CN114539738B - Preparation method of antistatic PET material - Google Patents
Preparation method of antistatic PET material Download PDFInfo
- Publication number
- CN114539738B CN114539738B CN202210315528.2A CN202210315528A CN114539738B CN 114539738 B CN114539738 B CN 114539738B CN 202210315528 A CN202210315528 A CN 202210315528A CN 114539738 B CN114539738 B CN 114539738B
- Authority
- CN
- China
- Prior art keywords
- zinc oxide
- stirring
- percent
- reaction
- pet material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a preparation method of an antistatic PET material, which belongs to the technical field of plastic preparation and comprises the following steps: firstly, dispersing aniline grafted nano zinc oxide in deionized water by ultrasonic, adding an ethanol solution of p-aminobenzoic acid, dropwise adding an ammonium persulfate solution at room temperature, stirring and reacting for 4-6 hours at 50 ℃ to obtain modified zinc oxide particles, and secondly, preparing the following raw materials in percentage by mass: 0.3 to 2.0 percent of antioxidant, 0.05 to 0.5 percent of lubricant, 0.1 to 1 percent of nucleating agent, 2 percent of modified zinc oxide particles, 0.3 to 0.5 percent of quaternary ammonium salt compound and the balance of PET resin; and thirdly, uniformly mixing all the raw materials in the second step, and then transferring the mixture into a double-screw extruder for melt extrusion granulation to obtain the antistatic PET material.
Description
Technical Field
The invention belongs to the technical field of plastic preparation, and particularly relates to a preparation method of an antistatic PET material.
Background
PET (polyethylene terephthalate) has the characteristics of high strength, good wear resistance, good rebound resilience, low cost and the like, so that the PET occupies a considerable proportion in textiles, and is engineering plastic with excellent performance and wide application. But the PET has high resistivity, the moisture absorption rate is only 0.4% under the conditions of 65% relative humidity and 25 ℃, and the resistivity is as high as 10 14 Omega cm, static electricity is extremely easy to generate, thereby limiting the application of the composite material in industries such as electronics, electrics and the like.
Antistatic PET is PET with antistatic properties, and the resistivity of PET is generally reduced by adding an antistatic agent, however, there are some points to be noted when antistatic modification is performed on PET: firstly, the processing temperature is high, and the heat resistance of the antistatic agent is high; secondly, the transparency of PET should not be affected as much as possible in the modification process; thirdly, the antistatic agent should not be easy to migrate and run off, so providing a PET material with good antistatic performance and meeting the above conditions is a technical problem to be solved at present.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a preparation method of an antistatic PET material.
The aim of the invention can be achieved by the following technical scheme:
the preparation method of the antistatic PET material comprises the following steps:
firstly, preparing the following raw materials in percentage by mass: 0.3 to 2.0 percent of antioxidant, 0.05 to 0.5 percent of lubricant, 0.1 to 1 percent of nucleating agent, 2 percent of modified zinc oxide particles, 0.3 to 0.5 percent of quaternary ammonium salt compound and the balance of PET resin;
and secondly, adding the PET resin, the antioxidant, the lubricant, the nucleating agent, the modified zinc oxide particles and the quaternary ammonium salt compound into a high-speed mixer, uniformly mixing, and transferring into a double-screw extruder for melt extrusion granulation to obtain the antistatic PET material, wherein the temperature of each section of a machine barrel of the double-screw extruder is respectively one zone 245 ℃, two zones 255 ℃, three zones 260 ℃ and four zones 250 ℃.
Further, the modified zinc oxide particles are made by the steps of:
step A1, adding zinc nitrate and gallium nitrate into distilled water, stirring uniformly, adding polyvinylpyrrolidone, stirring for 20-30min, adding a sodium hydroxide solution with the concentration of 0.1mol/L to adjust the pH value to 10-11, stirring at constant temperature for 30min to obtain a precursor solution, transferring the precursor solution into a hydrothermal reaction kettle, performing hydrothermal reaction at 160 ℃ for 3h, centrifuging and filtering after the reaction is finished, washing the precipitate, and drying in a baking oven at 75 ℃ until the weight is constant to obtain the doped nano zinc oxide;
wherein, the dosage ratio of zinc nitrate, gallium nitrate, distilled water and polyvinylpyrrolidone is 100g:1.8-2.1g:200mL:1-2g, preparing gallium-doped nano zinc oxide by a hydrothermal synthesis method, so that Ga element is doped into ZnO crystal lattice, and the conductivity of the ZnO crystal lattice is improved;
step A2, ultrasonically dispersing the doped nano zinc oxide in an ethanol solution with the mass fraction of 50%, then adding a coupling agent KH-590, magnetically stirring and reacting for 6-8h, centrifuging after the reaction is finished, washing and drying the precipitate to obtain an intermediate product; adding an intermediate product and 4-vinylaniline into toluene under the protection of nitrogen, stirring at the rotating speed of 60-80r/min for 5min, heating to 40 ℃, adding triethylamine as a catalyst, carrying out reflux reaction for 50min, cooling to room temperature, filtering, and distilling a filter cake to remove a solvent to obtain aniline grafted nano zinc oxide;
wherein, the dosage ratio of the doped nano zinc oxide to the ethanol solution to the KH-590 is 10g:100-120mL:0.3-0.5g, the dosage ratio of the intermediate product, 4-vinylaniline, triethylamine and toluene is 10g:1.4-1.6g:0.2-0.4g:110-120mL, carrying out surface modification treatment on the doped nano zinc oxide by using a coupling agent KH-590 to enable the surface of the doped nano zinc oxide to be rich in-SH bonds, and then carrying out addition reaction on the-SH bonds and-C=C-of 4-vinylaniline under the catalysis of triethylamine to obtain aniline grafted nano zinc oxide;
step A3, dispersing aniline grafted nano zinc oxide in deionized water by ultrasonic, then adding an ethanol solution of p-aminobenzoic acid, dropwise adding an ammonium persulfate solution at room temperature, stirring at 50 ℃ for reaction for 4-6 hours after the dropwise adding is finished, carrying out suction filtration after the reaction is finished, and drying a filter cake at 60 ℃ to constant weight to obtain modified zinc oxide particles;
wherein the dosage ratio of the aniline grafted nano zinc oxide, deionized water, ethanol solution of p-aminobenzoic acid and ammonium persulfate solution is 4-5g:40mL:6-6.5mL:40-50mL of ethanol solution of para-aminobenzoic acid, wherein the dosage ratio of the para-aminobenzoic acid to the ethanol is 2.4g:6mL of ammonium persulfate solution is prepared by mixing ammonium persulfate, deionized water and 10% mass fraction acetic acid solution according to the dosage ratio of 0.4g:50mL:2mL of the mixture.
Further, the quaternary ammonium salt compound is prepared by the steps of:
step B1, adding triethanolamine and 9H-carbazole-2, 7-dicarboxylic acid into a three-neck flask, heating to 100 ℃, stirring for 20-25min, adding p-toluenesulfonic acid, heating to 130 ℃, stirring and reacting for 2.5-3H, and obtaining an intermediate product 1 after the reaction is finished;
wherein the dosage ratio of triethanolamine, 9H-carbazole-2, 7-dicarboxylic acid and p-toluenesulfonic acid is 6g:7.65-9.18g:0.05-0.07g, under the catalysis of p-toluenesulfonic acid, carrying out esterification reaction on triethanolamine and 9H-carbazole-2, 7-dicarboxylic acid to obtain an intermediate product 1;
step B2, placing the intermediate product 1 in DMF, adding sodium chloroacetate, stirring at 80 ℃ for reaction for 7 hours, and removing DMF by reduced pressure distillation after the reaction is finished to obtain a quaternary ammonium salt compound;
wherein, the dosage ratio of the intermediate 1, DMF and sodium chloroacetate is 10g:150-200mL:4.6-5.1g, and the intermediate product 1 and sodium chloroacetate undergo quaternization reaction to obtain a quaternary ammonium salt compound.
The quaternary ammonium salt compound is prepared to enhance the antistatic performance of PET materials, the traditional quaternary ammonium salt compound antistatic agent has poor heat resistance and is easy to separate out, and the antistatic effect is difficult to be stably exerted when the quaternary ammonium salt compound is added into PET materials.
Further, the antioxidant is one or more of antioxidant 1010, antioxidant 1076 and antioxidant B215, which are mixed according to any proportion.
Further, the nucleating agent is one of talcum powder, sodium carboxylate and polytetrafluoroethylene with the particle size of 0.5-1.4 mu m.
Further, the lubricant is formed by mixing pentaerythritol stearate and silicone powder according to the mass ratio of 1-3:4-7.
The invention has the beneficial effects that:
according to the invention, the antistatic performance of the PET resin is improved by adding the modified zinc oxide particles and the quaternary ammonium salt compound into the PET resin, wherein the modified zinc oxide particles take gallium-doped nano zinc oxide as a base material, and then a polyaniline coating layer is formed on the surface of the gallium-doped nano zinc oxide by technical means such as chemical grafting, monomer polymerization and the like.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, 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
The invention provides modified zinc oxide particles, which are prepared by the following steps:
step A1, adding 100g of zinc nitrate and 1.8g of gallium nitrate into 200mL of distilled water, stirring uniformly, adding 1g of polyvinylpyrrolidone, stirring for 20min, adding a sodium hydroxide solution with the concentration of 0.1mol/L to adjust the pH value to 10, stirring at constant temperature for 30min to obtain a precursor solution, transferring the precursor solution into a hydrothermal reaction kettle, performing hydrothermal reaction at 160 ℃ for 3h, centrifuging after the reaction is finished, washing the precipitate, and drying in a drying oven at 75 ℃ to constant weight to obtain the doped nano zinc oxide;
step A2, dispersing 10g of doped nano zinc oxide in 100mL of ethanol solution with the mass fraction of 50%, then adding 0.3g of coupling agent KH-590, magnetically stirring and reacting for 6h, centrifuging after the reaction is finished, washing and drying the precipitate to obtain an intermediate product; under the protection of nitrogen, adding 10g of intermediate product and 1.4g of 4-vinylaniline into 110mL of toluene, stirring at a rotating speed of 60r/min for 5min, heating to 40 ℃, adding 0.2g of triethylamine, carrying out reflux reaction for 50min, cooling to room temperature, filtering, and distilling a filter cake to remove a solvent to obtain aniline grafted nano zinc oxide;
step A3, dispersing 4g of aniline grafted nano zinc oxide in 40mL of deionized water by ultrasonic, then adding an ethanol solution of p-aminobenzoic acid, dropwise adding an ammonium persulfate solution at room temperature, stirring at 50 ℃ for reaction for 4 hours after the dropwise adding is finished, carrying out suction filtration after the reaction is finished, and drying a filter cake at 60 ℃ to constant weight to obtain modified zinc oxide particles, wherein the ethanol solution of p-aminobenzoic acid is prepared from 2.4g of p-aminobenzoic acid and ethanol: 6mL of the mixture is mixed, and the ammonium persulfate solution is prepared from ammonium persulfate, deionized water and 10% acetic acid solution according to the mass fraction of 0.4g:50mL:2mL of the mixture.
Example 2
The invention provides modified zinc oxide particles, which are prepared by the following steps:
step A1, adding 100g of zinc nitrate and 1.9g of gallium nitrate into 200mL of distilled water, stirring uniformly, adding 1.5g of polyvinylpyrrolidone, stirring for 20min, adding a sodium hydroxide solution with the concentration of 0.1mol/L to adjust the pH value to 10, stirring at constant temperature for 30min to obtain a precursor solution, transferring the precursor solution into a hydrothermal reaction kettle, performing hydrothermal reaction at 160 ℃ for 3h, centrifuging after the reaction is finished, washing the precipitate, and drying in a drying oven at 75 ℃ until the weight is constant to obtain the doped nano zinc oxide;
step A2, dispersing 10g of doped nano zinc oxide in 100mL of ethanol solution with the mass fraction of 50%, then adding 0.3g of coupling agent KH-590, magnetically stirring and reacting for 6h, centrifuging after the reaction is finished, washing and drying the precipitate to obtain an intermediate product; under the protection of nitrogen, adding 10g of intermediate product and 1.4g of 4-vinylaniline into 110mL of toluene, stirring at a rotating speed of 60r/min for 5min, heating to 40 ℃, adding 0.3g of triethylamine, carrying out reflux reaction for 50min, cooling to room temperature, filtering, and distilling a filter cake to remove a solvent to obtain aniline grafted nano zinc oxide;
step A3, dispersing 4.5g of aniline grafted nano zinc oxide in 40mL of deionized water by ultrasonic, then adding an ethanol solution of p-aminobenzoic acid, dropwise adding an ammonium persulfate solution at room temperature, stirring at 50 ℃ for reaction for 5 hours after the dropwise adding is finished, carrying out suction filtration after the reaction is finished, and drying a filter cake at 60 ℃ to constant weight to obtain modified zinc oxide particles, wherein the ethanol solution of p-aminobenzoic acid is prepared from 2.4g of p-aminobenzoic acid and ethanol: 6mL of the mixture is mixed, and the ammonium persulfate solution is prepared from ammonium persulfate, deionized water and 10% acetic acid solution according to the mass fraction of 0.4g:50mL:2mL of the mixture.
Example 3
The invention provides modified zinc oxide particles, which are prepared by the following steps:
step A1, adding 100g of zinc nitrate and 2.1g of gallium nitrate into 200mL of distilled water, uniformly stirring, adding 2g of polyvinylpyrrolidone, stirring for 30min, adding a sodium hydroxide solution with the concentration of 0.1mol/L to adjust the pH value to 11, stirring at constant temperature for 30min to obtain a precursor solution, transferring the precursor solution into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 3h, centrifuging after the reaction is finished, washing the precipitate, and drying in a drying oven at 75 ℃ to constant weight to obtain the doped nano zinc oxide;
step A2, dispersing 10g of doped nano zinc oxide in 120mL of ethanol solution with the mass fraction of 50%, then adding 0.5g of coupling agent KH-590, magnetically stirring and reacting for 8 hours, centrifuging, washing and drying the precipitate after the reaction is finished to obtain an intermediate product; under the protection of nitrogen, adding 10g of intermediate product and 1.6g of 4-vinylaniline into 120mL of toluene, stirring at the rotating speed of 80r/min for 5min, heating to 40 ℃, adding 0.4g of triethylamine, carrying out reflux reaction for 50min, cooling to room temperature, filtering, and distilling a filter cake to remove a solvent to obtain aniline grafted nano zinc oxide;
step A3, dispersing 5g of aniline grafted nano zinc oxide in 40mL of deionized water by ultrasonic, then adding an ethanol solution of p-aminobenzoic acid, dropwise adding an ammonium persulfate solution at room temperature, stirring at 50 ℃ for reaction for 6 hours after the dropwise adding is finished, carrying out suction filtration after the reaction is finished, and drying a filter cake at 60 ℃ to constant weight to obtain modified zinc oxide particles, wherein the ethanol solution of p-aminobenzoic acid is prepared from 2.4g of p-aminobenzoic acid and ethanol: 6mL of the mixture is mixed, and the ammonium persulfate solution is prepared from ammonium persulfate, deionized water and 10% acetic acid solution according to the mass fraction of 0.4g:50mL:2mL of the mixture.
Comparative example 1
The invention provides modified zinc oxide particles, which are prepared by the following steps:
and A1, adding 100g of zinc nitrate and 2.1g of gallium nitrate into 200mL of distilled water, uniformly stirring, adding 2g of polyvinylpyrrolidone, stirring for 30min, adding a sodium hydroxide solution with the concentration of 0.1mol/L to adjust the pH value to 11, stirring at constant temperature for 30min to obtain a precursor solution, transferring the precursor solution into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 3h, centrifuging after the reaction is finished, washing the precipitate, and drying in a drying oven at 75 ℃ to constant weight to obtain modified zinc oxide particles.
Comparative example 2
The invention provides modified zinc oxide particles, which are prepared by the following steps:
step A1, adding 100g of zinc nitrate and 1.9g of gallium nitrate into 200mL of distilled water, stirring uniformly, adding 1.5g of polyvinylpyrrolidone, stirring for 20min, adding a sodium hydroxide solution with the concentration of 0.1mol/L to adjust the pH value to 10, stirring at constant temperature for 30min to obtain a precursor solution, transferring the precursor solution into a hydrothermal reaction kettle, performing hydrothermal reaction at 160 ℃ for 3h, centrifuging after the reaction is finished, washing the precipitate, and drying in a drying oven at 75 ℃ until the weight is constant to obtain the doped nano zinc oxide;
and A2, dispersing 10g of doped nano zinc oxide in 100mL of ethanol solution with the mass fraction of 50%, adding 0.3g of coupling agent KH-560, magnetically stirring and reacting for 6h, centrifuging after the reaction is finished, washing and drying the precipitate to obtain modified zinc oxide particles.
Example 4
The preparation method of the antistatic PET material comprises the following steps:
firstly, preparing the following raw materials in percentage by mass: 0.3% of antioxidant 1010, 0.05% of sodium carboxylate, 0.05% of lubricant, 2% of modified zinc oxide particles of example 1, 0.3% of quaternary ammonium salt compound and the balance of PET resin;
and secondly, adding the PET resin, the antioxidant, the lubricant, the nucleating agent, the modified zinc oxide particles and the quaternary ammonium salt compound into a high-speed mixer, uniformly mixing, and transferring into a double-screw extruder for melt extrusion granulation to obtain the antistatic PET material, wherein the temperature of each section of a machine barrel of the double-screw extruder is respectively one zone 245 ℃, two zones 255 ℃, three zones 260 ℃ and four zones 250 ℃.
Wherein the quaternary ammonium salt compound is prepared by the following steps:
step B1, adding 6g of triethanolamine and 7.65g of 9H-carbazole-2, 7-dicarboxylic acid into a three-neck flask, heating to 100 ℃, stirring for 20min, adding 0.05g of p-toluenesulfonic acid, heating to 130 ℃, stirring and reacting for 2.5h, and obtaining an intermediate product 1 after the reaction is finished;
and B2, placing 10g of the intermediate product 1 into 150mL of DMF, adding 4.6g of sodium chloroacetate, stirring at 80 ℃ for reaction for 7h, and removing DMF by reduced pressure distillation after the reaction is finished to obtain the quaternary ammonium salt compound.
The lubricant is formed by mixing pentaerythritol stearate and silicone powder according to a mass ratio of 1:4.
Example 5
The preparation method of the antistatic PET material comprises the following steps:
firstly, preparing the following raw materials in percentage by mass: antioxidant 1076.0%, lubricant 0.2%, nucleating agent 0.5%, modified zinc oxide particles 2% of example 2, quaternary ammonium salt compound 0.1% and PET resin in balance;
and secondly, adding the PET resin, the antioxidant, the lubricant, the nucleating agent, the modified zinc oxide particles and the quaternary ammonium salt compound into a high-speed mixer, uniformly mixing, and transferring into a double-screw extruder for melt extrusion granulation to obtain the antistatic PET material, wherein the temperature of each section of a machine barrel of the double-screw extruder is respectively one zone 245 ℃, two zones 255 ℃, three zones 260 ℃ and four zones 250 ℃.
Wherein the quaternary ammonium salt compound is prepared by the following steps:
step B1, adding 6g of triethanolamine and 8.18g of 9H-carbazole-2, 7-dicarboxylic acid into a three-neck flask, heating to 100 ℃, stirring for 22min, adding 0.06g of p-toluenesulfonic acid, heating to 130 ℃, stirring and reacting for 2.8h, and obtaining an intermediate product 1 after the reaction is finished;
and B2, placing 10g of the intermediate product 1 into 180mL of DMF, adding 4.9g of sodium chloroacetate, stirring at 80 ℃ for reaction for 7h, and removing DMF by reduced pressure distillation after the reaction is finished to obtain the quaternary ammonium salt compound.
Wherein the nucleating agent is talcum powder with the particle size of 0.8 mu m, and the lubricant is pentaerythritol stearate and silicone powder which are mixed according to the mass ratio of 2:6.
Example 6
The preparation method of the antistatic PET material comprises the following steps:
firstly, preparing the following raw materials in percentage by mass: 2.0% of antioxidant B215, 0.5% of lubricant, 1% of nucleating agent, 2% of modified zinc oxide particles of example 3, 0.5% of quaternary ammonium salt compound and the balance of PET resin;
and secondly, adding the PET resin, the antioxidant, the lubricant, the nucleating agent, the modified zinc oxide particles and the quaternary ammonium salt compound into a high-speed mixer, uniformly mixing, and transferring into a double-screw extruder for melt extrusion granulation to obtain the antistatic PET material, wherein the temperature of each section of a machine barrel of the double-screw extruder is respectively one zone 245 ℃, two zones 255 ℃, three zones 260 ℃ and four zones 250 ℃.
Wherein the quaternary ammonium salt compound is prepared by the following steps:
step B1, adding 6g of triethanolamine and 9.18g of 9H-carbazole-2, 7-dicarboxylic acid into a three-neck flask, heating to 100 ℃, stirring for 25min, adding 0.07g of p-toluenesulfonic acid, heating to 130 ℃, stirring and reacting for 3h, and obtaining an intermediate product 1 after the reaction is finished;
and B2, placing 10g of the intermediate product 1 into 200mL of DMF, adding 5.1g of sodium chloroacetate, stirring at 80 ℃ for reaction for 7h, and removing DMF by reduced pressure distillation after the reaction is finished to obtain the quaternary ammonium salt compound.
Wherein the nucleating agent is talcum powder with the particle size of 0.5-1.4 mu m, and the lubricant is pentaerythritol stearate and silicone powder which are mixed according to the mass ratio of 3:7.
Comparative example 3
The modified zinc oxide particles in example 4 were replaced with those in comparative example 1, and the other raw materials and the production process were the same as in example 4.
Comparative example 4
The modified zinc oxide particles in example 5 were replaced with the ones in comparative example 2, and the other raw materials and the production process were the same as in example 5.
Comparative example 5
The quaternary ammonium salt compound of example 6 was replaced with a polyquaternium M550 surfactant sold by Jinan Maifeng chemical Co., ltd. And the rest of the raw materials and the preparation process were the same as those of example 6.
The materials obtained in examples 4 to 6 and comparative examples 3 to 5 were passed through a platen press to prepare a PET plate having a thickness of 2mm, a sample of 5.5 cm. Times.5.5 cm was cut out, and the PET plate was tested for resistivity by a high insulation resistance measuring instrument, and the test results are shown in Table 1:
TABLE 1
As can be seen from Table 1, the PET materials obtained in examples 4-6 have lower surface resistivity than the PET composite materials obtained in comparative examples 3-5, and it can be seen from examples 4-5 and comparative examples 3-4 that the presence of the polyaniline layer doped with nano zinc oxide surface can exert a certain antistatic effect, and that the quaternary ammonium salt compound prepared in the present invention is more advantageous for increasing the antistatic property of PET as shown in examples 6 and comparative example 5.
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 invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (6)
1. The preparation method of the antistatic PET material is characterized by comprising the following steps of:
firstly, dispersing aniline grafted nano zinc oxide in deionized water by ultrasonic, adding an ethanol solution of p-aminobenzoic acid, dropwise adding an ammonium persulfate solution at room temperature, stirring at 50 ℃ for reaction for 4-6 hours, carrying out suction filtration, and drying a filter cake to obtain modified zinc oxide particles;
secondly, preparing the following raw materials in percentage by mass: 0.3 to 2.0 percent of antioxidant, 0.05 to 0.5 percent of lubricant, 0.1 to 1 percent of nucleating agent, 2 percent of modified zinc oxide particles, 0.3 to 0.5 percent of quaternary ammonium salt compound and the balance of PET resin;
thirdly, mixing all the raw materials in the second step, and then carrying out melt extrusion granulation to obtain an antistatic PET material;
the aniline grafted nano zinc oxide is prepared by the following steps:
dispersing doped nano zinc oxide in ethanol solution with the mass fraction of 50%, adding KH-590, magnetically stirring for reaction for 6-8h, and performing post-treatment to obtain an intermediate product; adding an intermediate product and 4-vinylaniline into toluene under the protection of nitrogen, stirring, heating to 40 ℃, adding triethylamine, carrying out reflux reaction for 50min, and carrying out aftertreatment to obtain aniline grafted nano zinc oxide;
the quaternary ammonium salt compound is prepared by the following steps:
step B1, mixing triethanolamine and 9H-carbazole-2, 7-dicarboxylic acid, stirring for 20-25min at 100 ℃, adding p-toluenesulfonic acid, heating to 130 ℃, and stirring for 2.5-3H to obtain an intermediate product 1;
and B2, placing the intermediate product 1 in DMF, adding sodium chloroacetate, stirring at 80 ℃ for reaction for 7 hours, and distilling under reduced pressure to remove DMF to obtain the quaternary ammonium salt compound.
2. The method for preparing the antistatic PET material according to claim 1, wherein the ethanol solution of the para-aminobenzoic acid comprises 2.4g of para-aminobenzoic acid and ethanol according to the dosage ratio: 6mL of ammonium persulfate solution is prepared by mixing ammonium persulfate, deionized water and 10% mass fraction acetic acid solution according to the dosage ratio of 0.4g:50mL:2mL of the mixture.
3. The method for preparing an antistatic PET material according to claim 1, wherein the doped nano zinc oxide is prepared by the steps of:
adding zinc nitrate and gallium nitrate into distilled water, stirring, adding polyvinylpyrrolidone, regulating the pH value to 10-11, stirring, transferring into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 3h, and carrying out aftertreatment to obtain the doped nano zinc oxide.
4. The method for preparing an antistatic PET material according to claim 3, wherein the dosage ratio of zinc nitrate, gallium nitrate, distilled water and polyvinylpyrrolidone is 100g:1.8-2.1g:200mL:1-2g.
5. The method for preparing an antistatic PET material according to claim 1, wherein the dosage ratio of triethanolamine, 9H-carbazole-2, 7-dicarboxylic acid and p-toluenesulfonic acid in step B1 is 6g:7.65-9.18g:0.05-0.07g.
6. The method for preparing an antistatic PET material according to claim 1, wherein the ratio of the amount of intermediate 1, DMF and sodium chloroacetate in step B2 is 10g:150-200mL:4.6-5.1g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210315528.2A CN114539738B (en) | 2022-03-28 | 2022-03-28 | Preparation method of antistatic PET material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210315528.2A CN114539738B (en) | 2022-03-28 | 2022-03-28 | Preparation method of antistatic PET material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114539738A CN114539738A (en) | 2022-05-27 |
| CN114539738B true CN114539738B (en) | 2023-09-05 |
Family
ID=81665503
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210315528.2A Active CN114539738B (en) | 2022-03-28 | 2022-03-28 | Preparation method of antistatic PET material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114539738B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115323617B (en) * | 2022-09-13 | 2023-07-14 | 吉祥三宝高科纺织有限公司 | Production method of home textile flocculus with peculiar smell eliminating effect |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104693694A (en) * | 2013-12-05 | 2015-06-10 | 上海杰事杰新材料(集团)股份有限公司 | Antistatic-improved polyethylene terephthalate composite material and preparation method thereof |
| CN105967594A (en) * | 2016-05-09 | 2016-09-28 | 陈毅忠 | Preparation method of modified graphene-polymer-cement waterproof coating |
| CN106280317A (en) * | 2016-08-22 | 2017-01-04 | 绍兴协众进出口有限公司 | A kind of antibacterial PET Masterbatch |
| CN108102364A (en) * | 2017-12-20 | 2018-06-01 | 合肥工业大学 | A kind of preparation method of the hud typed nickel/polyaniline compound wave-absorbing material of nanometer of chain |
| CN111892806A (en) * | 2018-05-12 | 2020-11-06 | 湖南辰砾新材料有限公司 | Preparation method of composite efficient antistatic agent for plastics |
| CN112575584A (en) * | 2020-11-19 | 2021-03-30 | 深圳市兴业卓辉实业有限公司 | Antistatic solution, preparation method and use method |
| CN113308047A (en) * | 2021-05-31 | 2021-08-27 | 常州优洁包装材料有限公司 | Impact-resistant antistatic sealing barrel and preparation method thereof |
| CN113699788A (en) * | 2021-09-06 | 2021-11-26 | 江阴市宏勇医疗科技发展有限公司 | Antistatic alcohol-resistant plasma-resistant medical non-woven fabric |
| CN114044932A (en) * | 2021-12-08 | 2022-02-15 | 江苏普清净化科技有限公司 | Anti-static polymer film rolling material and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108969537B (en) * | 2018-08-09 | 2020-11-17 | 陕西科技大学 | Preparation method of ZnO/GQD-PEI composite quantum dot antibacterial agent |
-
2022
- 2022-03-28 CN CN202210315528.2A patent/CN114539738B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104693694A (en) * | 2013-12-05 | 2015-06-10 | 上海杰事杰新材料(集团)股份有限公司 | Antistatic-improved polyethylene terephthalate composite material and preparation method thereof |
| CN105967594A (en) * | 2016-05-09 | 2016-09-28 | 陈毅忠 | Preparation method of modified graphene-polymer-cement waterproof coating |
| CN106280317A (en) * | 2016-08-22 | 2017-01-04 | 绍兴协众进出口有限公司 | A kind of antibacterial PET Masterbatch |
| CN108102364A (en) * | 2017-12-20 | 2018-06-01 | 合肥工业大学 | A kind of preparation method of the hud typed nickel/polyaniline compound wave-absorbing material of nanometer of chain |
| CN111892806A (en) * | 2018-05-12 | 2020-11-06 | 湖南辰砾新材料有限公司 | Preparation method of composite efficient antistatic agent for plastics |
| CN112575584A (en) * | 2020-11-19 | 2021-03-30 | 深圳市兴业卓辉实业有限公司 | Antistatic solution, preparation method and use method |
| CN113308047A (en) * | 2021-05-31 | 2021-08-27 | 常州优洁包装材料有限公司 | Impact-resistant antistatic sealing barrel and preparation method thereof |
| CN113699788A (en) * | 2021-09-06 | 2021-11-26 | 江阴市宏勇医疗科技发展有限公司 | Antistatic alcohol-resistant plasma-resistant medical non-woven fabric |
| CN114044932A (en) * | 2021-12-08 | 2022-02-15 | 江苏普清净化科技有限公司 | Anti-static polymer film rolling material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 水热法制备ZnO抗静电导电粉研究;刘雪佳等;《化工新型材料》;第第46卷卷(第第9期期);第253-255页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114539738A (en) | 2022-05-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114539738B (en) | Preparation method of antistatic PET material | |
| CN109778335B (en) | Modified polypropylene fiber and preparation method thereof | |
| CN108164751B (en) | Reactive halogen-free flame retardant suitable for TPV (thermoplastic vulcanizate), and preparation method and application thereof | |
| CN112590346B (en) | Antibacterial high-barrier co-extrusion composite film and preparation method thereof | |
| CN114891451B (en) | Compound thermoplastic polymer TPO waterproofing membrane | |
| CN113292688A (en) | Preparation method of composite antibacterial agent and antibacterial plastic | |
| CN113861688B (en) | Low-dielectric polyphenylene sulfide composite material and preparation method thereof | |
| CN110615915A (en) | Composite polypropylene nucleating agent and preparation method and application thereof | |
| CN109206677B (en) | Hyperbranched polymer modified carbon black surface and application thereof in rubber processing | |
| CN109776830A (en) | A kind of polyurethane/carboxymethyl chitosan/PAn conducting membrane preparation method | |
| CN112280260A (en) | High-barrier PLA/PBAT composite packaging film | |
| CN112063147A (en) | Two-dimensional organic metal framework MOF modified PC material | |
| CN112011039B (en) | Water-soluble polymer modifier with polyester structure for calcium carbonate surface modification and preparation method thereof | |
| CN114437447A (en) | Degradable composite foam material with high mechanical property and preparation method thereof | |
| CN113831638A (en) | Anti-aging BOPP film and preparation method and application thereof | |
| CN112266492A (en) | Preparation method of hydrophobic film with low water absorption | |
| CN108440693B (en) | High-melt-index resin and preparation method thereof | |
| CN114736408B (en) | Preparation method of high-dielectric PI/PVDF composite film | |
| CN111844984B (en) | Three-layer co-extrusion stretched high-temperature-resistant tear-resistant composite film and preparation method thereof | |
| CN113337131B (en) | High-strength and anti-ultraviolet soybean protein film and preparation method and application thereof | |
| CN113583228B (en) | Synthesis method of polyester chip for high-temperature-resistant film | |
| CN116144102B (en) | High-toughness polypropylene material and preparation method thereof | |
| CN115637030B (en) | Polyketone-containing composition and application thereof in preparation of polymer composite material | |
| CN111285946B (en) | Antibacterial and antistatic additive for migrating PE and preparation method thereof | |
| CN114075327B (en) | Intelligent response polyester, fiber and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |