CN115703904A - High-heat-resistance polyethylene pipe composition and preparation method thereof - Google Patents
High-heat-resistance polyethylene pipe composition and preparation method thereof Download PDFInfo
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- CN115703904A CN115703904A CN202110907918.4A CN202110907918A CN115703904A CN 115703904 A CN115703904 A CN 115703904A CN 202110907918 A CN202110907918 A CN 202110907918A CN 115703904 A CN115703904 A CN 115703904A
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Abstract
A high heat-resistant polyethylene pipe composition comprises the following components: ultrahigh molecular weight polyethylene, high density polyethylene, polyvinylidene fluoride, a compatilizer A, a compatilizer B and an antioxidant; the compatilizer A is fluorinated polystyrene, and the compatilizer B is chlorinated polyethylene with low chlorine content; and the compatibilizer A is added in the form of a solution of the compatibilizer A during the preparation of the high heat resistant polyethylene pipe composition. In the composition, the ultrahigh molecular weight polyethylene and the high density polyethylene are used as base resin, the polyvinylidene fluoride is used as a processing aid for reducing the processing temperature and improving the processing performance, the compatibility of the polyethylene and the polyvinylidene fluoride is enhanced under the action of the composite compatilizer, and the Vicat softening temperature of the pipe composition is greatly improved under the synergistic effect of the materials.
Description
Technical Field
The invention belongs to the field of processing and application of high polymer materials, and particularly relates to a high heat-resistant polyethylene pipe composition and a preparation method thereof.
Background
Polyethylene (PE) is a thermoplastic with excellent properties and is widely used. However, the polyethylene has low use temperature and low mechanical strength, and cannot be used at higher temperature for a long time, which limits the application in many fields.
In the field of steel pipe lining plastic pipes, the Vicat softening temperature of a polyethylene pipe is required to be above 130 ℃, some of the polyethylene pipes even reach 140 ℃, and meanwhile, the polyethylene pipe is required to have higher tensile strength and elongation at break.
The data show that the vicat softening temperature of the ultra-high molecular weight polyethylene is about 131 ℃ (A50) (mold pressing sample preparation), but the processing of the ultra-high molecular weight polyethylene is extremely difficult, part of common polyethylene needs to be added for modification, the vicat softening temperature is reduced because the extrusion pressure is lower than the pressure of mold pressing when the ultra-high molecular weight polyethylene is extruded into a pipe, and the heat-resistant temperature is reduced because small molecular weight additives need to be added in the processing process, so the vicat softening point of the extruded PE pipe is only 127-128 ℃.
Although the Vicat softening temperature can be improved by crosslinking, the creep resistance and the wear resistance of the polyethylene material after crosslinking modification are reduced, and the service life is shortened.
There are also data showing that the glass beads can increase the vicat softening point temperature of PE, but the addition of glass beads not only reduces the material properties, but also makes the processability worse.
Therefore, a new high heat resistant polyethylene pipe composition and a preparation method thereof are needed to solve the above technical problems.
Disclosure of Invention
The invention provides a high heat-resistant polyethylene pipe composition which comprises the following components in parts by weight:
wherein the molecular weight of the ultra-high molecular weight polyethylene is more than 150 ten thousand.
Wherein the density of the high density polyethylene>0.950g/cm 3 。
The molecular weight of the polyvinylidene fluoride is 40-50 ten thousand, and the polyvinylidene fluoride can be purchased from the Fuwanhao fluorine chemical company Limited in Sanyu.
The compatilizer A is fluorinated polystyrene which is fluorine-containing polystyrene particles synthesized by reaction under certain conditions, and the specific preparation method comprises the following steps:
(i) Adding 7.5 g of polyvinylpyrrolidone, 108 ml of absolute ethyl alcohol and 72 ml of water into a three-neck flask provided with a mechanical stirring pipe, a condensation pipe and a nitrogen inlet and outlet, uniformly stirring, putting into a constant-temperature water area at about 70 ℃, then adding 20 g of styrene and dodecafluoroheptyl methacrylate (wherein, the mol percentage of the styrene to the dodecafluoroheptyl methacrylate is 0.3, 1.0) and 0.3 g of azobisisobutyronitrile into the mixture, stirring and reacting for 10 hours, cooling, centrifugally separating the emulsion at the rotating speed of 5000 r/min, adding absolute ethyl alcohol after separation, performing ultrasonic dispersion and centrifugal separation to remove unreacted monomers and initiators, and drying the final product in a vacuum oven at 60 ℃ for 12 hours to obtain white fluorinated polystyrene powder with the particle size of 0.4-1.0 micron;
(ii) The fluorinated polystyrene white powder is dissolved in dimethylformamide according to the weight ratio of 0.8-1.2 (preferably 1.
Wherein, in the preparation process of the high heat resistant polyethylene pipe composition, the compatilizer A is added in the form of a solution of the compatilizer A, and the solution of the compatilizer A is a solution obtained by dissolving fluorinated polystyrene powder in dimethylformamide according to the weight ratio of 0.8-1.2 (preferably 1).
Wherein the compatilizer B is chlorinated polyethylene with low chlorine content and chlorine content of 5-9 wt%.
Wherein the antioxidant is a mixture of hindered phenol and phosphite antioxidant, and the mixing weight ratio is 1; preferably a mixture of hindered phenols 1010 and phosphites 168.
The invention also provides a preparation method of the high heat-resistant polyethylene pipe composition, which comprises the following steps:
(1) Firstly, weighing polyvinylidene fluoride and a solution of a compatilizer A according to a formula ratio, putting the polyvinylidene fluoride and the solution of the compatilizer A into a high-speed mixer, and mixing, wherein the solution of the compatilizer A contains 5-15 parts by weight of the compatilizer A;
(2) And weighing high-density polyethylene, ultrahigh molecular weight polyethylene, a compatilizer B and an antioxidant according to a proportion, adding the weighed materials into a high-speed mixer, mixing, fully mixing and absorbing all the components of the materials after the solvent is completely volatilized, and then discharging the materials to obtain the high-heat-resistant polyethylene pipe composition.
Wherein, in the step (1), the mixing time is 2-3 minutes.
Wherein in the step (2), the mixing temperature is 100 +/-5 ℃, and the mixing time is 3-5 minutes.
The invention also provides a pipe prepared from the high heat-resistant polyethylene pipe composition.
Wherein the specification of the pipe is phi 63 multiplied by 4mm.
The invention also provides a preparation method of the pipe, which comprises the following steps: and extruding and molding the high heat-resistant polyethylene pipe composition to obtain the pipe.
Wherein the extrusion molding is: the high heat-resistant polyethylene pipe composition is put on a single-screw pipe extrusion device to extrude a pipe, wherein the temperature of a charging barrel is 240-280 ℃, the rotating speed of a screw is 20-30 r/min, and the traction speed is 0.5-0.8 m/min.
The invention has the following beneficial technical effects:
according to the invention, the ultrahigh molecular weight polyethylene and the high density polyethylene are used as base resins, the polyvinylidene fluoride (PVDF) is used as a processing aid for reducing the processing temperature and improving the processing performance, the compatibility of the polyethylene and the polyvinylidene fluoride is greatly enhanced under the action of the composite compatilizer, and the Vicat softening temperature of the pipe composition is greatly increased under the synergistic effect of the polyethylene and the PVDF. Specifically, the method comprises the following steps:
(1) The pipe material composition adopts ultra-high molecular weight polyethylene and high density polyethylene as base resins, polyvinylidene fluoride (PVDF) is added as a processing aid for reducing processing temperature and improving processing performance, under the combined action of a compatilizer A and a compatilizer B, due to combination of fluorine and chlorine, the interfacial adhesion between the polyvinylidene fluoride and the polyethylene is greatly enhanced, meanwhile, the high temperature resistance of the composition is greatly improved, the compatilizer A also assists in improving the heat resistance of the composition, and the Vicat softening temperature of the pipe material composition is synergistically improved.
(2) The polyvinylidene fluoride is used as a processing aid, and not only can play a role in promoting the plasticization of the composition, but also can play a role in improving the high-temperature resistance of the composition.
(3) In the step (2) of the preparation method of the polyethylene pipe composition, the high-temperature mixing at about 100 ℃ is beneficial to the sufficient absorption, fusion and dispersion of the compatilizer and the auxiliary agent, and the dimethyl formamide solvent in the solution of the compatilizer A can be volatilized at the mixing temperature of about 100 ℃.
(4) The compatilizer A is added in the form of solution, which is favorable for the compatilizer A to be fully dispersed in the composition, so that the composition has better uniformity and compatibility.
(5) The compatilizer A and the compatilizer B play a role in interface bonding and fusion between polyvinylidene fluoride and polyethylene, and therefore the chlorinated polyethylene with low chlorine content is adopted as the compatilizer B, because the chlorinated polyethylene with low chlorine content not only keeps the heat property of polyethylene plastics, but also has better compatibility between chlorine and fluorine-containing polymer, so that the good effect of the compatilizer is achieved, and the Vicat softening point is not reduced. If the chlorine content is too high (15-60% chlorine), the material becomes an elastomer and the Vicat softening temperature is lowered, and if the chlorine content exceeds 70%, the chlorinated polyethylene becomes brittle and the impact properties and elongation of the composition are reduced.
(6) The pipe extruded by the composition prepared by the invention has smooth surface, good processing performance, high temperature resistance, higher Vicat softening point and tensile strength.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following table 1 shows the formulation of an example of the invention, in which:
the high density polyethylene has a density of 0.955g/cm 3 ；
The molecular weight of the ultra-high molecular weight polyethylene is 150 ten thousand;
the molecular weight of the polyvinylidene fluoride is 45 ten thousand;
the compatilizer A is added in the form of fluorinated styrene solution, i.e. fluorinated styrene white powder with the grain diameter of 1 micron is dissolved in dimethylformamide to prepare 1:1 (part by weight) solution, that is, 10 parts by weight solution containing fluorinated polystyrene 5 parts by weight;
the compatilizer B is low-chlorine content chlorinated polyethylene with chlorine content of 7.5 weight percent.
TABLE 1 formulation of the inventive examples
The preparation of the examples is as follows:
(1) Firstly, weighing polyvinylidene fluoride and fluorinated polystyrene solution according to a proportion, and putting the solution into a high-speed mixer for mixing for 2-3 minutes.
(2) And weighing high-density polyethylene, ultrahigh molecular weight polyethylene, chlorinated polyethylene and an antioxidant according to a proportion, adding the mixture into a mixer, mixing at a high speed for 3-5 minutes at the mixing temperature of 100 +/-5 ℃, fully mixing and absorbing all the components of the material after the solvent is completely volatilized, and then discharging the material to obtain the high heat-resistant polyethylene pipe composition.
(3) The mixed composition is directly put into single-screw pipe extrusion equipment to extrude a pipe, the specification of the pipe is phi 63 multiplied by 4, the temperature of a charging barrel is 240-280 ℃, the rotating speed of a screw is 30 r/min, and the traction speed is 0.6 m/min.
The following table 2 shows the formulation of the comparative example of the present invention, in which:
comparative example 1 compared with example 3, polyvinylidene fluoride was replaced with treated silicate, and the remaining components were the same;
compared with the embodiment 3, the comparative example 2 adopts the same part of polyethylene grafted maleic anhydride to replace fluorinated polystyrene, and the rest components are the same;
comparative example 3 compared with example 3, chlorinated polyethylene with a chlorine content of 50 wt% was used, and the remaining components were the same;
comparative example 4 compared with example 3, chlorinated polyethylene with a chlorine content of 71 wt% was used, and the remaining components were the same;
comparative example 5 compared with example 3, only chlorinated polyethylene (chlorine content 7.5 wt%) was used as a compatibilizer, and the remaining components were the same;
comparative example 6 compared with example 3, fluorinated polystyrene alone was used as a compatibilizer and the remaining components were the same.
TABLE 2 formulation of the comparative examples
The comparative example was prepared as follows:
(1) The components are weighed according to the proportion and put into a high-speed mixer for mixing for 5 minutes, and then the materials are discharged.
(2) The mixed composition is directly put into single-screw pipe extrusion equipment to extrude a pipe, the specification of the pipe is phi 63 multiplied by 4, the temperature of a charging barrel is 240-280 ℃, the rotating speed of a screw is 30 r/min, and the traction speed is 0.6 m/min.
Performance test
The results of the performance tests of the above examples and comparative examples are shown in tables 3 and 4 below.
Table 3 results of performance testing of examples
Table 4 comparative example performance test results
From the performance test results, the performance of the examples is better than that of the comparative example, particularly the Vicat softening temperature is reduced more than that of the comparative example. In the comparative example 4, the pipe is brittle and the elongation at break is reduced due to the adoption of the chlorinated polyethylene with extremely high chlorine content; in comparative examples 5 and 6, since a single compatibilizer was used, the compatibility was inferior to the effect of using two compatibilizers in combination, and both of the pipes had problems of a lower vicat softening temperature and a lower elongation at break.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A high heat-resistant polyethylene pipe composition comprises the following components in parts by weight:
wherein the compatilizer A is fluorinated polystyrene, and the compatilizer B is chlorinated polyethylene with low chlorine content and chlorine content of 5-9 wt%;
wherein, in the preparation process of the high heat resistant polyethylene pipe composition, the compatilizer A is added in the form of a solution of the compatilizer A, and the solution of the compatilizer A is a solution obtained by dissolving fluorinated polystyrene in dimethylformamide according to the weight ratio of 0.8-1.2.
2. The polyethylene pipe composition according to claim 1, wherein the polyvinylidene fluoride has a molecular weight of 40 to 50 ten thousand.
3. The polyethylene pipe composition according to claim 1, wherein the ultra high molecular weight polyethylene has a molecular weight of 150 ten thousand or more.
4. The polyethylene pipe composition according to claim 1, wherein the high density polyethylene has a density>0.950g/cm 3 。
5. The polyethylene pipe composition according to claim 1, wherein the antioxidant is a mixture of hindered phenol and phosphite antioxidants, and the mixing weight ratio of the hindered phenol and phosphite antioxidants is 1.
6. Process for the preparation of a polyethylene pipe composition according to claims 1-5 comprising:
(1) Firstly, weighing polyvinylidene fluoride and a solution of a compatilizer A according to a formula ratio, and putting the polyvinylidene fluoride and the solution of the compatilizer A into a high-speed mixer for mixing, wherein the solution of the compatilizer A contains 5-15 parts by weight of the compatilizer A;
(2) And weighing high-density polyethylene, ultrahigh molecular weight polyethylene, a compatilizer B and an antioxidant according to a proportion, adding the weighed materials into a high-speed mixer, mixing, fully mixing and absorbing all the components of the materials after the solvent is completely volatilized, and then discharging the materials to obtain the high-heat-resistant polyethylene pipe composition.
7. The method for preparing the polyethylene pipe composition according to claim 6, wherein the mixing temperature in the step (2) is 100 ± 5 ℃ and the mixing time is 3 to 5 minutes.
8. A pipe prepared from the high heat resistant polyethylene pipe composition according to any one of claims 1 to 5.
9. The method of making the pipe of claim 8, comprising: the high heat resistant polyethylene pipe composition according to any one of claims 1 to 5, which is extrusion molded to obtain the pipe.
10. The method for producing a pipe according to claim 8 or 9, wherein the high heat resistant polyethylene pipe composition according to any one of claims 1 to 5 is fed to a single screw pipe extrusion apparatus to extrude a pipe.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116515190A (en) * | 2023-05-29 | 2023-08-01 | 江苏众成复合材料有限责任公司 | Ageing-resistant low-migration polyethylene pipe and preparation method thereof |
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| CN102382344A (en) * | 2010-09-01 | 2012-03-21 | 中国石油化工股份有限公司 | Composition for preparing polyethylene pipe with superhigh molecular weight and preparation method thereof |
| CN103524861A (en) * | 2012-07-05 | 2014-01-22 | 中国石油化工股份有限公司 | High-temperature and high-pressure resistant polyethylene composition as well as preparation method thereof |
| CN107964182A (en) * | 2016-10-19 | 2018-04-27 | 顾地科技股份有限公司 | A kind of high temperature resistant, anti-impact PVC modified materials |
| CN112521674A (en) * | 2020-11-24 | 2021-03-19 | 胜利新大新材料股份有限公司 | High-temperature-resistant ultrahigh molecular weight polyethylene composite material, pipe and preparation method thereof |
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- 2021-08-09 CN CN202110907918.4A patent/CN115703904A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102382344A (en) * | 2010-09-01 | 2012-03-21 | 中国石油化工股份有限公司 | Composition for preparing polyethylene pipe with superhigh molecular weight and preparation method thereof |
| CN103524861A (en) * | 2012-07-05 | 2014-01-22 | 中国石油化工股份有限公司 | High-temperature and high-pressure resistant polyethylene composition as well as preparation method thereof |
| CN107964182A (en) * | 2016-10-19 | 2018-04-27 | 顾地科技股份有限公司 | A kind of high temperature resistant, anti-impact PVC modified materials |
| CN112521674A (en) * | 2020-11-24 | 2021-03-19 | 胜利新大新材料股份有限公司 | High-temperature-resistant ultrahigh molecular weight polyethylene composite material, pipe and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116515190A (en) * | 2023-05-29 | 2023-08-01 | 江苏众成复合材料有限责任公司 | Ageing-resistant low-migration polyethylene pipe and preparation method thereof |
| CN116515190B (en) * | 2023-05-29 | 2024-03-08 | 重庆维斯顿实业有限公司 | Ageing-resistant low-migration polyethylene pipe and preparation method thereof |
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