CN111471238A - Preparation method of polypropylene electret master batch - Google Patents

Preparation method of polypropylene electret master batch Download PDF

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CN111471238A
CN111471238A CN202010406069.XA CN202010406069A CN111471238A CN 111471238 A CN111471238 A CN 111471238A CN 202010406069 A CN202010406069 A CN 202010406069A CN 111471238 A CN111471238 A CN 111471238A
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polypropylene
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dispersant
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陆家浩
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Wuxi Deyu New Material Co ltd
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10—Homopolymers or copolymers of propene
    • C08J2323/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/10—Homopolymers or copolymers of propene
    • C08J2423/12—Polypropene
    • 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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • 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
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • 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
    • C08K3/38—Boron-containing 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/13—Phenols; Phenolates
    • C08K5/134—Phenols containing ester groups
    • C08K5/1345—Carboxylic esters of phenolcarboxylic acids
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract

The invention belongs to the field of high polymer materials, and particularly relates to a preparation method of polypropylene electret master batches, which comprises, by mass, 80-100 parts of polypropylene, 15-20 parts of tourmaline powder, 5-10 parts of aluminum hydroxide, 5-8 parts of graphene, 3-5 parts of a dispersing agent, 3-5 parts of an antioxidant and 1-2 parts of a coupling agent. The invention solves the problem of poor filtering efficiency in the prior art, and utilizes the anion characteristic of tourmaline powder and the oxygen storage property of activated alumina to form good negative oxygen ions, thereby greatly improving the filtering efficiency.

Description

Preparation method of polypropylene electret master batch
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a preparation method of a polypropylene electret master batch.
Background
Researches show that particles caused by pollution in the air, particularly particles with aerodynamic equivalent of less than or equal to 2.5 microns, have small particle size and are rich in toxic and harmful substances. The particles can stay in the air for a long time and are easily absorbed by people to enter the body, thereby causing diseases such as respiratory system diseases, lung injury, carcinogenesis, cardiovascular diseases, reproductive system, fetal development and the like. The polypropylene melt fiber produced by the melt-blown technology is fine, and the obtained melt-blown fabric has large specific surface area, small pores and large porosity, so the application characteristics of filterability, shielding property, heat insulation property, oil absorption property and the like are difficult to realize by non-woven fabrics produced by other processes. Generally, polypropylene melt-blown fabrics are widely used in the fields of filter materials, medical and health materials, oil absorbing materials, wiping cloths, thermal materials, battery separator materials, sound insulating materials, and the like. Therefore, the polypropylene melt-blown fabric is widely applied to the air purification and medical health industries, such as air conditioner filter screens, medical protective masks, dust masks and the like. However, the prior art directly performs electret treatment on the melt-blown polypropylene material, and has the defects of low filtration efficiency, large resistance and the like of melt-blown polypropylene fibers after the electret treatment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a polypropylene electret master batch, which solves the problem of poor filtering efficiency in the prior art, and utilizes the anion characteristic of tourmaline powder and the oxygen storage property of activated alumina to form good negative oxygen ions, thereby greatly improving the filtering efficiency.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of polypropylene electret master batch comprises the following mass formula:
80-100 parts of polypropylene, 15-20 parts of tourmaline powder, 5-10 parts of aluminum hydroxide, 5-8 parts of graphene, 3-5 parts of a dispersant, 3-5 parts of an antioxidant and 1-2 parts of a coupling agent.
The polypropylene is homopolymerized polypropylene, and the polypropylene is high-melt-index polypropylene with the melt index range of 1000-1400g/10 min.
The particle size of the tourmaline powder is 20-50 μm.
The aperture of the aluminum hydroxide is 3-7 μm.
The particle size of the graphene is 1-4 μm.
The dispersant adopts ethyl cellulose.
The antioxidant adopts pentaerythritol tetrakis [ β - (3 ', 5 ' -di-tert-butyl-4 ' -hydroxyphenyl) propionate ].
The coupling agent adopts isopropyl titanate.
The preparation method comprises the following steps:
step 1, uniformly stirring graphene and aluminum hydroxide, adding tourmaline powder, and continuously stirring to form uniformly mixed solid powder; the stirring speed is 1000-2000 r/min;
step 2, adding isopropyl titanate and a dispersant into absolute ethyl alcohol, and uniformly stirring to form a dispersion solution; the mass of the absolute ethyl alcohol is 10-20 times of that of the dispersant, and the stirring speed is 1000-1500 r/min;
step 3, slowly adding the solid powder into the dispersion solution, performing ultrasonic dispersion for 20-40min to obtain a solution, and then performing reduced pressure distillation for 20-40min to obtain viscous slurry; the slow adding speed is 2-4g/min, the ultrasonic frequency of ultrasonic dispersion is 40-80kHz, the temperature of reduced pressure distillation is 70-80 ℃, and the pressure is 80-90% of the atmospheric pressure;
and 4, uniformly mixing the viscous slurry, the antioxidant and the polypropylene, then performing melt extrusion through a double-screw mixing extruder, cooling through a water bath, and cutting to obtain the master batch.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of poor filtering efficiency in the prior art, and utilizes the anion characteristic of tourmaline powder and the oxygen storage property of activated alumina to form good negative oxygen ions, thereby greatly improving the filtering efficiency.
2. The invention utilizes the temperature of the molten state to convert aluminum hydroxide into activated aluminum oxide, achieves good activation treatment and forms a micropore oxygen storage system.
3. The graphene solves the problem of insulativity of aluminum oxide, and quickly transfers negative ions of tourmaline powder to form a stable physical adsorption-negative oxygen ion adsorption combined composite adsorption system.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of polypropylene electret master batch comprises the following mass formula:
80 parts of polypropylene, 15 parts of tourmaline powder, 5 parts of aluminum hydroxide, 5 parts of graphene, 3 parts of a dispersing agent, 3 parts of an antioxidant and 1 part of a coupling agent.
The polypropylene is homopolymerized polypropylene, and the polypropylene is high-melt-index polypropylene with a melt index range of 1000g/10 min.
The particle size of the tourmaline powder is 20 μm.
The pore diameter of the aluminum hydroxide is 3 μm.
The particle size of the graphene is 1 μm.
The dispersant adopts ethyl cellulose.
The antioxidant adopts pentaerythritol tetrakis [ β - (3 ', 5 ' -di-tert-butyl-4 ' -hydroxyphenyl) propionate ].
The coupling agent adopts isopropyl titanate.
The preparation method comprises the following steps:
step 1, uniformly stirring graphene and aluminum hydroxide, adding tourmaline powder, and continuously stirring to form uniformly mixed solid powder; the stirring speed is 1000 r/min;
step 2, adding isopropyl titanate and a dispersant into absolute ethyl alcohol, and uniformly stirring to form a dispersion solution; the mass of the absolute ethyl alcohol is 10 times of that of the dispersant, and the stirring speed is 1000 r/min;
step 3, slowly adding the solid powder into the dispersion solution, performing ultrasonic dispersion for 20min to obtain a solution, and then performing reduced pressure distillation for 20min to obtain viscous slurry; the slow adding speed is 2g/min, the ultrasonic frequency of ultrasonic dispersion is 40kHz, the temperature of reduced pressure distillation is 70 ℃, and the pressure is 80% of the atmospheric pressure;
and 4, uniformly mixing the viscous slurry, the antioxidant and the polypropylene, then performing melt extrusion through a double-screw mixing extruder, cooling through a water bath, and cutting to obtain the master batch.
Example 2
A preparation method of polypropylene electret master batch comprises the following mass formula:
100 parts of polypropylene, 20 parts of tourmaline powder, 10 parts of aluminum hydroxide, 8 parts of graphene, 5 parts of a dispersing agent, 5 parts of an antioxidant and 2 parts of a coupling agent.
The polypropylene is homopolymerized polypropylene, and the polypropylene is high-melt-index polypropylene with a melt index range of 1400g/10 min.
The particle size of the tourmaline powder is 50 μm.
The pore diameter of the aluminum hydroxide is 7 μm.
The particle size of the graphene is 4 μm.
The dispersant adopts ethyl cellulose.
The antioxidant adopts pentaerythritol tetrakis [ β - (3 ', 5 ' -di-tert-butyl-4 ' -hydroxyphenyl) propionate ].
The coupling agent adopts isopropyl titanate.
The preparation method comprises the following steps:
step 1, uniformly stirring graphene and aluminum hydroxide, adding tourmaline powder, and continuously stirring to form uniformly mixed solid powder; the stirring speed is 2000 r/min;
step 2, adding isopropyl titanate and a dispersant into absolute ethyl alcohol, and uniformly stirring to form a dispersion solution; the mass of the absolute ethyl alcohol is 20 times of that of the dispersant, and the stirring speed is 1500 r/min;
step 3, slowly adding the solid powder into the dispersion solution, performing ultrasonic dispersion for 40min to obtain a solution, and then performing reduced pressure distillation for 40min to obtain viscous slurry; the slow adding speed is 4g/min, the ultrasonic frequency of ultrasonic dispersion is 80kHz, the temperature of reduced pressure distillation is 80 ℃, and the pressure is 90% of the atmospheric pressure;
and 4, uniformly mixing the viscous slurry, the antioxidant and the polypropylene, then performing melt extrusion through a double-screw mixing extruder, cooling through a water bath, and cutting to obtain the master batch.
Example 3
A preparation method of polypropylene electret master batch comprises the following mass formula:
90 parts of polypropylene, 18 parts of tourmaline powder, 7 parts of aluminum hydroxide, 8 parts of graphene, 4 parts of a dispersing agent, 4 parts of an antioxidant and 2 parts of a coupling agent.
The polypropylene is homopolymerized polypropylene, and the polypropylene is high-melt-index polypropylene with the melt index range of 1300g/10 min.
The particle size of the tourmaline powder is 40 μm.
The pore diameter of the aluminum hydroxide is 5 μm.
The particle size of the graphene is 3 μm.
The dispersant adopts ethyl cellulose.
The antioxidant adopts pentaerythritol tetrakis [ β - (3 ', 5 ' -di-tert-butyl-4 ' -hydroxyphenyl) propionate ].
The coupling agent adopts isopropyl titanate.
The preparation method comprises the following steps:
step 1, uniformly stirring graphene and aluminum hydroxide, adding tourmaline powder, and continuously stirring to form uniformly mixed solid powder; the stirring speed is 1500 r/min;
step 2, adding isopropyl titanate and a dispersant into absolute ethyl alcohol, and uniformly stirring to form a dispersion solution; the mass of the absolute ethyl alcohol is 15 times of that of the dispersant, and the stirring speed is 1200 r/min;
step 3, slowly adding the solid powder into the dispersion solution, performing ultrasonic dispersion for 30min to obtain a solution, and then performing reduced pressure distillation for 30min to obtain viscous slurry; the slow adding speed is 3g/min, the ultrasonic frequency of ultrasonic dispersion is 60kHz, the temperature of reduced pressure distillation is 75 ℃, and the pressure is 85% of the atmospheric pressure;
and 4, uniformly mixing the viscous slurry, the antioxidant and the polypropylene, then performing melt extrusion through a double-screw mixing extruder, cooling through a water bath, and cutting to obtain the master batch.
The master batches of examples 1-3 were mixed with a polypropylene material at a ratio of 1:10 and sprayed through a spinneret to form fibers, which were processed to obtain a melt-blown nonwoven material.
The medium adopts NaCl particles with the number median diameter of 0.075 +/-0.02 mu m, the test flow rate is 85L/min, the filtration efficiency is carried out, and the escherichia coli is taken as a strain for antibacterial detection.
Comparative example a melt blown nonwoven material was prepared as described above using commercially available polypropylene masterbatch.
Figure BDA0002491332800000051
In summary, the invention has the following advantages:
1. the invention solves the problem of poor filtering efficiency in the prior art, and utilizes the anion characteristic of tourmaline powder and the oxygen storage property of activated alumina to form good negative oxygen ions, thereby greatly improving the filtering efficiency.
2. The invention utilizes the temperature of the molten state to convert aluminum hydroxide into activated aluminum oxide, achieves good activation treatment and forms a micropore oxygen storage system.
3. The graphene solves the problem of insulativity of aluminum oxide, and quickly transfers negative ions of tourmaline powder to form a stable physical adsorption-negative oxygen ion adsorption combined composite adsorption system.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.

Claims (9)

1. A preparation method of polypropylene electret master batch is characterized by comprising the following steps: the mass formula is as follows:
80-100 parts of polypropylene, 15-20 parts of tourmaline powder, 5-10 parts of aluminum hydroxide, 5-8 parts of graphene, 3-5 parts of a dispersant, 3-5 parts of an antioxidant and 1-2 parts of a coupling agent.
2. The method for preparing a polypropylene electret masterbatch according to claim 1, wherein: the polypropylene is homopolymerized polypropylene, and the polypropylene is high-melt-index polypropylene with the melt index range of 1000-1400g/10 min.
3. The method for preparing a polypropylene electret masterbatch according to claim 1, wherein: the particle size of the tourmaline powder is 20-50 μm.
4. The method for preparing a polypropylene electret masterbatch according to claim 1, wherein: the aperture of the aluminum hydroxide is 3-7 μm.
5. The method for preparing a polypropylene electret masterbatch according to claim 1, wherein: the particle size of the graphene is 1-4 μm.
6. The method for preparing a polypropylene electret masterbatch according to claim 1, wherein: the dispersant adopts ethyl cellulose.
7. The method for preparing polypropylene electret masterbatch according to claim 1, wherein the antioxidant is pentaerythritol tetrakis [ β - (3 ', 5 ' -di-tert-butyl-4 ' -hydroxyphenyl) propionate ].
8. The method for preparing a polypropylene electret masterbatch according to claim 1, wherein: the coupling agent adopts isopropyl titanate.
9. The method for preparing a polypropylene electret masterbatch according to claim 1, wherein: the preparation method comprises the following steps:
step 1, uniformly stirring graphene and aluminum hydroxide, adding tourmaline powder, and continuously stirring to form uniformly mixed solid powder; the stirring speed is 1000-2000 r/min;
step 2, adding isopropyl titanate and a dispersant into absolute ethyl alcohol, and uniformly stirring to form a dispersion solution; the mass of the absolute ethyl alcohol is 10-20 times of that of the dispersant, and the stirring speed is 1000-1500 r/min;
step 3, slowly adding the solid powder into the dispersion solution, performing ultrasonic dispersion for 20-40min to obtain a solution, and then performing reduced pressure distillation for 20-40min to obtain viscous slurry; the slow adding speed is 2-4g/min, the ultrasonic frequency of ultrasonic dispersion is 40-80kHz, the temperature of reduced pressure distillation is 70-80 ℃, and the pressure is 80-90% of the atmospheric pressure;
and 4, uniformly mixing the viscous slurry, the antioxidant and the polypropylene, then performing melt extrusion through a double-screw mixing extruder, cooling through a water bath, and cutting to obtain the master batch.
CN202010406069.XA 2020-05-14 2020-05-14 Preparation method of polypropylene electret master batch Pending CN111471238A (en)

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CN111957109A (en) * 2020-08-18 2020-11-20 绍兴市梓昂新材料有限公司 Efficient organic-inorganic composite filter material
CN112430337A (en) * 2020-11-17 2021-03-02 黑龙江康禄新材料科技有限公司 Electret master batch capable of naturally releasing negative oxygen ions, application and process
CN112941719A (en) * 2021-01-29 2021-06-11 江苏盛纺纳米材料科技股份有限公司 Hot air non-woven fabric special for electrostatic cotton mask and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111957109A (en) * 2020-08-18 2020-11-20 绍兴市梓昂新材料有限公司 Efficient organic-inorganic composite filter material
CN112430337A (en) * 2020-11-17 2021-03-02 黑龙江康禄新材料科技有限公司 Electret master batch capable of naturally releasing negative oxygen ions, application and process
CN112941719A (en) * 2021-01-29 2021-06-11 江苏盛纺纳米材料科技股份有限公司 Hot air non-woven fabric special for electrostatic cotton mask and preparation method thereof

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Application publication date: 20200731