CN114479386A - Super-black plastic master batch dispersed with nano carbon black, preparation method and application thereof - Google Patents
Super-black plastic master batch dispersed with nano carbon black, preparation method and application thereof Download PDFInfo
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- CN114479386A CN114479386A CN202210246461.1A CN202210246461A CN114479386A CN 114479386 A CN114479386 A CN 114479386A CN 202210246461 A CN202210246461 A CN 202210246461A CN 114479386 A CN114479386 A CN 114479386A
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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
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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
- 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
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- 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
- C08K2201/011—Nanostructured additives
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- 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
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- Polymers & Plastics (AREA)
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- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention relates to the field of functional textile chemical fibers, in particular to the technical field of B29, and more particularly relates to a super-black plastic master batch dispersed with nano carbon black, and a preparation method and application thereof. The super-black plastic master batch dispersed with the nano carbon black comprises, by weight, 100 parts of polyester powder and 50-100 parts of carbon black nano color paste. The super-black plastic master batch is added in the preparation process in the form of carbon black nano color paste, and the content of the dispersing agent in the carbon black nano color paste is low, so that the problem of carbon black agglomeration is solved, and the coloring effect is good.
Description
Technical Field
The invention relates to the field of functional textile chemical fibers, in particular to the technical field of B29, and more particularly relates to a super-black plastic master batch dispersed with nano carbon black, and a preparation method and application thereof.
Background
Ultra-black fibers refer to fibers having ultra-high absorption and very low reflectance in the visible range. The ultra-black fiber has an extremely strong hiding power because of its ultra-high visible light absorption rate. The garment made of the ultra-black fibers can still keep good black when being stretched, and the problem that other colors are exposed to the fabric made of common black fibers due to external force can be solved, so that the ultra-black fibers are huge in market demand and wide in prospect.
The preparation process of the ultra-black fiber mainly comprises a printing and dyeing processing method and a stock solution coloring method. At present, most of super-black fibers on the market are mainly prepared by a printing and dyeing processing mode, although the color and the blackness of the fiber products obtained by the processing mode are good, the color fastness is not good, in addition, the printing and dyeing processing process seriously pollutes the environment, and the health of human bodies can also be influenced. The stock solution coloring method not only can not generate industrial wastewater, but also has low energy consumption of system processing, and more importantly, can solve the problem of color fastness. However, the blackness of such dye-free polyester fibers has not achieved the effect of printing and dyeing processing, and is mainly due to problems of particle size and dispersibility of carbon black in the fiber mother particles. Dope dyeing methods are generally classified into a melt direct spinning method and a chip spinning method. For example, Chinese patent CN111286804A discloses a method for preparing melt direct spinning super-black polyester fiber, which can obviously improve the blackness of the prepared fiber by adding black color paste in the melt direct spinning process. However, the chip spinning method is generally used for producing the dyeing-free polyester fiber, because the chip spinning is more in line with the requirements of the existing high-speed spinning technology, and has the characteristics of convenience in variety replacement, rapid adjustment of the filler content in the fiber and the like. Therefore, the spinning mill provides the requirements of higher blackness, better spinnability and longer service cycle of the components for the black master batch.
Generally, the smaller the particle size of the carbon black in the fiber masterbatch, the better the dispersibility, and the higher the blackness of the produced fiber. For example, Chinese patents CN110885457A and CN110903611A adopt carbon black with the primary particle size of 19-20nm to be directly added into plastic powder to prepare master batches, and the blackness of fibers produced by the master batches is obviously improved through verification of downstream manufacturers. However, the smaller the particle diameter of carbon black, the larger the surface adsorption energy, and the more likely it is to cause aggregation, resulting in poor dispersibility of carbon black in the mother particles. The traditional method for directly dispersing carbon black powder into plastic powder cannot solve the problems of agglomeration of nano carbon black and poor dispersibility in master batches, and not only influences spinnability and the service cycle of components, but also influences fiber blackness. The carbon black color paste prepared by the traditional method has high dispersant content, so that the carbon black color paste can not be dried after being mixed with plastic powder, a screw rod slips during blanking, and the production requirement can not be met.
Therefore, a novel preparation technology of the ultra-black master batch is needed to solve the problems of nano carbon black agglomeration and dispersibility in the master batch.
Disclosure of Invention
Aiming at some problems in the prior art, the invention provides a super-black plastic master batch dispersed with nano carbon black, and the preparation raw materials comprise 100 parts of polyester powder and 50-100 parts of carbon black nano color paste by weight.
In one embodiment, the raw material for preparing the ultra-black plastic masterbatch dispersed with the nano carbon black further comprises 0-10 parts by weight of an auxiliary agent.
In one embodiment, the kind of the polyester powder is not particularly limited, and polybutylene terephthalate, polyethylene terephthalate, and the like can be exemplified.
Preferably, the melt index of the polyester powder at 265 ℃/2.16kg is 50-80g/10min, and more preferably 60-70g/10 min.
Preferably, the melting point of the polyester powder is 250-270 ℃, such as 250 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃ and the like.
The polyester powder with the melting point of 250-270 ℃ has a certain promotion effect on the dispersibility of the carbon black.
In one embodiment, the carbon black nanopigment has a primary particle size of 10-18nm, such as 10nm, 11nm, 12nm, 13nm, 14nm, 15nm, 16nm, 17nm, 18 nm.
The carbon black nanopigment preferably has a carbon black concentration of 10 to 30 wt%, and examples thereof include 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, 15 wt%, 20 wt%, 25 wt%, and 30 wt%.
The components except for carbon black in the carbon black nano color paste in the present application are not particularly limited, and may be a wetting agent, a dispersing agent, a solvent, etc., preferably, the concentration of the dispersing agent is 1 to 3 wt%, and the specific components can be selected by those skilled in the art according to actual needs.
In one embodiment, the carbon black nanopigment paste has a viscosity of 7000-8000cps at 25 ℃.
The original particle size of the carbon black is controlled to be 10-18nm, under the condition that the concentration of the dispersing agent is low, the excessive increase of carbon black aggregates can be avoided, the component types except the carbon black in the carbon black nano color paste and the preparation method of the carbon black nano color paste in the application do not influence the dispersibility and the coloring effect of the carbon black in the application, the unnecessary cost is saved, meanwhile, the raw materials are convenient and easy to obtain, the production efficiency is improved, the carbon black nano color paste is mixed with the polyester powder for granulation, the obtained ultra-black master batch is low in DF value, the carbon black is dispersed more uniformly, and the ultra-black fiber master batch with a low L value can be realized. The primary particle size of the carbon black is too large or too small, which can affect the dispersion effect of the carbon black and cause poor stability of the carbon black nano color paste. In addition, when the primary particle size of the carbon black is 10-18nm, even if the concentration of the carbon black in the carbon black nano color paste is kept below 15 wt%, a good coloring effect is obtained by using the plastic master batch.
As the auxiliary agent in this application, coupling agents, viscosity modifiers, antioxidants, foaming agents, surfactants, plasticizers, crosslinking agents, flame retardants, smoke suppressants and the like can be exemplified, and specific selection of the auxiliary agent can be made by those skilled in the art in a routine manner.
The second aspect of the invention provides a preparation method of a super-black plastic master batch dispersed with nano carbon black, which comprises the following steps:
(1) mixing the raw materials for preparing the ultra-black plastic master batch and drying;
(2) and (2) putting the material obtained in the step (1) into a double-screw extruder, and extruding and granulating at the temperature of 250-270 ℃.
In one embodiment, the preparation method of the nano carbon black dispersed ultra-black plastic master batch comprises the following steps:
(1) putting the raw materials for preparing the ultra-black plastic master batch into a high-speed mixer, heating and stirring until mixed powder is dried;
(2) putting the material obtained in the step (1) into a double-screw extruder for extrusion granulation: the uniformly mixed materials are fully plasticized in a double screw, and then are sheared and uniformly dispersed by a dispersing element in the double screw, and are extruded by a round hole die, cooled by a water tank, pulled by a brace and sent to a granulator to be cut into cylindrical particles with the length of 3mm +/-1 mm and the diameter of 2.5mm +/-1.5 mm; the double-screw extruder is provided with a vacuumizing device, and the length-diameter ratio of the double-screw extruder is not less than 40: 1; the process temperature during extrusion is 250-270 ℃.
The third aspect of the invention provides an application of the super-black plastic master batch dispersed with the nano carbon black in super-black fibers.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention improves the dispersibility of the carbon black in the master batch by using a wet feeding method, and converts the carbon black with the same concentration into the carbon black, and the L value in the fiber Lab value prepared by the ultra-black plastic master batch is lower than the L value of the fiber prepared by directly adding carbon black powder;
(2) the filter pressing value of the ultra-black master batch with 20 wt% of carbon black concentration prepared by the invention is not higher than 7Mpa, the L value can be not higher than 18 by adding 5 wt% into the fiber, and the L value is not higher than 15 after 10 wt% is added;
(3) the invention solves the problem that the carbon black with primary particle size less than 19nm is agglomerated into micron-sized carbon black due to overlarge surface adsorption energy during storage, thereby influencing the spinnability of master batches, and further prolonging the service cycle of a spinning assembly;
(4) the carbon black nano color paste contains 10-30 wt% of carbon black, but the content of the dispersing agent is only 1-3 wt%, so that the problem that a screw rod slips in the granulation process due to the fact that the traditional carbon black color paste is too high in dispersing agent content and cannot be completely dried after being mixed with plastic powder is solved;
(5) the carbon black nanometer color paste has high carbon black content, so that the organic solvent in other raw materials is less, the direct heating, mixing and drying time of a high-speed mixer is short, the time and the power consumption are saved, and in addition, the practical experience shows that compared with master batches prepared from slurry carbon black, the paste carbon black nanometer color paste in the application has a much lower filter pressing value than that of the carbon black nanometer color paste with the viscosity of 7000-8000cps at 25 ℃;
(6) the method controls the carbon black content and the primary particle size in the carbon black nano color paste, can solve the problem that the de-agglomeration of the carbon black cannot be realized in the common carbon black nano color paste, can also avoid the phenomenon of 'thickening' of the carbon black after being stored for a period of time, and can more effectively and stably store the carbon black nano color paste for use at any time;
(7) the carbon black nano color paste and the polyester powder or the auxiliary agent are directly mixed and dried to enter the granulator, the process is simple, the requirements of the existing high-speed spinning technology are met, and the carbon black nano color paste and the polyester powder have the characteristics of convenience in variety replacement, rapid adjustment of the filler content in the fiber and the like.
Drawings
FIG. 1 is a graph showing L values of black polyester fibers obtained by using master batches of examples 1 to 3 and comparative examples 1 to 3 of the present application at different concentrations.
Detailed Description
The present invention is illustrated by the following specific embodiments, but is not limited to the specific examples given below.
Example 1
The super-black plastic master batch dispersed with the nano carbon black comprises the following raw materials in parts by weight:
100 parts of PET powder, 100 parts of carbon black nano color paste and 1 part of antioxidant.
The PET powder is purchased from Jiangsu three-room lane, and the brand is CZ 5011; the primary particle size of carbon black in the carbon black nano color paste is 15nm, and the concentration is 30 wt%.
The preparation method of the super-black plastic master batch dispersed with the nano carbon black comprises the following steps:
(1) putting the raw materials into a high-speed mixer, heating and stirring until the mixed powder is dried, and removing the solvent of the nano color paste;
(2) putting into a double-screw extruder for extrusion granulation: fully plasticizing the uniformly mixed material in a double screw, shearing and uniformly dispersing the uniformly mixed material by a dispersing element in the double screw, extruding the uniformly mixed material through a round hole die, cooling the uniformly mixed material by a water tank, pulling a brace to a granulator, and cutting the uniformly mixed material into cylindrical particles with the length of 3mm +/-1 mm and the diameter of 2.5mm +/-1.5 mm; the double-screw extruder is provided with a vacuumizing device, and the length-diameter ratio of the double-screw extruder is not less than 40: 1; the process temperature during extrusion was 260 ℃.
Comparative example 1
The plastic master batch comprises the following raw materials in parts by weight:
100 parts of PET powder, 30 parts of nano carbon black powder and 1 part of antioxidant.
The PET powder is purchased from Jiangsu three-room lane, and the brand is CZ 5011; the type of the nano carbon black powder is consistent with that of carbon black in carbon black nano powder used in the embodiment.
The preparation method of the plastic master batch is the same as that in the embodiment 1, except that the step (1) is as follows: the raw materials are put into a high-speed mixer and fully stirred and uniformly mixed.
The master batches prepared in the above examples and comparative example 1 were mixed with white pellets (white pure PET master batches) according to a ratio of 2: 14, mixing, and testing the spinning filterability by adopting a 1400-mesh filter screen, wherein the spinning filter pressure value of the embodiment is 2.94MPa, and the spinning filter pressure value of the comparative example 1 is tested to be over-standard (more than or equal to 10MPa) in 11min, which can show that the dispersibility of the carbon black in the ultra-black master batch in the embodiment is better.
Example 2
The specific implementation mode of the plastic master batch is the same as that in example 1, except that the primary particle size of carbon black in the carbon black nano color paste is 10 nm.
The preparation method of the plastic masterbatch is the same as that of example 1.
Example 3
The specific implementation mode of the plastic master batch is the same as that in example 1, except that the primary particle size of carbon black in the carbon black nano color paste is 18 nm.
The preparation method of the plastic masterbatch is the same as that of example 1.
Comparative example 2
The specific implementation mode of the plastic master batch is the same as that in example 1, except that the primary particle size of carbon black in the carbon black nano color paste is 20 nm.
The preparation method of the plastic masterbatch is the same as that of example 1.
Comparative example 3
The specific implementation mode of the plastic master batch is the same as that in example 1, except that the primary particle size of carbon black in the carbon black nano color paste is 30 nm.
The preparation method of the plastic masterbatch is the same as that of example 1.
The master batches prepared in examples 2-3 and comparative examples 2-3 were mixed with white granules (white pure PET master batches) according to the following ratio of 2: 14, mix and test the spin filterability using a 1400 mesh filter screen.
The master batches prepared in the above examples 1 to 3 and comparative examples 1 to 3 were mixed with white pellets (white pure PET master batches) to produce black polyester fibers of 200D/96F standard in an amount of 2%, 4%, 6%, 8% and 10% by weight, respectively, and the L values of the produced fibers were measured using a color difference meter, with the results shown in table 1 and fig. 1.
TABLE 1
Claims (10)
1. The super-black plastic master batch dispersed with the nano carbon black is characterized in that the raw materials for preparing the super-black plastic master batch comprise, by weight, 100 parts of polyester powder and 50-100 parts of carbon black nano color paste.
2. The ultra-black plastic masterbatch dispersed with nano-carbon black according to claim 1, wherein the carbon black in the carbon black nanopigment has a primary particle size of 10 to 18 nm.
3. The ultra-black plastic masterbatch dispersed with nano-carbon black according to claim 2, wherein the concentration of carbon black in the carbon black nanopaste is 10 to 30 wt%.
4. The ultra-black plastic masterbatch dispersed with nano-carbon black of claim 3, wherein the carbon black nano-color paste further comprises 1-3 wt% of a dispersant.
5. The ultra-black plastic masterbatch dispersed with carbon black according to any one of claims 1 to 4, wherein the polyester powder has a melt index of 50 to 80g/10min at 265 ℃/2.16 kg.
6. The ultra-black plastic masterbatch dispersed with nano-carbon black of claim 5, wherein the melting point of the polyester powder is 250-270 ℃.
7. The nano-carbon black-dispersed ultra-black plastic masterbatch according to claim 5, wherein the raw material for preparing the nano-carbon black-dispersed ultra-black plastic masterbatch further comprises 0 to 10 parts by weight of an auxiliary agent, and the part by weight of the auxiliary agent does not comprise 0.
8. The nano carbon black-dispersed ultra-black plastic masterbatch according to claim 7, wherein the auxiliary agent is one or more selected from a coupling agent, a viscosity modifier, an antioxidant, a foaming agent, a surfactant, a plasticizer, a crosslinking agent, a flame retardant and a smoke suppressant.
9. The preparation method of the nano carbon black dispersed ultra-black plastic master batch according to any one of claims 1 to 8, which comprises the following steps:
(1) mixing the raw materials for preparing the ultra-black plastic master batch and drying;
(2) and (2) putting the material obtained in the step (1) into a double-screw extruder, and extruding and granulating at the temperature of 250-270 ℃.
10. Use of the ultra black plastic masterbatch dispersed with carbon black according to any one of claims 1 to 8 in ultra black fiber.
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| CN106867183A (en) * | 2017-03-10 | 2017-06-20 | 广州润锋化工有限公司 | A kind of direct use in injection molding bloom black agglomerate of resin and preparation method thereof |
| CN107325647A (en) * | 2017-07-21 | 2017-11-07 | 温州大学 | A kind of method that color is prepared by raw material of aqueous color paste |
| CN110885457A (en) * | 2019-12-04 | 2020-03-17 | 苏州宝丽迪材料科技股份有限公司 | Preparation method of super-black large-melting-index high-dispersibility black master batch |
| CN110903611A (en) * | 2019-12-04 | 2020-03-24 | 苏州宝丽迪材料科技股份有限公司 | Special ultra-black large-melt-index high-dispersibility black master batch for direct-spinning fine denier yarns |
| CN111286804A (en) * | 2019-11-29 | 2020-06-16 | 浙江华欣新材料股份有限公司 | Preparation method of dope-dyed melt direct-spinning super-black polyester fiber |
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- 2022-03-14 CN CN202210246461.1A patent/CN114479386A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867183A (en) * | 2017-03-10 | 2017-06-20 | 广州润锋化工有限公司 | A kind of direct use in injection molding bloom black agglomerate of resin and preparation method thereof |
| CN107325647A (en) * | 2017-07-21 | 2017-11-07 | 温州大学 | A kind of method that color is prepared by raw material of aqueous color paste |
| CN111286804A (en) * | 2019-11-29 | 2020-06-16 | 浙江华欣新材料股份有限公司 | Preparation method of dope-dyed melt direct-spinning super-black polyester fiber |
| CN110885457A (en) * | 2019-12-04 | 2020-03-17 | 苏州宝丽迪材料科技股份有限公司 | Preparation method of super-black large-melting-index high-dispersibility black master batch |
| CN110903611A (en) * | 2019-12-04 | 2020-03-24 | 苏州宝丽迪材料科技股份有限公司 | Special ultra-black large-melt-index high-dispersibility black master batch for direct-spinning fine denier yarns |
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