CN112831112B - Cross-linked polyethylene foam material and preparation method thereof - Google Patents
Cross-linked polyethylene foam material and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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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
- 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
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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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
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- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
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- C08K5/098—Metal salts of carboxylic acids
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- 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
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Abstract
The application discloses a cross-linked polyethylene foam material and a preparation method thereof. Compared with the prior art, the cross-linked polyethylene foam material has better antibacterial property which is more than 95%; the cross-linked polyethylene foam material has the advantages of higher surface tension, longer surface tension maintaining time, better product adhesion and wettability and more contribution to the gluing performance of the product.
Description
Technical Field
The embodiment of the invention relates to a high polymer material, in particular to a crosslinked polyethylene foam material and a preparation method thereof.
Background
The cross-linked polyethylene foam material is a novel foam plastic with a closed pore structure between soft (polyurethane) foam materials and hard (polystyrene) foam materials, has a series of characteristics of excellent toughness, elasticity, flexibility, wear resistance, chemical corrosion resistance, low temperature resistance, good insulativity and the like, and can be used as a good insulating, heat-insulating, shockproof and buoyancy material. The antibacterial polyethylene foam product is widely applied to the fields of mechanical shock absorption, ground mats, automotive interiors, electronic equipment and the like, and has higher requirements on the antibacterial performance of material products along with the update of the product.
The method for improving the antibacterial property of the polyethylene foaming product in the prior art mainly comprises the addition of an antibacterial agent, but the antibacterial agent is expensive and has poor compatibility with a polyethylene system, and the antibacterial agent is easy to migrate to the surface along with time, so that the antibacterial durability of the material is reduced, and the requirement of long-term use cannot be met.
In addition, the non-polar surface tension of the polyethylene foamed product is small, and the requirement of a gluing process can be met. However, corona equipment is expensive and high in energy consumption, and the surface tension of the polyethylene foamed product after corona treatment can only be maintained for about 2 weeks, so that the polyethylene foamed product cannot be stored for a long time. The addition of the ethylene-vinyl acetate copolymer resin (EVA) with polar ester groups can also improve the non-polar surface tension of the polyethylene foaming product, but the use of the ethylene-vinyl acetate copolymer resin (EVA) increases the process cost, and the ethylene-vinyl acetate copolymer resin (EVA) has weak polarity and needs to be added in a large amount, so that the product is easy to seriously self-adhere, and the yield is reduced.
Disclosure of Invention
The invention aims to provide a cross-linked polyethylene foam material which is more durable in antibiosis, higher in surface tension, better in surface adhesion and wettability and beneficial to the gluing performance of products.
In order to solve the technical problems, the invention provides a crosslinked polyethylene foam material in a first aspect, wherein the crosslinked polyethylene foam material is prepared by crosslinking polyethylene and alkenyl pyridinium.
The polyethylene density ranges are: 0.91 to 0.93; the polyethylene is preferably low density polyethylene, linear low density polyethylene, or a combination of both. When the polyethylene is a combination of low density polyethylene and linear low density polyethylene, the mass ratio of the low density polyethylene to the linear low density polyethylene is 100: 10-100: 60, preferably 100:30, and it is considered that when the mass ratio of the low density polyethylene to the linear low density polyethylene is in the above range, the prepared crosslinked polyethylene foam material has excellent gluing performance.
The alkenyl pyridine salt may be prepared by a complex reaction of alkenyl pyridine and metal salt, but is not limited thereto.
The alkenyl pyridine can be C-substituted at 2,3, 4, 5 and/or 6 position 1～6 Alkenyl-substituted pyridines, preferably alkenyl pyridines which may be C-substituted in the 2-, 4-and/or 6-position 1～6 Alkenyl-substituted pyridines; said C is 1～6 Alkenyl is preferably vinyl, propenyl, allyl, butenyl, butadienyl, cyclopentenyl, cyclopentadienyl, cyclohexenyl or cyclohexadienyl; the alkenyl pyridine at least contains one pyridyl group, and preferably contains one or two pyridyl groups; preferably, the alkenyl pyridine is at least one of 2-vinylpyridine, 4-vinylpyridine, 2-allylpyridine, 4-dipyridyl butadiene and 2, 3-cyclohexenopyridine.
In the alkenyl pyridine, 2,3, 4, 5 and 6 positions of the pyridine are respectively shown as follows:
the metal salt is at least one of zinc salt, calcium salt, copper salt, nickel salt, iron salt and cobalt salt. Preferably, the metal salt is a chloride salt of zinc, calcium, copper, nickel, iron or cobalt metal; and/or acetates of zinc, calcium, copper, nickel, iron or cobalt metals. For example: at least one of zinc chloride, zinc acetate, copper chloride, cobalt acetate, nickel chloride and iron acetate.
In some preferred embodiments, the mass ratio of the alkenyl pyridine to the metal salt in the complexation reaction is 1:1 to 1:2, and preferably, the mass ratio of the alkenyl pyridine to the metal salt is 1:1.5 to 1:2, for example: 100 parts by weight of the alkenyl pyridine compound and 150 to 300 parts by weight of the metal salt; the reaction medium of the complexation reaction is not limited to that which allows the dissolved reactant to react with the reactant, for example: ethanol; the temperature of the complex reaction is preferably 35-65 ℃; the reaction time of the complexing reaction is preferably 5-20 h; specifically, the complexation reaction is to stir 100 parts by weight of the alkenyl pyridine compound and 150-300 parts by weight of the metal salt in an ethanol solution at 35-65 ℃ for 5-20 hours to react to obtain the alkenyl pyridine salt.
The second aspect of the present invention provides a method for preparing the above cross-linked polyethylene foam material, wherein the method for preparing the cross-linked polyethylene foam material comprises the steps of:
(1) 65-90 parts by weight of polyethylene;
5-20 parts by weight of an alkenyl pyridinium;
5-25 parts by weight of an elastomer;
2-20 parts by weight of a foaming agent;
1-2 parts by weight of a sensitizer;
extruding 0.5-4 parts by weight of antioxidant to prepare a master slice;
(2) carrying out irradiation crosslinking on the master slice to obtain a crosslinked master slice;
(3) and (3) foaming the crosslinked master slice obtained in the step (2) to obtain the crosslinked polyethylene foam material.
The extrusion is preferably carried out in an extruder, the extrusion temperature is preferably 95-130 ℃, the screw rotation speed is preferably 50-130 rpm, and the die head temperature is preferably 110-130 ℃.
The irradiation dose of the irradiation crosslinking is 5-50 kGy.
The high-temperature foaming temperature is preferably 180-320 ℃, and the high-temperature foaming time is preferably 0.1-3 min.
Preferably, the step (3) is further followed by a step (4) of calendering the crosslinked polyethylene foam material obtained in the step (3).
The calendering treatment can be carried out according to a method conventional in the art, and in particular, the calendering treatment can be carried out by: and (3) placing the foamed master slice in a double roller for multi-time calendaring treatment, controlling the temperature of the double roller to be 80-130 ℃, and controlling the roller gap to be 1/2-1/3 of the thickness of foam cotton.
In some preferred embodiments, the elastomer comprises at least one of ethylene-propylene-diene monomer, ethylene-octene copolymer, ethylene-vinyl acetate copolymer, natural rubber, isoprene rubber, butadiene rubber, styrene-butadiene block copolymer (SBS), pentylene block copolymer (SIS), chlorinated polyethylene;
the foaming agent comprises at least one of azodicarbonamide, benzenesulfonyl hydrazide, dinitrosopentamethylenetetramine, toluenesulfonyl hydrazide and 4, 4' -oxybis-benzenesulfonyl hydrazide;
the sensitizer comprises at least one of zinc acetate, zinc stearate, cobalt stearate, zinc oxalate, zinc oxide and barium stearate;
the antioxidant comprises 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) thioether or tetra [ beta- (3, 5-di-tertiary butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010).
The third aspect of the invention provides the use of the cross-linked polyethylene foam material, and the cross-linked polyethylene foam material can be applied to mechanical shock resistance, floor mats, heat preservation pipes and electronic equipment. The thickness of the foam material is 0.1-3.4 mm, and the thickness deviation is within 10%; at least 2 layers of cells are included in the thickness direction.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The reagents and starting materials used in the present invention are commercially available.
The main advantages of the present invention with respect to the prior art include:
(1) the cross-linked polyethylene foam material has better antibacterial property which is more than 95 percent.
(2) The cross-linked polyethylene foam material has the advantages of higher surface tension, longer surface tension maintaining time, better product adhesion and wettability and more contribution to the gluing performance of the product.
(3) The preparation method can effectively adjust the antibacterial property and the caking property of the material by adjusting the structure and the dosage of the alkenyl pyridinium.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the present invention is further described below with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers. Unless otherwise indicated, percentages and parts are by weight.
It should be noted that:
(1) the invention adopts AATCC-100 method to test the antibacterial property of the cross-linked polyethylene foam material. The Test was carried out according TO AATCC Test Method l00 (bacterial count determination) TZ/TO2021-9 in the United states, and the sample was taken from a square having an edge length of about 1.8cm and placed in a 50mL conical flask with a cap. The inoculum was diluted from about l 08-109 cfu/mL to l X l 05-2X l05cfu/mL with 0.85% ice-cold physiological saline (0-4 ℃) to prepare an inoculum solution. The sample was washed with 20mL of 0.85% ice-cold physiological saline. The bacteriostatic activity of the sample was calculated using the formula:
the bacteriostasis rate is (viable count of blank control sample after l8 h-viable count of sample after l8 h)/l 8h, and viable count of the blank control sample after.
(2) The surface tension of the crosslinked polyethylene foam material is measured by the method described in the measurement of the wetting tension of GB-T14216-2008 plastic, film and sheet.
Example 1
Step one, preparation of zinc vinylpyridine salt
Dissolving 100 parts by mass of 4-vinylpyridine in 200 parts by mass of 95% ethanol, adding 45 parts by mass of zinc chloride, carrying out stirring reaction at 60 ℃ for 12 hours, carrying out suction filtration, and washing and drying with ethanol and ethyl acetate to obtain the zinc salt of vinylpyridine.
Step two, preparation of cross-linked polyethylene foam material
Uniformly mixing 80 parts by weight of low-density polyethylene, 10 parts by weight of zinc vinylpyridine salt, 10 parts by weight of ethylene-octene copolymer, 5 parts by weight of azodicarbonamide foaming agent, 1.5 parts by weight of zinc stearate and 1 part by weight of antioxidant 1010, adding the mixture into a single-screw extruder, extruding, and controlling the extrusion temperature to be 95-125 ℃, the screw rotation speed to be 75rpm and the die head temperature to be 125 ℃ to obtain a master slice with the thickness of 0.3 mm; then, carrying out irradiation crosslinking on the master slice by an electron accelerator, and controlling the irradiation dose to be 35kGy to form a crosslinked polymer network; and finally, placing the crosslinked master slice in a foaming furnace for foaming, controlling the temperature of the foaming furnace to be 160-260 ℃, and keeping the residence time of the crosslinked master slice to be 0.5min to obtain the high-strength irradiation crosslinked polyethylene foaming material. The antibacterial property, surface tension and surface tension after 6 months were measured to obtain 99% of the antibacterial property, the surface tension was 40mN/m, and the surface tension after 6 months of standing was 39 mN/m.
Examples 2 to 6
The reaction was carried out in the same manner as in example 1 except that different metal salts were selected.
TABLE 1
Examples 7 to 10
The reaction was carried out in the same manner as in example 1 except that different alkenyl pyridines were selected.
TABLE 2
Examples 11 to 14
The same procedure as in example 1 was followed except that the ratio of alkenylpyridinium salt to polyethylene was varied.
TABLE 3
Comparative example 1
According to the embodiment 1, no alkenyl pyridinium is added, 90 parts by weight of low-density polyethylene, 10 parts by weight of ethylene-octene copolymer, 5 parts by weight of foaming agent, 1.5 parts by weight of zinc oxalate and 1 part by weight of antioxidant 1010 are uniformly mixed, and then added into a single-screw extruder for extrusion, and the extrusion temperature is controlled to be 95-125 ℃, the screw rotation speed is 80rpm, and the die head temperature is controlled to be 125 ℃, so that a master slice with the thickness of 0.5mm is obtained; then, carrying out irradiation crosslinking on the master slice by an electron accelerator, and controlling the irradiation dose to be 35kGy to form a crosslinked polymer network; and finally, placing the crosslinked master slice in a foaming furnace for foaming, controlling the temperature of the foaming furnace to be 160-260 ℃, and keeping the residence time of the crosslinked master slice for 0.4min to obtain the irradiation crosslinked polyethylene foaming material, wherein the antibacterial property is 75%, the surface tension is 32mN/m, the cohesiveness is poor, the surface tension can reach 41mN/m after corona treatment, and the surface tension is 32mN/m after the irradiation crosslinked polyethylene foaming material is placed for 6 months, and the cohesiveness is still poor.
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples for carrying out the invention, and that various changes in form and details may be made therein without departing from the spirit and scope of the invention in practice.
Claims (10)
1. The method for preparing the cross-linked polyethylene foam material is characterized in that raw materials for preparing the cross-linked polyethylene foam material comprise polyethylene and alkenyl pyridinium; the method comprises the following steps:
(1) 65-90 parts by weight of polyethylene;
5-20 parts by weight of an alkenyl pyridinium;
5-25 parts by weight of an elastomer;
2-20 parts by weight of a foaming agent;
1-2 parts by weight of a sensitizer;
extruding 0.5-4 parts by weight of antioxidant to prepare a master slice;
(2) carrying out irradiation crosslinking on the master slice to obtain a crosslinked master slice;
(3) carrying out high-temperature foaming treatment on the crosslinked master slice obtained in the step (2) to obtain the crosslinked polyethylene foam material;
wherein the alkenyl pyridine salt is prepared by the complexation reaction of alkenyl pyridine and metal salt, and the alkenyl pyridine is formed by C at least one position of 2,3, 4, 5 and 6 positions 1~6 Alkenyl-substituted pyridines;
the metal salt is at least one of zinc salt, calcium salt, copper salt, nickel salt, iron salt and cobalt salt.
2. The method according to claim 1, wherein in step (1), the extruding is performed in an extruder;
and/or in the step (2), the irradiation dose of the irradiation crosslinking is 5-50 kGy;
and/or in the step (3), the high-temperature foaming temperature is 180-320 ℃;
and/or in the step (3), the high-temperature foaming time is 0.1-3 min.
3. The method according to claim 2, wherein in the step (1), the temperature of the extruder is 95-130 ℃;
and/or in the step (1), the rotating speed of a screw of the extruder is 50-130 rpm;
and/or in the step (1), the die head temperature of the extruder is 110-130 ℃.
4. The method according to claim 1, wherein the polyethylene is a low density polyethylene and/or a linear low density polyethylene.
5. The method according to claim 4, wherein the polyethylene is low density polyethylene and linear low density polyethylene, and the mass ratio of the low density polyethylene to the linear low density polyethylene is 100: 10-100: 60;
and/or the mass ratio of alkenyl pyridine to metal salt in the complexation reaction is 1: 1-2;
and/or the reaction medium of the complexation reaction is ethanol;
and/or the temperature of the complexing reaction is 35-65 ℃;
and/or the reaction time of the complexation reaction is 5-20 h.
6. The method of claim 5, wherein C is 1~6 Alkenyl is vinyl, propenyl, allyl, butenyl, butadienyl, cyclopentenyl, cyclopentadienyl, cyclohexenyl or cyclohexadienyl;
and/or the metal salt is chloride or acetate of zinc, calcium, copper, nickel, iron or cobalt metal.
7. The method of claim 6, wherein the alkenyl pyridinium salt is the product of the reaction of: stirring 100 parts by weight of the alkenyl pyridine compound and 150-300 parts by weight of the metal salt in an ethanol solution at 35-65 ℃ for 5-20 hours to react to obtain the alkenyl pyridine salt.
8. The method of claim 6, wherein the alkenyl pyridine is at least one of 2-vinyl pyridine, 4-vinyl pyridine, 2-allyl pyridine, 4-dipyridyl butadiene and 2, 3-cyclohexenopyridine;
and/or the metal salt is at least one of zinc chloride, zinc acetate, copper chloride, cobalt acetate, nickel chloride and ferric acetate.
9. The method according to any one of claims 1 to 8, wherein the elastomer is at least one of ethylene propylene diene monomer, ethylene-octene copolymer, ethylene-vinyl acetate copolymer, natural rubber, isoprene rubber, butadiene rubber, styrene butadiene block copolymer (SBS), pentylene block copolymer (SIS), chlorinated polyethylene;
and/or the foaming agent is at least one of azodicarbonamide, benzenesulfonylhydrazide, dinitrosopentamethylenetetramine, toluenesulfonylhydrazide and 4, 4' -oxybis-benzenesulfonylhydrazide;
and/or the sensitizer is at least one of zinc acetate, zinc stearate, cobalt stearate, zinc oxalate, zinc oxide and barium stearate;
and/or; the antioxidant is 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) thioether or tetra [ beta- (3, 5-di-tertiary butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester.
10. A cross-linked polyethylene foam material, characterized in that it is prepared by the process of any one of claims 1 to 9.
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Denomination of invention: Crosslinked polyethylene foam material and its preparation method Effective date of registration: 20230606 Granted publication date: 20220902 Pledgee: Industrial and Commercial Bank of China Limited Pan'an sub branch Pledgor: ZHEJIANG WANLI NEW MATERIALS TECHNOLOGY Co.,Ltd. Registration number: Y2023330001094 |
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