CN111647213A - Preparation method of monodisperse antistatic polyethylene micropowder - Google Patents
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- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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- 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
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- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
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- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
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Abstract
A preparation method of monodisperse antistatic polyethylene micropowder comprises the following technical steps. (1) Low-temperature nitrogen-filled ball milling, (2) compound solvent preparation, (3) resonance sound mixing and dissolving, (4) colloid mill grinding treatment, (5) ultrasonic wave and microwave synergistic treatment and (6) freeze drying. The polyethylene micropowder obtained by the invention has the characteristics of monodispersity and narrow particle size distribution.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and relates to a preparation method of monodisperse antistatic polyethylene micro powder.
Background
Polyethylene is a thermoplastic resin obtained by polymerizing ethylene. Polyethylene is insoluble in common solvents at normal temperature, has small water absorption and excellent electrical insulation; and the thermoplastic plastic is light in weight, non-toxic and good in comprehensive performance, and has wide application.
The micro powder product obtained by ultra-fining the polyethylene has important use value. The polyethylene micro powder has multiple use functions, can be used as a non-polar low-shrinkage additive, and is a particularly effective basic additive; can be used as the hot-melt adhesive of the anode ring of the alkaline battery; the physical properties of paint, pigment and printing ink can be modified, so that the smoothness and glossiness of the paint can be reduced, and the friction resistance can be improved when the pigment is added into the printing ink; the modified epoxy resin can be used for improving the performance of casting-grade epoxy resin, polystyrene, ABS, phenolic resin and PVC resin; and so on.
At present, the method for preparing the polyethylene micropowder mainly comprises a physical method and a chemical method. Physical methods include mechanical pulverization methods, evaporation-condensation methods, and melting methods. The physical method for preparing the polyethylene micropowder does not need a solvent, has the advantage of environmental protection, but has more defects. The disadvantages of the mechanical crushing method are: impurities are easy to be mixed and violent oxidation occurs, the shape is irregular, the particle size is large, the distribution is wide, and powder below the micron level is difficult to obtain. The disadvantages of the evaporation-condensation process are: the process is complex, the requirement on conditions is high, and the method is not suitable for large-scale production. The disadvantages of the melt process are: the particle size has high requirement on the precision of equipment, the particle size distribution is wide, and fibrous products are easily formed. The chemical method is the main method for preparing the polyolefin resin micro powder in laboratories and industries at present, and has the advantages of controllable reaction, uniform particle size distribution of products, regular shape and the like, but the polyolefin resin micro powder prepared by the chemical method has the defects of easy agglomeration, high static electricity and the like.
Disclosure of Invention
The invention aims to provide a preparation method of monodisperse antistatic polyethylene micropowder.
In order to achieve the above objects and other related objects, the present invention provides the following technical solutions: a preparation method of monodisperse antistatic polyethylene micropowder comprises the following steps:
step 1: under the condition that the temperature is 0-10 ℃ and under the protection of nitrogen, grinding the polyethylene raw material to 100-150 meshes to obtain polyethylene powder;
step 2: uniformly mixing 50-70 parts by weight of main solvent, 15-25 parts by weight of solubilizer, 0.5-5.0 parts by weight of dispersant and 0.5-5.0 parts by weight of antistatic agent to obtain a composite solvent; the main solvent is at least one of monochlorotoluene, dichlorotoluene and trichlorotoluene; the solubilizer is at least one of propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol butyl ether, ethylene glycol ethyl ether and ethylene glycol butyl ether; the dispersing agent is at least one of hydroxypropyl methyl cellulose, hydroxymethyl cellulose and hydroxyethyl cellulose; the antistatic agent is at least one of polyaniline, polypyrrole and polythiophene;
and step 3: mixing polyethylene powder and a composite solvent according to a mass ratio of 10-35:100, placing into a resonance sound mixing device, and treating for 15-30min under the conditions of frequency of 80-150Hz and amplitude of 1.0-2.0mm to obtain a mixed solution;
and 4, step 4: under the protection of nitrogen, grinding the mixed solution to the fineness of 10-50 μm to obtain a refined mixed solution;
and 5: simultaneously carrying out ultrasonic treatment and microwave treatment on the refined mixed solution, wherein the ultrasonic treatment conditions comprise ultrasonic frequency of 25-35KHz and power density of 0.25-0.50W/cm2The microwave treatment conditions include 2450MHz frequency and 0.2-2.0w/cm radiation intensity2The treatment time is 10-20 min;
step 6: and (5) freeze-drying the material obtained in the step (5) to obtain the material, namely the monodisperse antistatic polyethylene micropowder.
The preferable technical scheme is as follows: the polyethylene raw material is at least one of low density polyethylene, high density polyethylene and linear low density polyethylene.
The preferable technical scheme is as follows: the freeze drying process conditions are as follows: the vacuum gauge pressure is-0.09 to-0.10 MPa, and the temperature is-80 to-40 ℃, and the freeze drying treatment is carried out for 4 to 8 hours.
Due to the application of the technical scheme, compared with the prior art, the invention has the advantages that:
1. the composite solvent used in the invention has simple components and universal effect on different types of polyethylene raw materials.
2. The polyethylene micropowder obtained by the invention has the characteristics of monodispersity and narrow particle size distribution.
3. The polyethylene micropowder obtained by the invention has antistatic property.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Examples 1 to 4: preparation method of monodisperse antistatic polyethylene micropowder
A preparation method of monodisperse antistatic polyethylene micropowder comprises the following technical steps.
(1) Ball milling by filling nitrogen at low temperature
The polyethylene raw material is one or more of Low Density Polyethylene (LDPE), High Density Polyethylene (HDPE) and Linear Low Density Polyethylene (LLDPE).
Putting the polyethylene raw material into closed stainless steel ball milling equipment at the ambient temperature of 0-10 ℃, pumping out air in the ball milling equipment, filling nitrogen, starting the ball milling equipment, and fully grinding the polyethylene raw material to 100-150 meshes to obtain polyethylene powder for later use.
(2) Preparing composite solvent
Mixing 50-70 parts of main solvent, 15-25 parts of solubilizer, 0.5-5.0 parts of dispersant and 0.5-5.0 parts of antistatic agent according to a proportion, and fully and uniformly stirring to obtain the composite solvent for later use.
The main solvent is one or the combination of more than two of monochlorotoluene, dichlorotoluene and trichlorotoluene.
The solubilizer is one or the combination of more than two of propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol butyl ether, ethylene glycol ethyl ether and ethylene glycol butyl ether.
The dispersant is one or the combination of more than two of hydroxypropyl methyl cellulose, hydroxymethyl cellulose and hydroxyethyl cellulose.
The antistatic agent is one or the combination of more than two of polyaniline, polypyrrole and polythiophene.
(3) Resonance acoustic mixed dissolution
Mixing the polyethylene powder in the step (1) and the composite solvent in the step (2) according to the mass ratio of (10-35):100, putting the mixture into a resonance sound mixing device, and treating the mixture for 15-30min under the conditions of the frequency of 80-150Hz and the amplitude of 1.0-2.0mm to obtain a mixed solution.
(4) Grinding treatment with colloid mill
And (4) treating the mixed solution in the step (3) to the fineness of 10-50 mu m by using a colloid mill under the conditions of room temperature and nitrogen protection to obtain a refined mixed solution.
(5) Ultrasonic wave and microwave cooperative treatment
And (3) refining the mixed solution in the step (4), putting the refined mixed solution in an ultrasonic microwave reactor, and simultaneously performing ultrasonic treatment and microwave treatment, wherein the ultrasonic treatment conditions are that the ultrasonic frequency is 25-35KHz, the power density is 0.25-0.50W/cm2, the microwave treatment conditions are that the frequency is 2450MHz, the radiation intensity is 0.2-2.0W/cm2, and the treatment time is 10-20 min.
The ultrasonic microwave reactor is a chemical reactor provided with an ultrasonic generator and a microwave generator.
(6) Freeze drying
And (3) putting the material treated in the step (5) into a freeze drying device, and carrying out freeze drying treatment for 4-8h under the conditions of vacuum gauge pressure of-0.09-0.10 MPa and temperature of-80-40 ℃ to obtain the material, namely the monodisperse antistatic polyethylene micropowder.
The monodisperse antistatic polyethylene micropowder has the characteristics of monodispersity and narrow particle size distribution, and the particle size is 20-35 mu m; meanwhile, the antistatic coating has antistatic property.
Example 1
A preparation method of monodisperse antistatic polyethylene micropowder is prepared from the following component raw materials in parts by mass:
20 parts of low-density polyethylene particles;
main solvent: 45 parts of 4-chlorotoluene; solubilizer: 25 parts of propylene glycol methyl ether; dispersing agent: 1.5 parts of hydroxypropyl methyl cellulose; antistatic agent: 0.5 part of polyaniline.
The temperature for freeze-drying was-40 ℃.
Example 2
A preparation method of monodisperse antistatic polyethylene micropowder is prepared from the following component raw materials in parts by mass:
25 parts of low-density polyethylene particles;
main solvent: 50 parts of 2, 4-dichlorotoluene; solubilizer: 20 parts of propylene glycol ethyl ether; dispersing agent: 1.0 part of methyl cellulose; antistatic agent: 0.5 part of polypyrrole.
The temperature for freeze-drying was-50 ℃.
Example 3
A preparation method of monodisperse antistatic polyethylene micropowder is prepared from the following component raw materials in parts by mass:
20 parts of high-density polyethylene particles;
main solvent: 40 parts of 2, 6-dichlorotoluene; solubilizer: 15 parts of propylene glycol butyl ether; dispersing agent: 1.0 part of hydroxyethyl cellulose; antistatic agent: 2.0 parts of polythiophene.
The temperature for freeze-drying was-60 ℃.
Example 4
A preparation method of monodisperse antistatic polyethylene micropowder is prepared from the following component raw materials in parts by mass:
30 parts of linear low-density polyethylene particles;
main solvent: 40 parts of trichlorotoluene; solubilizer: 25 parts of ethylene glycol butyl ether; dispersing agent: 1.5 parts of hydroxyethyl cellulose; antistatic agent: 2.0 parts of polyaniline.
The temperature for freeze-drying was-80 ℃.
| Serial number | Polyethylene micropowder particle size/mum |
| Example 1 | 25 |
| Example 2 | 30 |
| Example 3 | 35 |
| Example 4 | 20 |
Example 5: preparation method of monodisperse antistatic polyethylene micropowder
A preparation method of monodisperse antistatic polyethylene micropowder comprises the following steps:
step 1: under the condition that the temperature is 0 ℃ and under the protection of nitrogen, grinding a polyethylene raw material to 100 meshes to obtain polyethylene powder;
step 2: uniformly mixing 50 parts by weight of a main solvent, 15 parts by weight of a solubilizer, 0.5 part by weight of a dispersant and 0.5 part by weight of an antistatic agent to obtain a composite solvent; the main solvent is monochlorotoluene and dichlorotoluene according to the weight ratio of 1: 2 in a volume ratio; the solubilizer is propylene glycol ethyl ether or ethylene glycol ethyl ether according to the weight ratio of 1: 1 in a volume ratio; the dispersing agent is hydroxypropyl methyl cellulose, methyl cellulose and hydroxymethyl cellulose, and the weight ratio of the dispersing agent to the hydroxypropyl methyl cellulose to the hydroxymethyl cellulose is 1: 2: 1 in a volume ratio; the antistatic agent is polyaniline and polypyrrole according to the weight ratio of 1: 1 in a volume ratio;
and step 3: mixing polyethylene powder and a composite solvent according to a mass ratio of 10:100, placing into a resonance sound mixing device, and treating for 15min under the conditions of frequency 80Hz and amplitude of 1.0mm to obtain a mixed solution;
and 4, step 4: grinding treatment with colloid mill
Under the protection of nitrogen, grinding the mixed solution to the fineness of 10 mu m to obtain a refined mixed solution;
and 5: simultaneously carrying out ultrasonic treatment and microwave treatment on the refined mixed solution, wherein the ultrasonic treatment conditions comprise ultrasonic frequency of 25KHz and power density of 0.25W/cm2The microwave treatment conditions are 2450MHz frequency and 0.2w/cm radiation intensity2Treating for 10 min;
step 6: and (5) freeze-drying the material obtained in the step (5) to obtain the material, namely the monodisperse antistatic polyethylene micropowder.
The preferred embodiment is: the polyethylene raw material is low-density polyethylene.
The preferred embodiment is: the freeze drying process conditions are as follows: freezing and drying for 4h under the conditions of vacuum gauge pressure of-0.09 MPa and temperature of-80 ℃.
Example 6: preparation method of monodisperse antistatic polyethylene micropowder
A preparation method of monodisperse antistatic polyethylene micropowder comprises the following steps:
step 1: under the condition of 10 ℃ and under the protection of nitrogen, grinding a polyethylene raw material to 150 meshes to obtain polyethylene powder;
step 2: uniformly mixing 70 parts by weight of main solvent, 25 parts by weight of solubilizer, 5.0 parts by weight of dispersant and 5.0 parts by weight of antistatic agent to obtain a composite solvent; the main solvents are monochlorotoluene, dichlorotoluene and trichlorotoluene according to the weight ratio of 1: 1: 1 in a volume ratio; the solubilizer is prepared from propylene glycol methyl ether, propylene glycol ethyl ether and ethylene glycol ethyl ether according to the weight ratio of 1: 1: 1 in a volume ratio; the dispersant is methyl cellulose, hydroxymethyl cellulose and hydroxyethyl cellulose in a ratio of 1: 1: 1 in a volume ratio; the antistatic agent is polyaniline, polypyrrole and polythiophene according to the weight ratio of 1: 1: 1 in a volume ratio;
and step 3: mixing polyethylene powder and a composite solvent according to a mass ratio of 35:100, placing into a resonance sound mixing device, and treating for 30min under the conditions of a frequency of 150Hz and an amplitude of 2.0mm to obtain a mixed solution;
and 4, step 4: under the protection of nitrogen, grinding the mixed solution to the fineness of 40-50 μm to obtain a refined mixed solution;
and 5: simultaneously carrying out ultrasonic treatment and microwave treatment on the refined mixed solution, wherein the ultrasonic treatment conditions comprise ultrasonic frequency of 35KHz and power density of 0.50W/cm2The microwave treatment condition is 2450MHz frequency and 2.0w/cm radiation intensity2Treating for 20 min;
step 6: and (5) freeze-drying the material obtained in the step (5) to obtain the material, namely the monodisperse antistatic polyethylene micropowder.
The preferred embodiment is: the polyethylene raw materials are low-density polyethylene and high-density polyethylene according to the weight ratio of 1: 1, in a mass ratio of 1.
The preferred embodiment is: the freeze drying process conditions are as follows: carrying out freeze drying treatment for 8h under the conditions of vacuum gauge pressure of-0.10 MPa and temperature of-40 ℃.
The foregoing is illustrative of the preferred embodiment of the present invention and is not to be construed as limiting thereof in any way, and any modifications or variations thereof that fall within the spirit of the invention are intended to be included within the scope thereof.
Claims (3)
1. A preparation method of monodisperse antistatic polyethylene micropowder is characterized by comprising the following steps: comprises the following steps:
step 1: under the condition that the temperature is 0-10 ℃ and under the protection of nitrogen, grinding the polyethylene raw material to 100-150 meshes to obtain polyethylene powder;
step 2: uniformly mixing 50-70 parts by weight of main solvent, 15-25 parts by weight of solubilizer, 0.5-5.0 parts by weight of dispersant and 0.5-5.0 parts by weight of antistatic agent to obtain a composite solvent; the main solvent is at least one of monochlorotoluene, dichlorotoluene and trichlorotoluene; the solubilizer is at least one of propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol butyl ether, ethylene glycol ethyl ether and ethylene glycol butyl ether; the dispersing agent is at least one of hydroxypropyl methyl cellulose, hydroxymethyl cellulose and hydroxyethyl cellulose; the antistatic agent is at least one of polyaniline, polypyrrole and polythiophene;
and step 3: mixing polyethylene powder and a composite solvent according to a mass ratio of 10-35:100, placing into a resonance sound mixing device, and treating for 15-30min under the conditions of frequency of 80-150Hz and amplitude of 1.0-2.0mm to obtain a mixed solution;
and 4, step 4: under the protection of nitrogen, grinding the mixed solution to the fineness of 10-50 mu m to obtain a refined mixed solution;
and 5: simultaneously carrying out ultrasonic treatment and microwave treatment on the refined mixed solution, wherein the ultrasonic treatment conditions comprise ultrasonic frequency of 25-35KHz and power density of 0.25-0.50W/cm2The microwave treatment conditions include 2450MHz frequency and 0.2-2.0w/cm radiation intensity2The treatment time is 10-20 min;
step 6: and (5) freeze-drying the material obtained in the step (5) to obtain the material, namely the monodisperse antistatic polyethylene micropowder.
2. The preparation method of the monodisperse antistatic polyethylene micropowder of claim 1, characterized by comprising the following steps: the polyethylene raw material is at least one of low density polyethylene, high density polyethylene and linear low density polyethylene.
3. The preparation method of the monodisperse antistatic polyethylene micropowder of claim 1, characterized by comprising the following steps: the freeze drying process conditions are as follows: vacuum gauge pressure of-0.09 to-0.10 MPa and temperature of-80 to-40 ℃ and freeze drying for 4 to 8 hours.
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