CN114752211A - Polyamide color master batch for high-temperature-resistant carbon black coloring and preparation method thereof - Google Patents
Polyamide color master batch for high-temperature-resistant carbon black coloring and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyamide color master batch colored by high-temperature-resistant carbon black and a preparation method thereof, and relates to the field of polyamide color master batches, wherein the polyamide color master batch colored by the high-temperature-resistant carbon black is obtained by mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, adding polyamide resin, mixing in an internal mixer, extruding and granulating, and the problems that the effective dispersion of particles is difficult to realize, the dyeing uniformity is poor, and the compatibility between a coloring agent and polyamide is poor in the existing preparation process of the polyamide color master batch are solved; the dispersing agent can generate stronger adsorption effect and steric hindrance effect, so that the carbon black colorant is uniformly dispersed in the polyamide aggregate, the compatilizer plays a role of a bridge, the compatibility of the polyamide color master batch is improved, the purpose of improving the stability and coloring effect of the color master batch in the polyamide is achieved, and the added antioxidant also enables the polyamide to have better thermal stability.
Description
Technical Field
The invention relates to the field of polyamide color master batches, in particular to a high-temperature-resistant carbon black colored polyamide color master batch and a preparation method thereof.
Background
The polyamide material has very excellent mechanical property, can resist repeated impact shock, has the use temperature range of-40-100 ℃, is resistant to oil, organic solvents such as hydrocarbon, lipid and the like, is not resistant to acid, easy to oxidize, easy to color and nontoxic, and is widely applied to PA6, PA66 and PAI010 which are most applied in the industry at present, wherein PA6 and PA66 are widely applied due to price advantage and good performance and processability, and the modification research of polyamide fiber is still in the development and trial stage at present, but the functional modification of polyamide has wide development prospect at present when green and environment protection is advocated.
The color master batch is a special colorant for high polymer materials, generally comprises three main components of pigment, carrier resin and additive, and the color master batch and the carrier are spun in a blending mode before spinning, so that the pigment can be more uniformly mixed in filaments, the spinning process is simplified, the production cost is reduced, the pollution problem can be solved, and the health of workers in a workshop is ensured.
The modification of polyamide is firstly put into use by the world famous tire manufacturers, the tire cords of double endurance companies, Goodyear companies, Fissister companies and the like are all manufactured by adopting modified polyamide 66 dipped cord fabrics, some performances of common cords are improved, and then domestic industrial personnel are put into functional modification research of polyamide in many times, wherein the research, development and application of colored polyamide color master batches are increasingly concerned recently.
However, the prior polyamide color master batch preparation process is difficult to realize effective dispersion of particles, so that the dispersibility of a master batch pigment obtained by a screw extrusion mode is difficult to control, the dyeing uniformity is poor, and the compatibility between a colorant and polyamide is poor, thereby reducing the stability and the coloring effect of the color master batch in the polyamide.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a polyamide color master batch with high temperature resistance and carbon black coloring and a preparation method thereof:
(1) mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, adding polyamide resin, mixing in an internal mixer, and extruding and granulating through a double-screw extruder to obtain the high-temperature-resistant carbon black colored polyamide color master batch, so that the problems that effective dispersion of particles is difficult to realize, the dyeing uniformity is poor, and the compatibility between a colorant and the polyamide resin is poor in the existing preparation process of the polyamide color master batch are solved;
(2) placing polyoxypropylene diol in a three-neck flask, adding p-phenylene diisocyanate, adding 2, 2-dimethylolpropionic acid and 1, 4-butanediol, adding acetone, adding stannous octoate and dibutyltin dilaurate, adding polyethylene glycol, placing in an emulsification barrel, adding triethylamine for neutralization, adding deionized water, and performing high-speed shearing emulsification to obtain the dispersing agent, so that the problems that effective dispersion of particles is difficult to realize and the dyeing uniformity is poor in the existing polyamide color master batch preparation process are solved;
(3) the preparation method comprises the steps of weighing maleic anhydride and ethylene glycol, adding the maleic anhydride and the ethylene glycol into a four-neck reaction bottle, adding a catalyst to obtain an intermediate E, adding the intermediate E into the four-neck flask, adding 1, 4-butanediol and dibutyltin dilaurate, and then adding p-phenylene diisocyanate to obtain the compatilizer, so that the problem of poor compatibility between a coloring agent and polyamide in the existing polyamide color master batch preparation process is solved.
The purpose of the invention can be realized by the following technical scheme:
the polyamide color master batch resistant to high-temperature carbon black coloring comprises the following components in parts by weight:
60-80 parts of carbon black, 100-120 parts of polyamide resin, 8-10 parts of a dispersing agent, 2-5 parts of a silane coupling agent, 1-5 parts of a compatilizer and 1-5 parts of an antioxidant;
the polyamide color master batch for coloring the high-temperature-resistant carbon black is prepared by the following steps:
s1: mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, and performing ultrasonic dispersion;
s2: and adding polyamide resin, stirring uniformly, mixing in an internal mixer, and extruding and granulating by a double-screw extruder to obtain the high-temperature-resistant carbon black colored polyamide color master batch.
As a further scheme of the invention: the dispersing agent is prepared by the following steps:
s21: placing weighed polyoxypropylene glycol into a three-neck flask, adding a thermometer, a condenser tube and a stirring rod, then carrying out vacuum dehydration for 30-40min at the temperature of 100-120 ℃, cooling to 45-50 ℃, adding p-phenylene diisocyanate and introducing dry nitrogen for protection, heating to 90-100 ℃, reacting for 3-5h, and cooling to 40-50 ℃ to obtain an intermediate A;
the chemical reaction formula is as follows:
s22: adding 2, 2-dimethylolpropionic acid and 1, 4-butanediol into the intermediate A, adding acetone, heating to 80-90 ℃, reacting for 1-2h, and cooling to 45-50 ℃ to obtain an intermediate B;
the chemical reaction formula is as follows:
s23: adding stannous octoate and dibutyltin dilaurate into the intermediate B, heating to 70-80 ℃, reacting for 3.5h, cooling to 40-50 ℃, adding polyethylene glycol, reacting for 3-5h, and cooling to 30-40 ℃ to obtain an intermediate C;
the chemical reaction formula is as follows:
s24: and (3) placing the intermediate C in an emulsification barrel, adding triethylamine for neutralization at the rotating speed of 1000-1500r/min, adding deionized water, and performing high-speed shearing emulsification for 10-20min to obtain the dispersing agent.
As a further scheme of the invention: the amount ratio of polyoxypropylene to p-phenylene diisocyanate used in step S21 was 21.6 g: 26.68g, the dosage ratio of the intermediate A, the 2, 2-dimethylolpropionic acid, the 1, 4-butanediol and the acetone in the step S22 is 32.5 g: 2.60 g: 3.66 g: 4g of the total weight.
As a further scheme of the invention: in the step S23, the dosage ratio of the intermediate B, stannous octoate, dibutyltin dilaurate to polyethylene glycol was 20.26 g: 3.5 g: 1.5 g: 5.99g, wherein the dosage ratio of the intermediate C, triethylamine and deionized water in the step S24 is 24.9 g: 3.3 mL: 15 mL.
As a further scheme of the invention: the compatilizer is prepared by the following steps:
s51: weighing maleic anhydride and ethylene glycol, adding into a four-mouth reaction bottle with temperature control, stirring and reflux devices, and introducing N2Protecting, heating at 10-12 ℃/min, reacting for 0.5-1h when the temperature is raised to 80-90 ℃, gradually dissolving maleic anhydride, heating to 140-145 ℃ at 10-15 ℃/min, reacting for 4-6h, adding a catalyst, heating to 190-200 ℃ at 5-8 ℃/min, reacting for 4-6h, cooling to 135-140 ℃, and carrying out vacuum pumping reaction for 2.5-3h to obtain an intermediate E;
s52: adding the intermediate E into a four-neck flask, heating to 130-140 ℃, vacuumizing to 0.06-0.08MPa, dehydrating for 2.5-3h, cooling to 70-80 ℃, adding 1, 4-butanediol and dibutyltin dilaurate, stirring and mixing uniformly, then adding p-phenylene diisocyanate, stirring, vacuumizing and defoaming, introducing nitrogen for protection, and reacting for 3.5-5h to obtain the compatilizer.
As a further scheme of the invention: in the step S51, the dosage ratio of the maleic anhydride to the ethylene glycol is 10 g: 13.5g of p-toluenesulfonic acid as the catalyst, wherein the amount of the catalyst is 5% of the mass of the maleic anhydride, and the ratio of the amounts of the intermediate E, the 1, 4-butanediol and the p-phenylene diisocyanate in the step S52 is 15.9 g: 14.5 g: 20.6g, and the using ratio of the dibutyltin dilaurate is 3% of the mass of the intermediate E.
As a further scheme of the invention: in the step S1, the silane coupling agent is vinyl triethoxysilane, and the antioxidant is a hindered phenol antioxidant.
The preparation method of the polyamide color master batch colored by the high-temperature resistant carbon black comprises the following steps:
s1: mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, and performing ultrasonic dispersion;
s2: and adding polyamide resin, stirring uniformly, mixing in an internal mixer, and extruding and granulating by a double-screw extruder to obtain the high-temperature-resistant carbon black colored polyamide color master batch.
The invention has the beneficial effects that:
(1) according to the invention, the carbon black, the silane coupling agent, the dispersing agent, the compatilizer and the antioxidant are mixed, then the polyamide resin is added, the mixture is transferred into an internal mixer for mixing, and the mixture is extruded and granulated by a double-screw extruder to obtain the high-temperature-resistant carbon black colored polyamide color master batch;
(2) placing polyoxypropylene diol into a three-neck flask, adding p-phenylene diisocyanate, adding 2, 2-dimethylolpropionic acid and 1, 4-butanediol, adding acetone, adding stannous octoate and dibutyltin dilaurate, adding polyethylene glycol, placing into an emulsification barrel, adding triethylamine for neutralization, adding deionized water, and performing high-speed shearing emulsification to obtain the dispersing agent, wherein the conventional dispersing agent has a small molecular weight, has a single anchoring group combined with carbon black particles and a small quantity, cannot form firm adsorption, is easily influenced by factors such as temperature, impurity ions and the like, has a poor effect in practical use, has a long molecular chain and a large quantity of anchoring groups, can generate strong adsorption and steric hindrance effects, two polyethylene glycol chain segments at two ends of the molecular chain of the dispersing agent provide limited steric hindrance effect and form strong electrostatic repulsion force with ions carried by the chain segments, these two effects hinder aggregation between the carbon black particles, thereby uniformly dispersing the carbon black colorant in the polyamide aggregate;
(3) the preparation method comprises the steps of weighing maleic anhydride and ethylene glycol, adding the maleic anhydride and the ethylene glycol into a four-neck reaction bottle, adding a catalyst to obtain an intermediate E, adding the intermediate E into the four-neck flask, adding 1, 4-butanediol and dibutyltin dilaurate, and then adding p-phenylene diisocyanate to obtain the compatilizer, wherein the interfacial compatibility of the polyamide color master batch is obviously improved, carbon-carbon double bonds and isocyanate groups are contained in the compatilizer, the carbon-carbon double bonds can form hydrogen bonds with a base material, the isocyanate groups and polyurethane are subjected to a chemical crosslinking reaction, so that the compatilizer, a polyurethane matrix and a carbon black colorant are mutually wound to form a whole, the compatilizer plays a role of a bridge, the compatibility of the polyamide color master batch is improved, and the purposes of improving the stability and the coloring effect of the color master batch in polyamide are achieved.
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.
Example 1:
this example is a high temperature carbon black colored polyamide masterbatch, which is prepared by the following steps:
60 parts of carbon black, 100 parts of polyamide resin, 8 parts of dispersing agent, 2 parts of silane coupling agent, 1 part of compatilizer and 1 part of antioxidant;
s81: mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, and performing ultrasonic dispersion for 20 min;
s82: adding polyamide resin, stirring uniformly, mixing for 20min in an internal mixer, and extruding and granulating by a double-screw extruder to obtain the polyamide color master batch colored by the high-temperature resistant carbon black;
the dispersing agent is prepared by the following steps:
s21: placing 21.6g of weighed polyoxypropylene glycol into a three-neck flask, adding a thermometer, a condenser tube and a stirring rod, then carrying out vacuum dehydration for 30min at 100 ℃, cooling to 45 ℃, adding 26.68g of p-phenylene diisocyanate, introducing dry ammonia gas for protection, heating to 90 ℃, reacting for 3h, and cooling to 40 ℃ to obtain an intermediate A;
s22: adding 2.60g of 2, 2-dimethylolpropionic acid and 3.66g of 1, 4-butanediol into 32.5g of the intermediate A, adding 4g of acetone, heating to 80 ℃, reacting for 1 hour, and cooling to 45 ℃ to obtain an intermediate B;
s23: adding 3.5g of stannous octoate and 1.5g of dibutyltin dilaurate into 20.26g of the intermediate B, heating to 70 ℃, reacting for 3.5h, cooling to 40 ℃, adding 5.99g of polyethylene glycol, reacting for 3h, and cooling to 30 ℃ to obtain an intermediate C;
s24: putting 24.9g of the intermediate C into an emulsification barrel, adding 3.3mL of triethylamine for neutralization at the rotating speed of 1000r/min, adding 15mL of deionized water, and carrying out high-speed shearing emulsification for 10min to obtain the dispersing agent;
the compatilizer is prepared by the following steps:
s51: 10g of maleic anhydride and 13 g of maleic anhydride were weighed outAdding 5g of ethylene glycol into a four-mouth reaction bottle with a temperature control, stirring and reflux device, and introducing N2Protecting, heating at 10 ℃/min, reacting for 0.5h when the temperature is heated to 80 ℃, gradually dissolving maleic anhydride, adding dimethylbenzene as a water-carrying agent, heating to 140 ℃ at 10 ℃/min, reacting for 4h, adding a catalyst, heating to 190 ℃ at 5 ℃/min, reacting for 4h, cooling to 135 ℃, and carrying out vacuum pumping reaction for 2.5h to obtain an intermediate E;
s52: adding 15.9g of the intermediate E into a four-neck flask, heating to 130 ℃, vacuumizing to 0.06MPa, dehydrating for 2.5h, cooling to 70 ℃, adding 14.5g of 1, 4-butanediol and dibutyltin dilaurate, stirring and mixing uniformly, then adding 20.6g of p-phenylene diisocyanate, stirring, vacuumizing and defoaming, introducing nitrogen for protection, and reacting for 3.5h to obtain the compatilizer.
Example 2:
this example is a high temperature carbon black colored polyamide masterbatch, which is prepared by the following steps:
60 parts of carbon black, 100 parts of polyamide resin, 8 parts of dispersing agent, 5 parts of silane coupling agent, 5 parts of compatilizer and 5 parts of antioxidant;
s81: mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, and performing ultrasonic dispersion for 20 min;
s82: adding polyamide resin, stirring uniformly, mixing for 20min in an internal mixer, and extruding and granulating by a double-screw extruder to obtain the polyamide color master batch colored by the high-temperature resistant carbon black;
the dispersing agent is prepared by the following steps:
s21: placing 21.6g of weighed polyoxypropylene glycol into a three-neck flask, adding a thermometer, a condenser tube and a stirring rod, then carrying out vacuum dehydration for 30min at 100 ℃, cooling to 45 ℃, adding 26.68g of p-phenylene diisocyanate, introducing dry ammonia gas for protection, heating to 90 ℃, reacting for 3h, and cooling to 50 ℃ to obtain an intermediate A;
s22: adding 2.60g of 2, 2-dimethylolpropionic acid and 3.66g of 1, 4-butanediol into 32.5g of the intermediate A, adding 4g of acetone, heating to 80 ℃, reacting for 1h, and cooling to 45 ℃ to obtain an intermediate B;
s23: adding 3.5g of stannous octoate and 1.5g of dibutyltin dilaurate into 20.26g of the intermediate B, heating to 70 ℃, reacting for 3.5h, cooling to 40 ℃, adding 5.99g of polyethylene glycol, reacting for 3h, and cooling to 30 ℃ to obtain an intermediate C;
s24: putting 24.9g of the intermediate C into an emulsification barrel, adding 3.3mL of triethylamine for neutralization at the rotating speed of 1000r/min, adding 15mL of deionized water, and carrying out high-speed shearing emulsification for 10min to obtain the dispersing agent;
the compatilizer is prepared by the following steps:
s51: 10g of maleic anhydride and 13.5g of ethylene glycol are weighed into a four-neck reaction flask with a temperature control, stirring and reflux device, and N is introduced2Protecting, heating at 12 ℃/min, reacting for 1h when the temperature is raised to 90 ℃, gradually dissolving maleic anhydride, adding dimethylbenzene as a water-carrying agent, heating at 15 ℃/min to 145 ℃, reacting for 6h, adding a catalyst, heating at 8 ℃/min to 200 ℃, reacting for 6h, cooling to 140 ℃, and carrying out vacuum pumping reaction for 3h to obtain an intermediate E;
s52: adding 15.9g of the intermediate E into a four-neck flask, heating to 140 ℃, vacuumizing to 0.08MPa, dehydrating for 3 hours, cooling to 80 ℃, adding 14.5g of 1, 4-butanediol and dibutyltin dilaurate, stirring and mixing uniformly, then adding 20.6g of p-phenylene diisocyanate, stirring, vacuumizing and defoaming, introducing nitrogen for protection, and reacting for 5 hours to obtain the compatilizer.
Example 3:
this example is a high temperature carbon black colored polyamide masterbatch, which is prepared by the following steps:
60 parts of carbon black, 120 parts of polyamide resin, 10 parts of dispersing agent, 5 parts of silane coupling agent, 5 parts of compatilizer and 5 parts of antioxidant;
s81: mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, and performing ultrasonic dispersion for 30 min;
s82: adding polyamide resin, stirring uniformly, mixing in an internal mixer for 30min, and extruding and granulating by a double-screw extruder to obtain the polyamide color master batch colored by the high-temperature resistant carbon black;
the dispersing agent is prepared by the following steps:
s21: placing 21.6g of weighed polyoxypropylene glycol in a three-neck flask, adding a thermometer, a condenser and a stirring rod, then carrying out vacuum dehydration at 120 ℃ for 40min, cooling to 50 ℃, adding 26.68g of p-phenylene diisocyanate, introducing dry ammonia gas for protection, heating to 100 ℃, reacting for 5h, and cooling to 50 ℃ to obtain an intermediate A;
s22: adding 2.60g of 2, 2-dimethylolpropionic acid and 3.66g of 1, 4-butanediol into 32.5g of the intermediate A, adding 4g of acetone, heating to 90 ℃, reacting for 2 hours, and cooling to 50 ℃ to obtain an intermediate B;
s23: adding 3.5g of stannous octoate and 1.5g of dibutyltin dilaurate into 20.26g of the intermediate B, heating to 80 ℃, reacting for 3.5h, cooling to 50 ℃, adding 5.99g of polyethylene glycol, reacting for 5h, and cooling to 40 ℃ to obtain an intermediate C;
s24: placing 24.9g of the intermediate C in an emulsification barrel, adding 3.3mL of triethylamine for neutralization at the rotating speed of 1500r/min, adding 15mL of deionized water, and carrying out high-speed shearing emulsification for 20min to obtain the dispersing agent;
the compatilizer is prepared by the following steps:
s51: 10g of maleic anhydride and 13.5g of ethylene glycol are weighed into a four-neck reaction flask with a temperature control, stirring and reflux device, and N is introduced2Protecting, heating at 12 ℃/min, reacting for 1h when the temperature is raised to 90 ℃, gradually dissolving maleic anhydride, adding dimethylbenzene as a water-carrying agent, heating at 15 ℃/min to 145 ℃, reacting for 6h, adding a catalyst, heating at 8 ℃/min to 200 ℃, reacting for 6h, cooling to 140 ℃, and carrying out vacuum pumping reaction for 3h to obtain an intermediate E;
s52: adding 15.9g of the intermediate E into a four-neck flask, heating to 140 ℃, vacuumizing to 0.08MPa, dehydrating for 3 hours, cooling to 80 ℃, adding 14.5g of 1, 4-butanediol and dibutyltin dilaurate, stirring and mixing uniformly, then adding 20.6g of p-phenylene diisocyanate, stirring, vacuumizing and defoaming, introducing nitrogen for protection, and reacting for 5 hours to obtain the compatilizer.
Comparative example 1:
comparative example 1 differs from example 1 in that no dispersant is added.
Comparative example 2:
comparative example 2 differs from example 1 in that no compatibilizer is added.
Performance test
The polyurethane color masterbatches of examples 1 to 3 and comparative examples 1 to 2 were tested, the surface gloss of the compositions was measured using a surface gloss meter, the results of 60 ° were read, and the compositions were added to PA66 resin in an amount of 1%, molded at 200 ℃ to prepare square plates having a dimension length width thickness of 100mm 2mm, the surfaces of the square plates were bright, and the L, a, b values of the surfaces of the square plates were measured using a color difference meter;
the results are shown in the following table:
as can be seen from the above table, the gloss of the examples reaches 99, the gloss of the comparative example 1 without the dispersant is 88, the gloss of the comparative example 2 without the compatibilizer is 92, the hue L value of the examples is 13.5 to 14.8, the a value is-0.1, and the b value is-1.3 to-1.2, the hue L value of the comparative example 1 without the dispersant is 30.6, the a value is 0.2, the b value is 1.9, the hue L value of the comparative example 2 without the compatibilizer is 28.4, the a value is 0.2, and the b value is 0.7.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The polyamide color master batch capable of resisting high-temperature carbon black coloring is characterized by comprising the following components in parts by weight:
60-80 parts of carbon black, 100-120 parts of polyamide resin, 8-10 parts of a dispersing agent, 2-5 parts of a silane coupling agent, 1-5 parts of a compatilizer and 1-5 parts of an antioxidant;
the polyamide color master batch for coloring the high-temperature-resistant carbon black is prepared by the following steps:
s1: mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, and performing ultrasonic dispersion;
s2: and adding polyamide resin, stirring uniformly, mixing in an internal mixer, and extruding and granulating by a double-screw extruder to obtain the high-temperature-resistant carbon black colored polyamide color master batch.
2. The high temperature carbon black pigmented polyamide color masterbatch according to claim 1, wherein the dispersant is prepared by the steps of:
s21: placing polyoxypropylene glycol into a three-neck flask, adding p-phenylene diisocyanate and introducing dry nitrogen for protection to obtain an intermediate A;
s22: adding 2, 2-dimethylolpropionic acid and 1, 4-butanediol into the intermediate A, and adding acetone to obtain an intermediate B;
s23: adding stannous octoate and dibutyltin dilaurate into the intermediate B, and adding polyethylene glycol to obtain an intermediate C;
s24: and (3) placing the intermediate C in an emulsification barrel, adding triethylamine for neutralization, adding deionized water, and carrying out high-speed shearing emulsification to obtain the dispersing agent.
3. The high temperature carbon black coloration polyamide color masterbatch according to claim 2, wherein the amount ratio of polyoxypropylene to p-phenylene diisocyanate in step S21 is 21.6 g: 26.68g, the dosage ratio of the intermediate A, the 2, 2-dimethylolpropionic acid, the 1, 4-butanediol and the acetone in the step S22 is 32.5 g: 2.60 g: 3.66 g: 4g of the total weight.
4. The high temperature carbon black coloration polyamide color masterbatch according to claim 2, wherein the amount ratio of intermediate B, stannous octoate, dibutyltin dilaurate to polyethylene glycol in step S23 is 20.26 g: 3.5 g: 1.5 g: 5.99g, wherein the dosage ratio of the intermediate C, triethylamine and deionized water in the step S24 is 24.9 g: 3.3 mL: 15 mL.
5. The high temperature carbon black pigmented polyamide color masterbatch according to claim 1, wherein the compatibilizer is prepared by the steps of:
s51: weighing maleic anhydride and ethylene glycol, adding into a four-mouth reaction bottle, and introducing N2Protecting, and adding a catalyst to obtain an intermediate E;
s52: and adding the intermediate E into a four-neck flask, adding 1, 4-butanediol and dibutyltin dilaurate, and then adding p-phenylene diisocyanate to obtain the compatilizer.
6. The high temperature carbon black coloration polyamide color masterbatch according to claim 5, wherein the ratio of the amounts of maleic anhydride and ethylene glycol used in step S51 is 10 g: 13.5g, wherein the catalyst is p-toluenesulfonic acid, the amount of the catalyst is 5% of the mass of the maleic anhydride, and the ratio of the amount of the intermediate E to the amount of the 1, 4-butanediol to the amount of the p-phenylene diisocyanate in step S52 is 15.9 g: 14.5 g: 20.6g, and the using ratio of the dibutyltin dilaurate is 3% of the mass of the intermediate E.
7. The high temperature carbon black colorable polyamide color masterbatch of claim 1 wherein said silane coupling agent is vinyltriethoxysilane, and said antioxidant is hindered phenolic antioxidant in step S1.
8. The process for the preparation of a high temperature carbon black pigmented polyamide color masterbatch according to any of claims 1-7, characterized in that it comprises the following steps:
the polyamide color master batch for coloring the high-temperature-resistant carbon black is prepared by the following steps:
s1: mixing carbon black, a silane coupling agent, a dispersing agent, a compatilizer and an antioxidant, and performing ultrasonic dispersion;
s2: and adding polyamide resin, stirring uniformly, mixing in an internal mixer, and extruding and granulating by a double-screw extruder to obtain the high-temperature-resistant carbon black colored polyamide color master batch.
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