequence for high-speed stirring, wherein the stirring speed of the high-speed stirrer is set to 2500r/min, and the stirring time is 50s, so that a mixture C is obtained;
s4: and putting the mixture C into an extruder for melt extrusion and wire drawing, and performing water cooling, grain cutting and drying on the strand wires to obtain 68.5kg of finished iron oxide red pigment master batch.
It is to be understood that, when polymer resin particles with relatively high viscosity are used in the actual production process, white oil can be added into the polymer resin particles, so that during granulation, the white oil can play a role in lubrication, reduce the shear heat during granulation, and further effectively prevent the pasty phenomenon caused by the fact that the polymer resin particles have too high viscosity and are difficult to granulate, and meanwhile, the white oil is a colorless and transparent hydrocarbon oily liquid without odor, and the mixture of the n-isoparaffin of C16-C31 as the main component has good compatibility with the polymer resin particles, and can play a certain role in dispersing the inorganic dye.
Comparative example one:
a commercially available red iron oxide powder of type Y101 (with an average particle diameter of 0.3 μm) was used for comparison.
Comparative experiment:
sequentially taking 20g, 20.5g, 19.8g and 19.5g of finished iron oxide red pigment master batches in the first embodiment to the fourth embodiment and 20g of iron oxide red powder with the model number of Y101 in the first comparative embodiment for later use, then taking 20kg of polypropylene resin particles for later use, drying at the temperature of 70 ℃ for 8 hours in an air-blast drying oven, after drying, 20kg of polypropylene resin particles are equally divided into five parts (4 kg each), then the prepared finished iron oxide red pigment master batches in the first to fourth embodiments and the iron oxide red powder with the model Y101 in the first comparative example are respectively and uniformly mixed with the five parts of polypropylene resin particles to obtain a polypropylene resin particle mixture, at the moment, the content of the iron oxide red powder in each part of polypropylene resin particle mixture is 20g, the mixture is sequentially marked as a first sample to a fifth sample, and further, an injection molding machine is adopted to sequentially perform injection molding on each part of polypropylene resin particle mixture to obtain a color plate.
It should be noted that the injection molding machine used in the comparative test is a small injection molding machine of T-80 type, which is manufactured by ningbo haitian plastic machine group ltd, and during injection molding, the temperatures from the injection molding head to the discharge hopper are set to 220 ℃, 200 ℃, 180 ℃ and 150 ℃ in sequence, the mold temperature is set to 56 ℃, the injection molding pressure is set to 80Mpa, the injection molding time is 10s, the cooling time is 10s, and the screw rotation speed is set to 70rpm, and the injection molding processes are sequentially performed on the first to fifth samples to obtain the injection molded color plates.
The invention mixes the polymer resin particles and the inorganic pigment through a high-speed stirring process, so that the inorganic pigment and the polymer resin particles in the prepared organic pigment master batch are uniformly dispersed, the prepared master batch particles are larger, the surface energy of the master batch particles is extremely low, the master batch particles are not easy to agglomerate in an aqueous medium, the dispersion stability is better, the inorganic dye can be further and fully dispersed in the master batch through the preparation and addition of the olefin organic sodium phosphate salt in the preparation process, and meanwhile, the preparation method of the organic sodium phosphate salt is simple, so the preparation cost is lower, and the market competitiveness is certain.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method of a water-based easily-dispersible azo organic pigment is characterized by comprising the following steps: the preparation method comprises the following steps:
s1: adding a sodium hydroxide solution into a closed container with stirring and temperature control functions, controlling the temperature of the sodium hydroxide solution to be 50-70 ℃ through a temperature control function, then adding organic phosphoric acid into the closed container, maintaining the temperature to be 50-70 ℃, stirring the mixture for 20-40 minutes, and obtaining a reaction solution A;
s2: carrying out ethyl acetate pair extraction on the reaction liquid A, extracting for three times to obtain an extraction liquid, placing the extraction liquid into a distillation container, and distilling to remove ethyl acetate to obtain a reactant B;
s3: putting the reactant B, the polymer resin particles and the inorganic pigment powder into a solid stirrer in sequence for stirring to obtain a mixture C;
s4: and putting the mixture C into an extruder for melt extrusion and wire drawing, and performing water cooling, particle cutting and drying on the strand silk to obtain the finished pigment master batch.
2. The method for preparing an aqueous dispersible azo organic pigment according to claim 1, wherein: the concentration of the sodium hydroxide solution in the step S1 is 1.5-2%, and the organic phosphoric acid is any one or a mixture of 1, 12-dodecane diphosphonic acid, 1-decyl phosphoric acid and 1-tetradecyl phosphoric acid.
3. The method for preparing an aqueous dispersible azo organic pigment according to claim 1, wherein: the distillation mode in the step S2 adopts reduced pressure distillation, the distillation temperature is 70-75 ℃, and the distillation pressure is 10-15 KPa.
4. The method for preparing an aqueous dispersible azo organic pigment according to claim 1, wherein: the stirring speed of the high-speed stirrer in the step S3 is set to be 2000-3000r/min, and the stirring time is 40-60S.
5. The method for preparing an aqueous dispersible azo organic pigment according to claim 1, wherein: the polymer resin particles in the step of S3 are any one or a mixture of more of polyethylene particles, polypropylene particles, poly-1-butene particles, poly-1-pentene particles, poly-1-hexene particles, poly-1-octene particles and poly-4-methyl-1-pentene particles.
6. The method for preparing an aqueous dispersible azo organic pigment according to claim 1, wherein: the inorganic pigment in the step S3 is an inorganic pigment containing an iron element or an aluminum element, and the particle diameter of the inorganic pigment is 0.1 to 0.5 μm.
7. The method for preparing an aqueous dispersible azo organic pigment according to claim 1, wherein: the molar ratio of the sodium hydroxide in the sodium hydroxide solution in the step S1 to the organic phosphoric acid is 1-2: 1.
8. The method for preparing an aqueous dispersible azo organic pigment according to claim 1, wherein: the mass ratio of the reactant B, the polymer resin particles and the inorganic pigment powder in the step S3 is 2-7: 30-45: 100 respectively.
9. An aqueous easily dispersible azo organic pigment characterized in that: prepared according to any one of claims 1 to 8.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1258636A (en) * | 1999-12-30 | 2000-07-05 | 清华大学 | Alternate extraction-counter extraction process of producing phosphate |
| US6646037B1 (en) * | 2002-07-31 | 2003-11-11 | Millennium Inorganic Chemicals, Inc. | Pigments treated with organosulfonic compounds |
| CN105121533A (en) * | 2013-03-14 | 2015-12-02 | 水晶无机化学瑞士有限公司 | Non-micronized pigment for plastics applications |
| CN109503922A (en) * | 2018-11-19 | 2019-03-22 | 深圳免喷材料科技有限公司 | A kind of preparation method of pigment functional agglomerate and products thereof and application |
| CN114410132A (en) * | 2021-12-27 | 2022-04-29 | 江西隆源化工股份有限公司 | Preparation method of easily-dispersible pigment |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1258636A (en) * | 1999-12-30 | 2000-07-05 | 清华大学 | Alternate extraction-counter extraction process of producing phosphate |
| US6646037B1 (en) * | 2002-07-31 | 2003-11-11 | Millennium Inorganic Chemicals, Inc. | Pigments treated with organosulfonic compounds |
| CN105121533A (en) * | 2013-03-14 | 2015-12-02 | 水晶无机化学瑞士有限公司 | Non-micronized pigment for plastics applications |
| CN109503922A (en) * | 2018-11-19 | 2019-03-22 | 深圳免喷材料科技有限公司 | A kind of preparation method of pigment functional agglomerate and products thereof and application |
| CN114410132A (en) * | 2021-12-27 | 2022-04-29 | 江西隆源化工股份有限公司 | Preparation method of easily-dispersible pigment |
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