CN119307044B - An antistatic PP composite material based on high gloss carbon black and preparation method thereof - Google Patents
An antistatic PP composite material based on high gloss carbon black and preparation method thereof Download PDFInfo
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
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Abstract
The invention relates to an antistatic PP composite material based on high-gloss carbon black and a preparation method thereof, and belongs to the technical field of polypropylene composite materials, wherein the composite material comprises, by weight, 100 parts of PP resin, 15-20 parts of POE resin, 8.5-12 parts of high-gloss carbon black, 0.6-0.8 part of antistatic auxiliary agent, 10-15 parts of filler, 2.5-3.5 parts of lubricant and 0.12-0.15 part of antioxidant, the surface of the high-gloss carbon black is smooth, scattering and absorption of light among carbon black particles are reduced, more light can directly pass through plastics or be reflected on the surface of the carbon black instead of being scattered to all directions, and further the glossiness of the composite material is higher.
Description
Technical Field
The invention belongs to the technical field of polypropylene compounding, and particularly relates to an antistatic PP composite material based on high-gloss carbon black and a preparation method thereof.
Background
Polypropylene (PP) materials are widely used in various industries as an important thermoplastic due to their excellent chemical stability and cost effectiveness. Polypropylene is particularly favored in the composite and decorative fields due to its light weight, dimensional stability, and chemical resistance.
However, pure polypropylene materials have poor antistatic properties and tend to accumulate static electricity in certain environments, which limits the range of applications in certain static-sensitive applications, particularly in facing materials, where static electricity tends to adsorb dust from the air, resulting in an aesthetically undesirable facing.
In order to overcome the problems, the prior art adopts various methods including adding conductive fillers to reduce the electrostatic property of the polypropylene material, wherein carbon black is an ideal conductive filler, has remarkable effect on long-acting antistatic property due to extremely high conductive property and low cost, but carbon black particles have complex porous structure and more surface area, so that the carbon black particles can effectively absorb or scatter light, and the surface glossiness of the polypropylene material is reduced, so that the polypropylene product loses transparency and smooth appearance, and the application of the carbon black particles in the fields with higher decorative and luster requirements is obviously limited.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention aims to provide an antistatic PP composite material based on high-gloss carbon black and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
The antistatic PP composite material based on the high-gloss carbon black comprises, by weight, 100 parts of PP resin, 15-20 parts of POE resin, 8.5-12 parts of high-gloss carbon black, 0.6-0.8 part of antistatic auxiliary agent, 10-15 parts of filler, 2.5-3.5 parts of lubricant and 0.12-0.15 part of antioxidant.
The high gloss carbon black is prepared by the following method:
Step A1, pre-heating pentaerythritol tetraacrylate, p-hydroxy thiophenol and ethyl acetate for miscibility, introducing nitrogen for protection, adding a photoinitiator for uniform mixing, controlling the temperature to be 55-70 ℃, adopting 150-220W/m 2 ultraviolet irradiation, applying 90-120rpm for stirring reaction for 2.5-3.5 hours, and removing the ethyl acetate after the reaction is finished to obtain the surface modifier;
Further, the feeding ratio of pentaerythritol tetraacrylate, p-hydroxy thiophenol, photoinitiator and ethyl acetate is 10mmol:40mmol:6-10mg:80-110mL, under the ultraviolet initiation, the active thiophenol structure of the p-hydroxy thiophenol and the terminal double bond of the pentaerythritol tetraacrylate are subjected to click addition, and the specific reaction process can be expressed as follows:
A2, heating and mixing the surface modifier and acetone, adding conductive carbon black for ultrasonic dispersion, standing the dispersion for 24 hours, taking a bottom sediment, washing the bottom sediment with ethanol, centrifuging again, taking the sediment, and vacuum drying the sediment to constant weight to obtain modified carbon black;
Further, the feeding ratio of the conductive carbon black to the surface modifier to the acetone is 50g:3.2-4.4g:270-350mL, the molecules of the surface modifier are relatively high, the molecules contain a large number of benzene ring structures, the porous structure on the surface of the conductive carbon black has a strong adsorption effect, and the surface modifier is adsorbed and loaded on the surface pore wall of the conductive carbon black to form composite modification;
Preferably, the conductive carbon black has an average particle diameter of 30-50nm, and in the particle diameter range, the conductive carbon black is favorable for dispersion and coloring of the carbon black and formation of a continuous conductive network, and meanwhile, the conductive carbon black has good adsorptivity, and the surface modifier is effectively loaded in the gaps.
Step A3, stirring and dispersing the modified carbon black, aniline and tetrahydrofuran, adding hydrochloric acid for mixing, controlling the water bath temperature to be 40-60 ℃, slowly adding ammonium persulfate solution for reaction for 3.5-5.5 hours, centrifuging after the reaction is finished, taking precipitate, washing the precipitate with water to be neutral, and drying to obtain high-gloss carbon black;
Further, the feeding ratio of the modified carbon black to the aniline to the ammonium persulfate to the hydrochloric acid to the tetrahydrofuran is 50g:7.8-9.5g:1.2-1.8g:300-400mL:70-90mL, a large amount of ester groups and phenolic hydroxyl groups are contained in the surface modifier molecules adsorbed on the surface of the modified carbon black, hydrogen bonding is generated between the surface modifier molecules and the aniline, the aniline is enriched in the surface gaps of the modified carbon black, protons are provided for the phenolic hydroxyl groups, so that aniline molecules in the gaps are protonated, a polymerization process is preferentially started, and polyaniline sealing is formed in the carbon black gaps.
Preferably, the antistatic aid is selected from anionic antistatic agents that synergistically reduce the surface resistance of the composite.
Preferably, the filler is compounded by talcum powder and glass fiber powder.
The preparation method of the antistatic PP composite material based on the high-gloss carbon black comprises the steps of premixing the high-gloss carbon black, an antistatic auxiliary agent and a filler, then melting and blending PP resin, POE resin, a lubricant and an antioxidant at 180-190 ℃, adding the premix, continuously heating to 210 ℃ for banburying until torque is stable, discharging and cooling to obtain the PP composite material.
The invention has the beneficial effects that:
The invention is based on the carbon black composite PP antistatic material, carries out surface modification on the traditional carbon black to prepare high-gloss carbon black, and endows the composite material with good antistatic performance and high glossiness after being blended with the PP material, thereby having wide application prospect in the high-gloss antistatic facing material; compared with the common carbon black materials, the high-gloss carbon black disclosed by the invention has the advantages that the scattering and absorption of light among carbon black particles are reduced, more light can directly pass through plastics or be reflected on the surfaces of the carbon black, the glossiness of the composite material is higher, in addition, the carbon black is used as a disperse phase in the composite material, the surface smoothness of the carbon black is easier to be uniformly dispersed in the material, and the surface smoothness of the carbon black is easier to be used as a disperse phase, so that the polyaniline is easy to be uniformly dispersed in the material, and the surface smoothness of the carbon black is better in electrostatic conductivity, so that the polyaniline is good in conductivity, and the electric conductivity of the composite material is remarkably improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an electron microscopic image of the high gloss carbon black prepared in example 4 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1 an antistatic PP composite based on high gloss carbon black was prepared, the specific implementation procedure being as follows:
(1) Preparation of high gloss carbon black
Step A1, pre-heating pentaerythritol tetraacrylate, p-hydroxy thiophenol and ethyl acetate to 40 ℃ for mixing, introducing nitrogen for protection, adding a photoinitiator for uniform mixing, controlling the temperature to 70 ℃, adopting 150W/m 2 ultraviolet irradiation, and applying 120rpm for stirring reaction for 2.5 hours, wherein the feeding ratio of the pentaerythritol tetraacrylate, the p-hydroxy thiophenol, the photoinitiator and the ethyl acetate is 10mmol:40mmol:6mg:110mL, the photoinitiator is selected from the photoinitiator 1173, and the ethyl acetate is removed by rotary evaporation after the reaction is finished, so that the surface modifier is obtained.
And A2, heating the surface modifier and acetone to 50 ℃ for mixing, adding conductive carbon black for ultrasonic dispersion, and standing the dispersion for 24 hours, wherein the feeding ratio of the conductive carbon black to the surface modifier to the acetone is 50g:3.2g:270mL, the conductive carbon black is selected from LI-400 type raw materials, the average particle size is 48nm, then taking a bottom sediment, washing the bottom sediment with ethanol, centrifuging again, taking the sediment, and vacuum drying the sediment to constant weight to obtain the modified carbon black.
And A3, stirring and dispersing the modified carbon black, aniline and tetrahydrofuran, adding hydrochloric acid for mixing, controlling the temperature in a water bath to be 60 ℃, applying 90rpm for stirring, slowly adding ammonium persulfate solution for reaction for 3.5 hours, wherein the feeding ratio of the modified carbon black, aniline, ammonium persulfate, hydrochloric acid and tetrahydrofuran is 50g to 7.8g to 1.2g to 300mL to 70mL, the ammonium persulfate solution is saturated aqueous solution at room temperature, the concentration of hydrochloric acid is 1mol/L, centrifuging after the reaction is finished, taking the precipitate, washing with water to be neutral, and drying to obtain the high-gloss carbon black.
(2) Preparation of PP composite material
The raw materials are 100 parts of PP resin, 20 parts of POE resin, 670-type LC resin, 12 parts of high-gloss carbon black, 0.8 part of antistatic auxiliary agent selected from sodium dodecyl benzene sulfonate, 10 parts of filler selected from talcum powder and glass fiber powder according to the weight ratio of 2:1, 3.5 parts of lubricant selected from calcium stearate and 0.12 part of antioxidant selected from antioxidant 1010 and antioxidant 168 according to the weight ratio of 1:1.
And (3) blending, namely premixing high-gloss carbon black, an antistatic additive and a filler, then carrying out melt blending on PP resin, POE resin, a lubricant and an antioxidant at 180 ℃, adding the premix, continuously heating to 210 ℃ for banburying until the torque is stable, discharging and cooling to obtain the PP composite material.
Example 2 an antistatic PP composite based on high gloss carbon black was prepared, the specific implementation procedure being as follows:
(1) Preparation of high gloss carbon black
Step A1, pre-heating pentaerythritol tetraacrylate, p-hydroxy thiophenol and ethyl acetate to 40 ℃ for mixing, introducing nitrogen for protection, adding a photoinitiator for uniform mixing, controlling the temperature to 55 ℃, adopting 220W/m 2 ultraviolet irradiation, and applying 90rpm for stirring reaction for 3.5 hours, wherein the feeding ratio of the pentaerythritol tetraacrylate, the p-hydroxy thiophenol, the photoinitiator and the ethyl acetate is 10mmol:40mmol:10mg:80mL, the photoinitiator is selected from the photoinitiator 1173, and the ethyl acetate is removed after the reaction is finished by rotary evaporation, so that the surface modifier is obtained.
And A2, heating the surface modifier and acetone to 50 ℃ for mixing, adding conductive carbon black for ultrasonic dispersion, and standing the dispersion for 24 hours, wherein the feeding ratio of the conductive carbon black to the surface modifier to the acetone is 50g:4.4g:350mL, the conductive carbon black is selected from VULCAN XC-72 type raw materials, the average particle size is 30nm, then taking a bottom sediment, washing the bottom sediment with ethanol, centrifuging again, taking the sediment, and vacuum drying to constant weight to obtain the modified carbon black.
And A3, stirring and dispersing the modified carbon black, aniline and tetrahydrofuran, adding hydrochloric acid for mixing, controlling the temperature in a water bath to be 40 ℃, applying 60rpm for stirring, slowly adding ammonium persulfate solution for reacting for 5.5 hours, wherein the feeding ratio of the modified carbon black, aniline, ammonium persulfate, hydrochloric acid and tetrahydrofuran is 50g:9.5g:1.8g:400mL:90mL, the ammonium persulfate solution is saturated aqueous solution at room temperature, the concentration of hydrochloric acid is 1mol/L, centrifuging after the reaction is finished, taking the precipitate, washing with water to be neutral, and drying to obtain the high-gloss carbon black.
(2) Preparation of PP composite material
The raw materials are 100 parts of PP resin, 15 parts of POE resin, 670-type LC resin, 8.5 parts of high-gloss carbon black, 0.6 part of antistatic auxiliary agent selected from sodium dodecyl benzene sulfonate, 15 parts of filler selected from talcum powder and glass fiber powder according to the weight ratio of 2:1, 2.5 parts of lubricant selected from calcium stearate and 0.15 part of antioxidant selected from antioxidant 1010 and antioxidant 168 according to the weight ratio of 1:1.
And (3) blending, namely premixing high-gloss carbon black, an antistatic additive and a filler, then carrying out melt blending on PP resin, POE resin, a lubricant and an antioxidant at 190 ℃, adding the premix, continuously heating to 210 ℃ for banburying until torque is stable, discharging and cooling to obtain the PP composite material.
Example 3 an antistatic PP composite based on high gloss carbon black was prepared, the specific implementation procedure being as follows:
(1) Preparation of high gloss carbon black
Step A1, pre-heating pentaerythritol tetraacrylate, p-hydroxy thiophenol and ethyl acetate to 40 ℃ for mixing, introducing nitrogen for protection, adding a photoinitiator for uniform mixing, controlling the temperature to 60 ℃, adopting 180W/m 2 ultraviolet irradiation, and applying 120rpm for stirring reaction for 3.2h, wherein the feeding ratio of the pentaerythritol tetraacrylate, the p-hydroxy thiophenol, the photoinitiator and the ethyl acetate is 10mmol:40mmol:8mg:100mL, the photoinitiator is selected from the photoinitiator 1173, and the ethyl acetate is removed after the reaction is finished by rotary evaporation, so that the surface modifier is obtained.
And A2, heating the surface modifier and acetone to 50 ℃ for mixing, adding conductive carbon black for ultrasonic dispersion, and standing the dispersion for 24 hours, wherein the feeding ratio of the conductive carbon black to the surface modifier to the acetone is 50g:3.8g:300mL, the conductive carbon black is selected from LI-400 type raw materials, the average particle size is 48nm, then taking a bottom sediment, washing the bottom sediment with ethanol, centrifuging again, taking the sediment, and vacuum drying the sediment to constant weight to obtain the modified carbon black.
And A3, stirring and dispersing the modified carbon black, aniline and tetrahydrofuran, adding hydrochloric acid for mixing, controlling the temperature in a water bath to be 55 ℃, applying 90rpm for stirring, slowly adding ammonium persulfate solution for reacting for 4.5 hours, wherein the feeding ratio of the modified carbon black, aniline, ammonium persulfate, hydrochloric acid and tetrahydrofuran is 50g:9g:1.4g:400mL:90mL, the ammonium persulfate solution is saturated aqueous solution at room temperature, the concentration of hydrochloric acid is 1mol/L, centrifuging after the reaction is finished, taking the precipitate, washing with water to be neutral, and drying to obtain the high-gloss carbon black.
(2) Preparation of PP composite material
The raw materials are 100 parts of PP resin, 17 parts of POE resin, 670-type LC resin, 10 parts of high-gloss carbon black, 0.7 part of antistatic auxiliary agent selected from sodium dodecyl benzene sulfonate, 12 parts of filler selected from talcum powder and glass fiber powder according to the weight ratio of 2:1, 3.2 parts of lubricant selected from calcium stearate and 0.15 part of antioxidant selected from antioxidant 1010 and antioxidant 168 according to the weight ratio of 1:1.
And (3) blending, namely premixing high-gloss carbon black, an antistatic additive and a filler, then carrying out melt blending on PP resin, POE resin, a lubricant and an antioxidant at 180 ℃, adding the premix, continuously heating to 210 ℃ for banburying until the torque is stable, discharging and cooling to obtain the PP composite material.
Example 4 an antistatic PP composite based on high gloss carbon black was prepared, the specific implementation procedure being as follows:
(1) Preparation of high gloss carbon black
Step A1, pre-heating pentaerythritol tetraacrylate, p-hydroxy thiophenol and ethyl acetate to 40 ℃ for mixing, introducing nitrogen for protection, adding a photoinitiator for uniform mixing, controlling the temperature to 65 ℃, adopting 180W/m 2 ultraviolet irradiation, and applying 120rpm for stirring reaction for 2.8 hours, wherein the feeding ratio of the pentaerythritol tetraacrylate, the p-hydroxy thiophenol, the photoinitiator and the ethyl acetate is 10mmol:40mmol:8mg:100mL, the photoinitiator is selected from the photoinitiator 1173, and the ethyl acetate is removed after the reaction is finished by rotary evaporation, so that the surface modifier is obtained.
And A2, heating the surface modifier and acetone to 50 ℃ for mixing, adding conductive carbon black for ultrasonic dispersion, and standing the dispersion for 24 hours, wherein the feeding ratio of the conductive carbon black to the surface modifier to the acetone is 50g:4g:300mL, the conductive carbon black is selected from VULCAN XC-72 type raw materials, the average particle size is 30nm, then taking a bottom sediment, washing the bottom sediment with ethanol, centrifuging again, taking the sediment, and vacuum drying the sediment to constant weight to obtain the modified carbon black.
And A3, stirring and dispersing the modified carbon black, aniline and tetrahydrofuran, adding hydrochloric acid for mixing, controlling the temperature in a water bath to be 50 ℃, applying 90rpm for stirring, slowly adding ammonium persulfate solution for reacting for 5 hours, wherein the feeding ratio of the modified carbon black to the aniline to the ammonium persulfate to the hydrochloric acid to the tetrahydrofuran is 50g to 9g to 1.6g to 350mL to 80mL, the ammonium persulfate solution is saturated aqueous solution at room temperature, the concentration of hydrochloric acid is 1mol/L, centrifuging after the reaction, taking the precipitate for washing to be neutral, and drying to obtain the high-gloss carbon black.
(2) Preparation of PP composite material
The raw materials are 100 parts of PP resin, 18 parts of POE resin, 670-type LC resin, 11 parts of high-gloss carbon black, 0.7 part of antistatic auxiliary agent selected from sodium dodecyl benzene sulfonate, 13 parts of filler selected from talcum powder and glass fiber powder according to the weight ratio of 2:1, 3 parts of lubricant selected from calcium stearate and 0.15 part of antioxidant selected from antioxidant 1010 and antioxidant 168 according to the weight ratio of 1:1.
And (3) blending, namely premixing high-gloss carbon black, an antistatic additive and a filler, then carrying out melt blending on PP resin, POE resin, a lubricant and an antioxidant at 190 ℃, adding the premix, continuously heating to 210 ℃ for banburying until torque is stable, discharging and cooling to obtain the PP composite material.
Comparative example 1 the high gloss carbon black of example 4 was replaced with a commercial high gloss carbon black of the Raven 1060 Ultra type, and the remainder of the procedure was identical to example 3.
Comparative example 2, preparation of polyaniline-carbon black particles by referring to the prior art, specifically, the method comprises the steps of stirring aniline and hydrochloric acid for dispersion, adding conductive carbon black for ultrasonic dispersion for 30min, slowly adding ammonium persulfate solution into the dispersion, controlling the adding reaction time to be 8h, wherein the feeding ratio of the conductive carbon black to the aniline to the ammonium persulfate to the hydrochloric acid is 50g to 10g to 2.2g to 500mL, centrifuging at the end of the reaction, taking the precipitate, washing the precipitate to be neutral, drying to obtain polyaniline-carbon black particles, and replacing the high-gloss carbon black in example 4 with the same amount, wherein the rest implementation processes are completely the same.
Taking materials from the PP composite material obtained in the above way, hot-pressing the materials into sheets by adopting a flat vulcanizing machine at 220 ℃ and 2.0MPa, cutting the sheets, detecting surface resistivity by referring to IEC 61340 5-1-2016 standard, detecting electrostatic decay time by referring to ANSI/ESD S20.20-2021 standard, detecting 60-DEG angular glossiness by referring to GB/T8807-1988 standard, and specifically detecting the results shown in table 1:
TABLE 1 test sample antistatic Properties and gloss test results
As can be seen from the test results in Table 1, the examples have good antistatic properties while maintaining higher gloss than the comparative examples, and the high-gloss carbon black prepared in example 4 was observed by electron microscopy based on the above test results, particularly as shown in FIG. 1, and the high-gloss carbon black has a spheroid-like shape and a relatively smooth surface.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, 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 present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. 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 merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
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| CN114874543A (en) * | 2022-05-05 | 2022-08-09 | 安徽超星新材料科技有限公司 | High-strength conductive plastic and preparation method thereof |
| CN117229655A (en) * | 2023-09-14 | 2023-12-15 | 安徽光理智能科技有限公司 | Modified carbon black and preparation method and application thereof |
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