CN113831624A - Modified polyethylene breathable master batch and preparation method thereof - Google Patents
Modified polyethylene breathable master batch and preparation method thereof Download PDFInfo
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- 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
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- 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
- C08J2423/04—Homopolymers or copolymers of ethene
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Abstract
The invention relates to a modified polyethylene air-permeable master batch and a preparation method thereof, wherein the master batch comprises raw materials of polyethylene, modified graphene dispersion liquid, talcum powder, calcium carbonate and an auxiliary agent, and the preparation method comprises the steps of mixing and stirring the polyethylene, the talcum powder, the calcium carbonate, an antioxidant and a stabilizer uniformly, and then melting, extruding, granulating and drying the mixture; and completely soaking the obtained polyethylene particles in the modified graphene dispersion liquid, heating and stirring, removing the solvent, and drying by blowing to obtain the modified polyethylene breathable master batch. The modified polyethylene breathable master batch prepared by the invention can effectively improve the mechanical property of the polyethylene material and realize the preparation of the ultrathin breathable film with smaller gram weight. The method is simple, economical and environment-friendly, and can realize large-scale continuous production.
Description
Technical Field
The invention relates to the field of composite materials, and particularly relates to a modified polyethylene breathable master batch and a preparation method thereof.
Background
The polyethylene breathable film is widely applied to products such as disposable medical mattresses, protective clothing, baby diapers, building waterproofing and the like. The polyethylene breathable film is generally a breathable master batch prepared by adding inorganic filler into polyethylene, and is formed into a film by casting, calendaring and blow molding methods, and then is stretched to form the breathable film with nano micropores. However, the breathable film prepared from the existing polyethylene breathable colloidal particles has the defects of insufficient tensile property, thicker prepared breathable film, larger gram weight and the like, and the application range of the breathable film is limited to a certain extent.
At present, researches show that the performance of the polymer can be obviously improved by adding the graphene into the polymer in the form of nano-filler, but the specific surface area of the graphene is very large, and the agglomeration and stacking in a dry state are easily caused by the van der waals force between layers, so that the product effect of the composite material can be influenced. Therefore, how to uniformly and stably disperse the graphene in the polyethylene matrix is a key technology for preparing the modified polyethylene breathable master batch.
Patent CN111995811A discloses a graphene modified ultra-high molecular weight polyethylene and a preparation method thereof, wherein the preparation method comprises mixing, melting and shearing graphene, a second filler, a flow modifier, a surface modifier and an antioxidant; and then carrying out secondary melting and blending with the ultrahigh molecular weight polyethylene and the nucleating agent to obtain the graphene modified ultrahigh molecular weight polyethylene composite material. The preparation method adds the second filler such as silicon carbide, carbon fiber and the like and the surface modifier such as silane coupling agent, titanate coupling agent and the like, simultaneously the melting temperature reaches about 200 ℃, the cost is high, the process is complex, the requirement on equipment is high, and the preparation method is not suitable for industrial production.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides the modified polyethylene master batch which has uniform dispersion and good mechanical property and can realize the preparation of the breathable film with ultra-small gram weight and the preparation method thereof.
The technical scheme for solving the technical problems is as follows:
the invention provides a modified polyethylene breathable master batch which is characterized by comprising the following components in parts by weight: 40-70 parts of polyethylene, 0.5-2.5 parts of talcum powder, 35-60 parts of calcium carbonate, 0.1-2 parts of antioxidant, 0.1-2 parts of stabilizer and 80-110 parts of modified graphene dispersion liquid; the modified graphene dispersion liquid comprises 0.1-2 parts of graphene, 0.1-1 part of a dispersing agent and 60-100 parts of a solvent;
preferably 45-65 parts of polyethylene, 1-2 parts of talcum powder, 40-55 parts of calcium carbonate, 1-2 parts of antioxidant, 1-2 parts of stabilizer and 80-105 parts of modified graphene dispersion liquid; the modified graphene dispersion liquid comprises 0.4-1.2 parts of graphene, 0.1-0.7 part of dispersant and 80-100 parts of solvent;
further, the polyethylene is low-density polyethylene with the density of 0.910-0.925 g/cm3;
Further, the transverse size of the graphene is 0.4-50 microns, and the number of sheets is less than 10;
further, the particle size distribution of the calcium carbonate is 0.4-10 μm;
further, the antioxidant is one or more of a phenolic antioxidant, a sulfur antioxidant, a phosphorus antioxidant or a natural antioxidant; the stabilizer is one or more of an ultraviolet absorbent or a light stabilizer; the dispersant is one or more of BYK dispersant, WS dispersant, Silok dispersant, AKN2261 dispersant, EFKA4047 dispersant or TEGO dispersant;
further, the solvent is one or more of methanol, ethanol, dichloromethane, chloroform, N-dimethylformamide or xylene;
the invention also provides a preparation method of the modified polyethylene breathable master batch, which is characterized by comprising the following steps:
(1) weighing various raw materials of polyethylene, talcum powder, calcium carbonate, antioxidant and stabilizer in parts by weight, uniformly stirring, melting, extruding, granulating and drying;
(2) completely soaking the polyethylene particles obtained in the step (1) in the modified graphene dispersion liquid, heating and stirring, removing the solvent, and drying by blowing to obtain modified polyethylene breathable master batches;
further, the heating temperature zone of the screw extrusion in the step (1) is as follows: the temperature of the drying machine is 150 ℃ in the region 1, 160 ℃ in the region 2, 180 ℃ in the region 3, 190 ℃ in the region 4, 200 ℃ in the region 5, 205 ℃ in the region 6, 210 ℃ in the region 7, 210 ℃ in the region 8, 205 ℃ in the head, and 95-115 ℃ in the drying temperature; the preferable drying temperature is 105 ℃;
further, the heating temperature of the step (2) is 90-115 ℃, and the drying temperature is 115-135 ℃; preferably, the heating temperature is 95-110 ℃, and the drying temperature is 125 ℃;
further, the preparation method of the modified graphene dispersion liquid comprises the following steps: weighing graphene, a dispersing agent and a solvent according to the parts by weight, adding the graphene, the dispersing agent and the solvent into a grinding disperser, stirring and dispersing, and performing ultrasonic treatment to obtain the graphene/graphene composite material;
further, in the preparation step of the modified graphene dispersion liquid, stirring time is 30-50 min, stirring speed is 1600-2400 r/min, and ultrasonic time is 30-60 min; preferably, the stirring time is 40-50 min, the stirring speed is 2000r/min, and the ultrasonic time is 30-50 min.
The invention has the beneficial effects that:
(1) through a multiple dispersion technology, agglomeration and uneven dispersion of graphene are effectively avoided;
(2) graphene is uniformly added into a polyethylene material, so that the mechanical property of the polyethylene breathable master batch is effectively improved, and the preparation of the breathable film with ultra-small gram weight can be realized;
(3) the invention can recycle the solvent, is economic and environment-friendly, and is suitable for large-scale industrial production.
Detailed Description
The invention is illustrated but not limited by the following examples. The technical solutions protected by the present invention are all the simple replacements or modifications made by the skilled person in the art.
Example 1:
weighing 45 parts of polyethylene, 1 part of talcum powder, 40 parts of nano calcium carbonate, 1 part of antioxidant and 1 part of stabilizer in a stirring dispersion machine, mixing and stirring for 30min at the rotating speed of 600r/min, uniformly mixing, and performing melt extrusion, wherein a heating temperature area extruded by a screw is as follows: 150 ℃ in the region 1, 160 ℃ in the region 2, 180 ℃ in the region 3, 190 ℃ in the region 4, 200 ℃ in the region 5, 205 ℃ in the region 6, 210 ℃ in the region 7, 210 ℃ in the region 8, 205 ℃ in the head, granulating by water cooling, and drying by blowing at 105 ℃ for later use;
weighing 0.4 part of graphene and 0.1 part of dispersing agent, adding the mixture into 80 parts of solvent under stirring, and grinding and dispersing for 40min by using a grinding disperser at the rotating speed of 2000 r/min. Then transferring the graphene into a water bath ultrasonic machine, carrying out ultrasonic treatment for 30min at the ultrasonic frequency of 50%, and obtaining a modified graphene dispersion liquid for later use after the ultrasonic treatment is finished;
and adding the dried polyethylene particles into the newly prepared modified graphene dispersion liquid, completely soaking the polyethylene particles, heating to 95 ℃, carrying out reduced pressure distillation, collecting the solvent, carrying out forced air drying on the residual solid at 125 ℃ to obtain the modified polyethylene breathable colloidal particles, and carrying out moisture-proof sealed storage.
Example 2:
weighing 49 parts of polyethylene, 1.2 parts of talcum powder, 46 parts of nano calcium carbonate, 1.2 parts of antioxidant and 1.2 parts of stabilizer in a stirring dispersion machine, mixing and stirring for 30min at the rotating speed of 600r/min, uniformly mixing, and performing melt extrusion, wherein a heating temperature zone for screw extrusion is as follows: 150 ℃ in the region 1, 160 ℃ in the region 2, 180 ℃ in the region 3, 190 ℃ in the region 4, 200 ℃ in the region 5, 205 ℃ in the region 6, 210 ℃ in the region 7, 210 ℃ in the region 8, 205 ℃ in the head, granulating by water cooling, and drying by blowing at 105 ℃ for later use;
0.6 part of graphene and 0.2 part of dispersing agent are weighed and added into 95 parts of solvent under stirring, and a grinding disperser is used for grinding and dispersing for 45min at the rotating speed of 2000 r/min. Then transferring the graphene into a water bath ultrasonic machine, carrying out ultrasonic treatment for 40min at the ultrasonic frequency of 50%, and obtaining a modified graphene dispersion liquid for later use after the ultrasonic treatment is finished;
and adding the dried polyethylene particles into the newly prepared modified graphene dispersion liquid, completely soaking the polyethylene particles, heating to 100 ℃, carrying out reduced pressure distillation, collecting the solvent, carrying out forced air drying on the residual solid at 125 ℃ to obtain the modified polyethylene breathable colloidal particles, and carrying out moisture-proof sealed storage.
Example 3:
weighing 53 parts of polyethylene, 2 parts of talcum powder, 51 parts of nano calcium carbonate, 1.6 parts of antioxidant and 1.6 parts of stabilizer in a stirring dispersion machine, mixing and stirring for 40min at the rotating speed of 600r/min, uniformly mixing, and performing melt extrusion, wherein a heating temperature zone for screw extrusion is as follows: 150 ℃ in the region 1, 160 ℃ in the region 2, 180 ℃ in the region 3, 190 ℃ in the region 4, 200 ℃ in the region 5, 205 ℃ in the region 6, 210 ℃ in the region 7, 210 ℃ in the region 8, 205 ℃ in the head, granulating by water cooling, and drying by blowing at 105 ℃ for later use;
weighing 0.8 part of graphene and 0.4 part of dispersing agent, adding the graphene and the dispersing agent into 100 parts of solvent under stirring, and grinding and dispersing for 45min by using a grinding disperser at the rotating speed of 2000 r/min. Then transferring the graphene into a water bath ultrasonic machine, carrying out ultrasonic treatment for 45min at an ultrasonic frequency of 50%, and obtaining a modified graphene dispersion liquid for later use after the ultrasonic treatment is finished;
and adding the dried polyethylene particles into the newly prepared modified graphene dispersion liquid, completely soaking the polyethylene particles, heating to 105 ℃, carrying out reduced pressure distillation, collecting the solvent, carrying out forced air drying on the residual solid at 125 ℃ to obtain the modified polyethylene breathable colloidal particles, and carrying out moisture-proof sealed storage.
Example 4:
weighing 55 parts of polyethylene, 2 parts of talcum powder, 55 parts of nano calcium carbonate, 2 parts of antioxidant and 2 parts of stabilizer in a stirring dispersion machine, mixing and stirring for 50min at the rotating speed of 600r/min, uniformly mixing, and performing melt extrusion, wherein a heating temperature area extruded by a screw is as follows: 150 ℃ in the region 1, 160 ℃ in the region 2, 180 ℃ in the region 3, 190 ℃ in the region 4, 200 ℃ in the region 5, 205 ℃ in the region 6, 210 ℃ in the region 7, 210 ℃ in the region 8, 205 ℃ in the head, granulating by water cooling, and drying by blowing at 105 ℃ for later use;
weighing 1.2 parts of graphene and 0.7 part of dispersing agent, adding into 80 parts of solvent under stirring, and grinding and dispersing for 50min by using a grinding disperser at the rotating speed of 2000 r/min. Then transferring the graphene into a water bath ultrasonic machine, carrying out ultrasonic treatment for 50min at the ultrasonic frequency of 50%, and obtaining a modified graphene dispersion liquid for later use after the ultrasonic treatment is finished;
and adding the dried polyethylene particles into the newly prepared modified graphene dispersion liquid, completely soaking the polyethylene particles, heating to 110 ℃, carrying out reduced pressure distillation, collecting the solvent, carrying out forced air drying on the residual solid at 125 ℃ to obtain the modified polyethylene breathable colloidal particles, and carrying out moisture-proof sealed storage.
Comparative example 1:
weighing 45 parts of polyethylene, 0.4 part of graphene, 1 part of talcum powder, 40 parts of nano calcium carbonate, 1 part of antioxidant and 1 part of stabilizer in a stirring dispersion machine, mixing and stirring for 30min at the rotating speed of 600r/min, uniformly mixing, and performing melt extrusion, wherein a heating temperature zone extruded by a screw is as follows: 150 ℃ in the region 1, 160 ℃ in the region 2, 180 ℃ in the region 3, 190 ℃ in the region 4, 200 ℃ in the region 5, 205 ℃ in the region 6, 210 ℃ in the region 7, 210 ℃ in the region 8, 205 ℃ in the head, water-cooling and granulating, and drying by blowing at 125 ℃ to obtain the modified polyethylene breathable colloidal particles, and storing in a moisture-proof and sealed manner.
Comparative example 2:
weighing 45 parts of polyethylene, 1 part of talcum powder, 40 parts of nano calcium carbonate, 1 part of antioxidant and 1 part of stabilizer in a stirring dispersion machine, mixing and stirring for 30min at the rotating speed of 600r/min, uniformly mixing, and performing melt extrusion, wherein a heating temperature area extruded by a screw is as follows: 150 ℃ in the region 1, 160 ℃ in the region 2, 180 ℃ in the region 3, 190 ℃ in the region 4, 200 ℃ in the region 5, 205 ℃ in the region 6, 210 ℃ in the region 7, 210 ℃ in the region 8, 205 ℃ in the head, water-cooling and granulating, and drying by blowing at 125 ℃ to obtain the modified polyethylene breathable colloidal particles, and storing in a moisture-proof and sealed manner.
Comparative example 3:
weighing 45 parts of polyethylene, 1 part of talcum powder, 40 parts of nano calcium carbonate, 1 part of antioxidant and 1 part of stabilizer in a stirring dispersion machine, mixing and stirring for 30min at the rotating speed of 600r/min, uniformly mixing, and performing melt extrusion, wherein a heating temperature area extruded by a screw is as follows: 150 ℃ in the region 1, 160 ℃ in the region 2, 180 ℃ in the region 3, 190 ℃ in the region 4, 200 ℃ in the region 5, 205 ℃ in the region 6, 210 ℃ in the region 7, 210 ℃ in the region 8, 205 ℃ in the head, granulating by water cooling, and drying by blowing at 105 ℃ for later use;
weighing 0.4 part of graphene and 0.1 part of dispersing agent, adding the mixture into 80 parts of solvent under stirring, and grinding and dispersing for 60min by using a grinding disperser at the rotating speed of 800 r/min. Then transferring the graphene into a water bath ultrasonic machine, carrying out ultrasonic treatment for 30min at the ultrasonic frequency of 50%, and obtaining a modified graphene dispersion liquid for later use after the ultrasonic treatment is finished;
and adding the dried polyethylene particles into the newly prepared modified graphene dispersion liquid, completely soaking the polyethylene particles, heating to 95 ℃, carrying out reduced pressure distillation, collecting the solvent, carrying out forced air drying on the residual solid at 125 ℃ to obtain the modified polyethylene breathable colloidal particles, and carrying out moisture-proof sealed storage.
Test example:
the master batches obtained in examples 1-4 and comparative examples 1-2 were used to prepare breathable films for performance testing, and the results were as follows:
the foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (10)
1. The modified polyethylene breathable master batch is characterized by comprising the following components in parts by weight: 40-70 parts of polyethylene, 0.5-2.5 parts of talcum powder, 35-60 parts of calcium carbonate, 0.1-2 parts of antioxidant, 0.1-2 parts of stabilizer and 80-110 parts of modified graphene dispersion liquid; the modified graphene dispersion liquid comprises 0.1-2 parts of graphene, 0.1-1 part of a dispersing agent and 60-100 parts of a solvent.
2. The modified polyethylene breathable masterbatch of claim 1, wherein the polyethylene is low density polyethylene with a density of 0.910-0.925 g/cm3。
3. The modified polyethylene breathable master batch of claim 1, wherein the graphene has a transverse dimension of 0.4-50 μm and has less than 10 layers.
4. The modified polyethylene breathable master batch according to claim 1, wherein the antioxidant is one or more of a phenolic antioxidant, a sulfur antioxidant, a phosphorus antioxidant or a natural antioxidant; the stabilizer is one or more of an ultraviolet absorbent or a light stabilizer; the dispersant is one or more of BYK dispersant, WS dispersant, Silok dispersant, AKN2261 dispersant, EFKA4047 dispersant or TEGO dispersant.
5. The modified polyethylene breathable masterbatch according to claim 1, wherein the solvent is one or more of methanol, ethanol, dichloromethane, chloroform, N-dimethylformamide or xylene.
6. The preparation method of the modified polyethylene breathable master batch according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) weighing various raw materials of polyethylene, talcum powder, calcium carbonate, antioxidant and stabilizer in parts by weight, uniformly stirring, melting, extruding, granulating and drying;
(2) and (2) completely soaking the polyethylene particles obtained in the step (1) in the modified graphene dispersion liquid, heating and stirring, removing the solvent, and drying by blowing to obtain the modified polyethylene breathable master batch.
7. The preparation method of the modified polyethylene breathable master batch according to claim 6, wherein the heating temperature zone of the screw extrusion in the step (1) is as follows: 145-155 ℃ in the area 1, 155-165 ℃ in the area 2, 175-185 ℃ in the area 3, 185-195 ℃ in the area 4, 195-205 ℃ in the area 5, 200-210 ℃ in the area 6, 205-215 ℃ in the area 7, 205-215 ℃ in the area 8, 205 ℃ in the head, and 95-135 ℃ in the drying temperature.
8. The preparation method of the modified polyethylene breathable master batch according to claim 6, wherein the heating temperature in the step (2) is 90-115 ℃, and the drying temperature is 115-135 ℃.
9. The preparation method of the modified polyethylene breathable masterbatch according to claim 6, wherein the preparation step of the modified graphene dispersion liquid comprises the following steps: weighing graphene, a dispersing agent and a solvent according to the parts by weight, adding the graphene, the dispersing agent and the solvent into a grinding disperser, stirring and dispersing, and performing ultrasonic treatment to obtain the graphene/graphene composite material.
10. The preparation method of the modified polyethylene breathable master batch according to claim 9, wherein in the preparation step of the modified graphene dispersion, the stirring time is 30-50 min, the stirring speed is 1600-2400 r/min, and the ultrasonic time is 30-60 min.
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