CN111607152B - High-wear-resistance crosslinked polyethylene material and preparation method thereof - Google Patents
High-wear-resistance crosslinked polyethylene material and preparation method thereof Download PDFInfo
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
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- C08L2312/00—Crosslinking
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Abstract
The invention discloses a high-wear-resistance crosslinked polyethylene material and a preparation method thereof, belonging to the technical field of polymer processing. The material specifically consists of the following materials: 100-120 parts of high-density polyethylene, 15-30 parts of low-density polyethylene, 20-30 parts of crosslinking master batch, 0.5-2 parts of antioxidant master batch, 1-8 parts of epoxy resin, 0.1-1 part of curing agent and 1-5 parts of inorganic filler. The materials are mixed evenly and then put into a pair roller extruder with the temperature of 140-190 ℃ for mixing and melting, and then are extruded and granulated. The cross-linked polyethylene material disclosed by the invention has good wear resistance and mechanical properties.
Description
Technical Field
The invention relates to the field of material processing, in particular to a high-wear-resistance crosslinked polyethylene material and a preparation method thereof.
Background
Polyethylene has good physical and chemical stability and is widely applied to storage, transportation, construction and living goods, but the current polyethylene materials have relatively weak properties in the aspects of friction resistance, scratch resistance and the like, so that improvement and promotion are needed.
Patent CN 103725157A discloses a wear-resisting polyethylene pipe of anticorrosive, including body and anticorrosive wearing layer, this anticorrosive wearing layer's composition is as follows according to the part by weight count: 80-120 parts of epoxy resin, 80-120 parts of polyurethane, 30-60 parts of coal tar, 18-32 parts of curing agent, 22-45 parts of antirust agent, 6-26 parts of lubricant, 30-180 parts of white oil, 1.5-8 parts of aluminum oxide, 5-12 parts of copper dioxide, 8-15 parts of xylene and 3-10 parts of n-butyl ester. The polyethylene pipe comprises a polyethylene pipe body and an anti-corrosion wear-resistant layer, the preparation process of the material needs to be divided into two parts, the integration of the anti-corrosion wear-resistant layer and the pipe body is not realized, and the preparation process is complex; in addition, the contents of epoxy resin, polyurethane and coal tar pitch in the anti-corrosion wear-resistant layer are high, and the preparation cost is high.
Patent CN 1015924768A discloses a flame-retardant wear-resistant polypropylene cable material, which comprises the following raw materials in parts by weight: 60-80 parts of polypropylene, 30-40 parts of modified polyurethane, 20-30 parts of carbon black, 15-25 parts of light calcium carbonate, 10-15 parts of kaolin, 3-4 parts of trioctyl acetylcitrate, 1-2 parts of epoxidized soybean oil, 20-30 parts of microencapsulated red phosphorus, 5-10 parts of zinc borate, 1-2 parts of 3-aminopropyltriethoxysilane, 1-3 parts of dicumyl peroxide, 0.2-0.4 part of sulfur, 0.1-0.3 part of accelerator, 0.3-0.5 part of accelerator CZ, 1-2 parts of Ca/Zn composite stabilizer, 1-2 parts of rare earth stabilizer, 1-2 parts of dibutyltin dichloride, 0.2-0.3 part of anti-aging agent MB, 0.1-0.3 part of anti-aging agent RD and 2-4 parts of silicone powder. The modified polyurethane is adopted to modify polypropylene, and the modified polyurethane needs to be prepared in advance, so that the preparation process and the cost are increased; in addition, a large amount of stabilizers, antioxidants, accelerators and crosslinking agents are added into the material, so that the addition variety is large, and the complexity of operation is further increased.
Patent CN 106589521A discloses a flame-retardant wear-resistant PE plastic pipe, which is prepared from the following raw materials in parts by weight: 70-78 parts of high-density polyethylene, 18-24 parts of ethylene-octene block copolymer, 15-20 parts of coumarone resin, 5-9 parts of silicon dioxide, 12-14 parts of yellow lead, 4-9 parts of phthalic acid dimethyl anhydride, 10-10 parts of silane coupling agent KH 56006, 20-25 parts of epoxy resin, 10-15 parts of bentonite and 5-9 parts of triphenyl phosphite. This patent not only adopts coumarone resin to carry out the allotment again of resin matrix to polyethylene, but also adopts epoxy resin, silane coupling agent to modify polyethylene, has still increased bentonite, acid anhydride at last and has carried out the enhancement processing to the resin, has integrateed multiple allotment mode, and the material variety that adds the modifier is more, and is comparatively complicated.
Disclosure of Invention
In order to solve the problems, the application provides a high-wear-resistance crosslinked polyethylene material with a simple preparation method and a preparation method thereof. The invention introduces the cross-linking agent into the polyethylene resin to form a cross-linking system, and simultaneously introduces the binder with strong binding property, excellent mechanical property and wear resistance to further strengthen the polyethylene, the types of the additives are less, the preparation process is simple, and the prepared material has good wear resistance and excellent mechanical property.
The technical scheme of the invention is as follows:
a high-wear-resistance cross-linked polyethylene material mainly comprises the following components in parts by weight:
100 portions and 120 portions of high-density polyethylene;
15-30 parts of low-density polyethylene;
20-30 parts of a crosslinking master batch;
0.5-2 parts of antioxidant master batch;
1-5 parts of inorganic filler;
1-8 parts of epoxy resin;
0.1-1 part of curing agent.
The preparation method of the crosslinking master batch comprises the following steps: uniformly mixing a peroxide crosslinking agent, a crosslinking accelerator and high-density polyethylene according to the mass ratio of (1-10) to (0.01-0.5) to 100, then melting and mixing in a double-pair-roller extruder at the temperature of 140-190 ℃, and extruding and granulating.
The peroxide crosslinking agent is selected from at least one of alkyl peroxide, aryl peroxide, acyl peroxide and ketone peroxide; the crosslinking accelerator is selected from at least one of 1,2 polybutadiene, diallyl terephthalate (DATP), Divinylbenzene (DVB), triallyl cyanurate (TAC), triallyl isocyanate (TAIC), and derivatives thereof.
The preparation method of the antioxidant master batch comprises the following steps: uniformly mixing the antioxidant and the high-density polyethylene resin according to the mass ratio of (0.001-0.03):100, then carrying out melt mixing in a pair-roller extrusion at the temperature of 140-; the antioxidant is at least one of an antioxidant 1010, an antioxidant 168 or dioctadecyl thiodipropionate.
The inorganic filler comprises at least one of graphite powder, talcum powder, carborundum and quartz powder.
The epoxy resin is thermoplastic solid powder.
The curing agent is a hidden curing agent, namely the curing reaction temperature is higher than 140 ℃;
the hidden curing agent is an acid anhydride curing agent or an aromatic curing agent;
a preparation method of a high-wear-resistance crosslinked polyethylene material comprises the following steps: uniformly mixing high-density polyethylene resin, low-density polyethylene resin, crosslinking master batch, antioxidant master batch, epoxy resin, curing agent and inorganic filler according to a certain mass ratio, melting and blending the mixture in a double-screw extruder or an internal mixer at 140-190 ℃ and 90-120rpm, and extruding and granulating; pressing the prepared polyethylene material in a tabletting machine with the temperature of 210-; cooling to obtain the final product.
The material has the advantages of simple preparation method, realization of industrial production and continuous supply of raw materials, good wear resistance, good adhesive property, excellent mechanical property, flat surface of a coating layer, and no bubbles or defects.
The beneficial technical effects of the invention are as follows:
(1) the cross-linking agent is introduced into the polyethylene resin system to form a cross-linking system, the cross-linked polyethylene material has high wear resistance, and the requirement for improving the wear resistance of the material can be met only by adding a small amount of high-performance binder on the basis.
(2) The preparation method provided by the application is simple, the types of auxiliary agents required to be added are few, the industrial foundation is firm, and the industrialization and the industrial popularization are easier to realize.
Detailed Description
In the following examples, the performance testing methods involved are as follows:
1. wear rate testing
The wear rate of the crosslinked polyethylene product was determined according to GB5478-85 by the following test method: the pressed sheet was cut to a size of 100mm X100 mm, a hole of 6.5mm diameter was made in the center of the sheet, and the weight was measured and designated M1(ii) a Slowly putting down the grinding wheel and the dust collector, continuously operating each sample for 1000 revolutions, and controlling the rotating speed of the grinding wheel to be 60 r/min; after the operation is stopped, wiping off powder impurities by using a cleaning cloth, and weighing the mass M of the sample2(ii) a Mass wear Mr-M1-M2. Not less than 5 samples per group.
2. Flexural Strength test
The flexural strength of the steel is measured according to GB/T9341-2000, and the test method is as follows: cutting the plate into a strip with the length of 80mm and the width of 10mm, and measuring the width and the thickness of the middle part of the sample; adjusting the span L to be 60mm, and setting the test speed to be 2 mm/min; the test specimen is placed symmetrically on two supports and a force is applied to the center of the span. Finally, reading the bending stress and the bending modulus value.
3. Impact strength test
The impact strength was tested according to GB/T1043-93, the test method is as follows: cutting the plate into a strip with the length of 80mm and the width of 10mm, and measuring the width and the thickness of the middle part of the sample; the pendulum is selected according to the energy required to try to break, and the pendulum is released gently, reading the impact energy from the dial. Not less than 10 samples per group.
4. Shore hardness test
According to the standard of Shore hardness test of GB/T2411-1980, the test method is as follows: the sample is placed on the sample platform of the test stand with the tip of the needle at least 12mm from the edge of the sample, and the durometer is pressed against the sample smoothly and without impact by a set weight and immediately after 15 seconds of full contact with the sample from the lower platen. If instantaneous readings are specified, the lower platen reads within 1 second of full contact with the sample. Not less than 5 samples per group.
Examples 1 to 4:
HDPE I8007 (melt index 8.2g/10min, density 0.965g/cm3) is available from the Mount Cantonia petrochemical company.
HDPE II 2911 (melt index 20g/10min, density 0.960g/cm3) was supplied by the King-Korea company.
LLDPE 7042 (melt index of 2g/10min, density of 0.924g/cm3) is supplied by Shenhua corporation.
Preparing a crosslinking master batch: the peroxide crosslinking agent is di-tert-butyl peroxide; the crosslinking accelerator is triacrylate isocyanurate (TAIC), the high-density polyethylene resin is HDPE I8007, and the mass ratio of the three is 10:0.1: 100; after being uniformly mixed, the mixture is put into a pair roller extruder at 140 ℃ for melt mixing, and then is extruded and granulated.
Preparing an antioxidant master batch: antioxidant 1010 and high density polyethylene 8007 are mixed uniformly, put into a pair roller extruder at 140 ℃ for uniform mixing, and extruded and granulated.
The epoxy resin is pure thermoplastic epoxy resin powder E-15; the curing agent is adipic acid dihydrazide; the inorganic filler is 120-mesh quartz sand.
Taking high-density polyethylene II with certain mass, low-density polyethylene, crosslinking master batch, antioxidant master batch, thermoplastic epoxy resin powder, curing agent and quartz sand, uniformly mixing the materials, putting the materials into a double-screw extruder at the temperature of 140 ℃ and the rotating speed of 120rpm to extrude to prepare the high-cohesiveness crosslinking polyethylene composition of the embodiment 1-4, then cutting and granulating the high-cohesiveness crosslinking polyethylene composition, and grinding the high-cohesiveness crosslinking polyethylene composition into powder by a plastic mill, wherein the specific types and the content of various components are shown in Table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | |
| HDPE II 2911 | 100 | 120 | 110 | 120 |
| LLDPE 7042 | 30 | 25 | 15 | 28 |
| Cross-linking masterbatch | 30 | 28 | 22 | 21 |
| Antioxidant master batch | 2 | 0.6 | 0.4 | 2 |
| Epoxy resin | 5 | 8 | 6 | 7 |
| Curing agent | 0.5 | 0.8 | 0.6 | 0.7 |
| Inorganic filler | 3 | 2 | 1 | 4 |
Placing the prepared high-wear-resistance crosslinked polyethylene powder in a grinding tool with the thickness of about 4mm, pressing for 30min in a tablet press with the temperature of 220 ℃ and the pressure of 100MPa, then cooling to 60 ℃ for 10min, and taking out the plate after pressure relief; and cooling to obtain a plate with the thickness of about 4mm, measuring the wear resistance rate of the crosslinked polyethylene material according to GB5478-85, measuring the bending strength according to GB/T9341-2000 and measuring the impact strength according to GB/T1043-93, wherein the test results are shown in Table 2.
TABLE 2
Comparative examples 1 to 4:
HDPE I8007 (melt index 8.2g/10min, density 0.965 g/cm)3) Supplied by the Chinese petrochemical Mount roller Co
HDPEII 2911 (melt index 20g/10min, density 0.960 g/cm)3) Supplied by the well-petrochemical monster company.
LLDPE 7042 (melt index of 2g/10min, density of 0.924 g/cm)3) Supplied by Shenhua corporation.
Preparing a crosslinking master batch: the cross-linking agent is di-tert-butyl peroxide; the crosslinking accelerator is triacrylate isocyanurate (TAIC) and HDPE I8007, and the mass ratio of the three is 10:0.1: 100; after being uniformly mixed, the mixture is put into a pair roller extruder at 140 ℃ for melt mixing, and then is extruded and granulated.
Preparing an antioxidant master batch: antioxidant 1010 and high density polyethylene 8007 are mixed uniformly, put into a pair roller extruder at 140 ℃ for uniform mixing, and extruded and granulated.
Taking a certain mass of high-density polyethylene II, low-density polyethylene, a cross-linked master batch, an antioxidant master batch, thermoplastic epoxy resin powder E-15, a curing agent adipic dihydrazide and quartz sand, uniformly mixing the above materials, putting the mixture into a twin-screw extruder with the temperature of 140 ℃ and the rotating speed of 120rpm to extrude and prepare the high-cohesiveness cross-linked polyethylene composition of the comparative examples 1 to 4, then cutting and granulating the mixture, and grinding the mixture into powder by a plastic mill. The specific types and amounts of the various components are shown in table 3.
TABLE 3
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| HDPEII 2911 | 100 | 120 | 110 | 120 |
| LLDPE 7042 | 30 | 25 | 15 | 28 |
| Cross-linking masterbatch | 30 | 28 | 22 | 21 |
| Antioxidant master batch | 2 | 0.6 | 0.4 | 2 |
| Epoxy resin | -- | 8 | -- | -- |
| Curing agent | 0.5 | -- | -- | -- |
| Inorganic filler | 3 | 2 | 1 | -- |
Placing the prepared high-wear-resistance crosslinked polyethylene powder in a grinding tool with the thickness of about 4mm, pressing for 30min in a tablet press with the temperature of 220 ℃ and the pressure of 100MPa, then cooling to 60 ℃ for 10min, and taking out the plate after pressure relief; cooling to obtain a plate with the thickness of about 4 mm. The abrasion resistance of the crosslinked polyethylene material was measured according to GB5478-85, the flexural strength thereof was measured according to GB/T9341-2000 and the impact strength was measured according to GB/T1043-93, the results of which are shown in Table 4.
TABLE 4
| Rate of wear/%) | hardness/A | Impact Strength/kJ/mm2 | Flexural Strength/MPa | |
| Comparative example 1 | 0.124 | 97 | 53.44 | 430.27 |
| Comparative example 2 | 0.855 | 91 | 60.90 | 394.63 |
| Comparative example 3 | 0.424 | 90.5 | 53.44 | 375.15 |
| Comparative example 4 | 0.895 | 82 | 48.46 | 425.44 |
As can be seen from the comparison of the data listed in tables 2 and 4, the crosslinked polyethylene material protected by the present application has good wear resistance and excellent mechanical properties.
Those of ordinary skill in the art will understand that: the invention is not to be considered as limited to the specific embodiments thereof, but is to be understood as being modified in all respects, all changes and equivalents that come within the spirit and scope of the invention.
Claims (4)
1. The high-wear-resistance crosslinked polyethylene material is characterized by comprising the following components in parts by weight:
100 portions and 120 portions of high-density polyethylene;
15-30 parts of low-density polyethylene;
20-30 parts of a crosslinking master batch;
0.5-2 parts of antioxidant master batch;
1-5 parts of inorganic filler;
1-8 parts of epoxy resin;
0.1-1 part of curing agent;
the preparation method of the crosslinking master batch comprises the following steps: uniformly mixing a peroxide crosslinking agent, a crosslinking accelerator and high-density polyethylene according to a mass ratio of 1-10:0.01-0.5:100, then melting and mixing in a double-pair-roller extruder at the temperature of 140-;
the preparation method of the antioxidant master batch comprises the following steps: uniformly mixing the antioxidant and the high-density polyethylene resin according to the mass ratio of 0.001-0.03:100, then carrying out melt mixing in pair-roller extrusion at the temperature of 140-;
the peroxide crosslinking agent is at least one of alkyl peroxide, aryl peroxide, acyl peroxide and ketone peroxide; the crosslinking accelerator is at least one of 1,2 polybutadiene, diallyl terephthalate, divinylbenzene, triallyl cyanurate, triallyl isocyanate and derivatives thereof; the antioxidant is at least one of an antioxidant 1010, an antioxidant 168 or dioctadecyl thiodipropionate; the inorganic filler is at least one of graphite powder, talcum powder, carborundum and quartz powder; the curing agent is an acid anhydride curing agent or an aromatic curing agent.
2. The high abrasion resistant crosslinked polyethylene material of claim 1, wherein said epoxy resin is a thermoplastic solid powder.
3. The high abrasion resistant crosslinked polyethylene material of claim 1 wherein said curing agent has a curing reaction temperature greater than 140 ℃.
4. The preparation method of the high wear-resistant crosslinked polyethylene material according to any one of claims 1 to 3, characterized in that the high density polyethylene resin, the low density polyethylene resin, the crosslinking master batch, the antioxidant master batch, the epoxy resin, the curing agent and the inorganic filler are uniformly mixed according to a certain mass ratio, the mixture is melted and blended in a double screw extruder or an internal mixer under the conditions of 140-190 ℃ and 90-120rpm, and extruded and granulated; pressing the prepared polyethylene material in a tabletting machine with the temperature of 210-; cooling to obtain the final product.
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| JPS54161643A (en) * | 1978-06-13 | 1979-12-21 | Hitachi Ltd | Coating composition for friction material |
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| CN102061030A (en) * | 2010-12-10 | 2011-05-18 | 南京聚隆科技股份有限公司 | High-abrasion-resistant corrosion-resistant inorganic particle crosslinking polyethylene composite material and preparation method thereof |
| CN108485023A (en) * | 2018-02-06 | 2018-09-04 | 山东大正新材料科技股份有限公司 | A kind of polythene material and preparation method thereof and product |
| CN110408111A (en) * | 2018-04-27 | 2019-11-05 | 吴飞 | A kind of heatproof heat-resistant halogen-free flame-retardant environment-friendly cable material |
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