CN116162301A - Reinforced polyethylene pipe and production method thereof - Google Patents
Reinforced polyethylene pipe and production method thereof Download PDFInfo
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- CN116162301A CN116162301A CN202211695971.3A CN202211695971A CN116162301A CN 116162301 A CN116162301 A CN 116162301A CN 202211695971 A CN202211695971 A CN 202211695971A CN 116162301 A CN116162301 A CN 116162301A
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- -1 polyethylene Polymers 0.000 title claims abstract description 60
- 239000004698 Polyethylene Substances 0.000 title claims abstract description 47
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 73
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000010445 mica Substances 0.000 claims abstract description 44
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 44
- 239000011787 zinc oxide Substances 0.000 claims abstract description 31
- 229920001903 high density polyethylene Polymers 0.000 claims abstract description 28
- 239000004700 high-density polyethylene Substances 0.000 claims abstract description 28
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 21
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 239000004593 Epoxy Substances 0.000 claims abstract description 13
- 239000000806 elastomer Substances 0.000 claims abstract description 11
- 229920001971 elastomer Polymers 0.000 claims abstract description 11
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- XBICPFKOMKSLJI-UHFFFAOYSA-N trimethyl (3-propyloxiran-2-yl)methyl silicate Chemical compound C(CC)C1C(CO[Si](OC)(OC)OC)O1 XBICPFKOMKSLJI-UHFFFAOYSA-N 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 239000003495 polar organic solvent Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- 239000003063 flame retardant Substances 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000000314 lubricant Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 2
- 239000004599 antimicrobial Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 22
- 238000012546 transfer Methods 0.000 abstract description 4
- 239000012763 reinforcing filler Substances 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000012360 testing method Methods 0.000 description 7
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 125000003700 epoxy group Chemical group 0.000 description 4
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000011256 inorganic filler Substances 0.000 description 4
- 229910003475 inorganic filler Inorganic materials 0.000 description 4
- 125000003545 alkoxy group Chemical group 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000011592 zinc chloride Substances 0.000 description 3
- 235000005074 zinc chloride Nutrition 0.000 description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000003805 vibration mixing Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L23/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2423/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2423/08—Copolymers of ethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses an enhanced polyethylene pipe, which comprises the main components of high-density polyethylene and enhanced master batch according to the mass ratio of (2-4.5): 1, blending to obtain the product; the reinforcing master batch comprises the following main components in parts by weight: 7 parts of high-density polyethylene, 3.5-6 parts of polyethylene octene co-elastomer, 0.2-0.8 part of epoxy silane coupling agent, 0.03-0.09 part of epoxy acrylate monomer, 10-20 parts of mica powder and 20-35 parts of rod-shaped zinc oxide. The reinforced polyethylene pipe adopts two reinforcing fillers of mica powder and rod-shaped zinc oxide to prepare composite powder; the reinforced master batch is prepared by blending the composite powder with the high-density polyethylene and polyethylene octene co-elastomer, and the composite powder of the rod-shaped zinc oxide and mica powder in the composite powder is favorable for load transfer and transfer, so that the strength of the polyethylene composite material is improved to a certain extent. The invention also discloses a production method of the reinforced polyethylene pipe.
Description
Technical Field
The invention relates to the field of water supply and drainage pipeline production, in particular to an enhanced polyethylene pipe and a production method thereof.
Background
The high-density polyethylene drain pipe has the advantages of corrosion resistance, small water flow resistance, light weight and the like, so that the high-density polyethylene drain pipe is widely applied to the fields of municipal engineering drainage, mining drainage, farmland irrigation and the like. However, polyethylene has poor low temperature impact resistance, and a nonpolar polyethylene material has poor compatibility with other materials such as inorganic filler, etc., which limits the applicable range of the high density polyethylene drain pipe.
The improved technical scheme is that a filler is added to strengthen and toughen a pipeline, for example, inorganic filler and a coupling agent are added to high-density polyethylene serving as a base material of a polyethylene composite pipe, wherein the inorganic filler is selected from hollow microspheres, mica, glass fibers and the like, the coupling agent is selected from gamma-aminopropyl triethoxysilane, gamma-aminopropyl triethoxysilane and the like, and the dispersion performance of the inorganic filler in the high-density polyethylene is improved by utilizing the silane coupling agent. How to optimize the distribution of different types of fillers, so that the different types of fillers are compounded and the strength of the pipe is improved complementarily is one of main development directions of the polyethylene filling modified composite material.
Disclosure of Invention
One of the purposes of the invention is to overcome the defects in the prior art and provide an enhanced polyethylene pipe, wherein the silane coupling agent containing epoxy groups and the acrylic ester monomer are introduced into the raw materials to prepare the composite powder of mica and rod-shaped zinc oxide, and the composite powder is beneficial to improving the low-temperature impact resistance of the enhanced polyethylene pipe.
In order to achieve the technical effects, the technical scheme of the invention is as follows: the reinforced polyethylene pipe consists of high density polyethylene and reinforced mother grain in the weight ratio of 2-4.5: 1, blending to obtain the product;
the reinforcing master batch comprises the following main components in parts by mass: 7 parts of high-density polyethylene, 3.5-6 parts of polyethylene octene co-elastomer, 0.2-0.8 part of epoxy silane coupling agent, 0.03-0.09 part of epoxy acrylate monomer, 10-20 parts of mica powder and 20-35 parts of rod-shaped zinc oxide.
Further, the mass ratio of the high-density polyethylene to the reinforcing master batch is (2.4-4): 1, a step of; the main composition of the reinforced master batch is as follows: 7 parts of high-density polyethylene, 4-6 parts of polyethylene octene co-elastomer, 0.45-0.7 part of epoxy silane coupling agent, 0.04-0.07 part of epoxy acrylate monomer, 12-18 parts of mica powder and 24-32 parts of rod-shaped zinc oxide.
The preferable technical proposal is that the particle size of the mica powder is 10-200 mu m; the diameter of the rod-shaped zinc oxide is 200-400 nm, and the length is 8-10 nm. Further, the particle size of the mica powder is 30 to 100. Mu.m.
The preferable technical scheme is that the epoxy silane coupling agent is formed by combining (3-epoxypropyl propoxy) trimethoxy silane and 2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane, and the mass ratio of the (3-epoxypropyl propoxy) trimethoxy silane to the 2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane is (1.7-2.5): 1. Further, the mass ratio of (3-epoxypropylpropoxy) trimethoxysilane to 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane is (1.9-2.3): 1.
The preferable technical scheme is that the reinforced master batch further comprises at least one of a lubricant, an antioxidant, a flame retardant and an antibacterial agent.
The second object of the present invention is to provide a method for producing reinforced polyethylene pipe, based on the reinforced polyethylene pipe, comprising the following steps:
s1: dispersing mica powder in a mixed solution of a water-soluble polar organic solvent and an organic acid, adding an epoxy acrylate monomer under the protection of ultrasonic oscillation and inert gas, heating to 80-100 ℃ for reacting for at least 5 hours, cooling to room temperature, filtering out the mica powder, cleaning and drying to constant weight to obtain pretreated mica powder;
s2: dispersing rod-shaped zinc oxide in an alcohol solution of an epoxy silane coupling agent, carrying out ultrasonic oscillation, mixing and heating to 50-80 ℃ for reaction for at least 30min, cooling to room temperature, adding S1 pretreatment mica powder and deionized water into a reaction system, regulating pH to 5.5-6.5, carrying out heating reaction for 0.5-1 h, cooling, filtering out powder, drying to constant weight, crushing and sieving to obtain modified powder;
s3: and (3) blending and drying the modified powder of the S2 and the high-density polyethylene and polyethylene octene co-elastomer in proportion, and carrying out melt extrusion and pelleting by a double-screw extruder to obtain the reinforced master batch.
S4: and (3) feeding the reinforced master batch of the S3 and the high-density polyethylene into a pipe extruder, and obtaining the reinforced polyethylene pipe through melt extrusion, cooling, traction and cutting.
The preferable technical proposal is that the mass concentration of solute in the epoxy silane coupling agent solution in S2 is 1 percent to 2 percent.
The preferable technical proposal is that the pretreated mica powder in S2 is added into a reaction system and then heated to 45-55 ℃. The temperature of the reaction system is further raised to 50-55 ℃.
The preferable technical proposal is that the solvent of the epoxy silane coupling agent is isopropanol; the addition amount of deionized water in S2 is 4-10% of the volume of the solvent. Further, the addition amount of deionized water in S2 is 5-8% of the mass of the solvent.
The preferable technical proposal is that the volume ratio of the S1 water-soluble polar organic solvent to the organic acid is (15-25) 1, and the volume ratio of the mass of the mica powder to the mixed solution is 1.5-2.5 g/10ml. The volume ratio of the water-soluble polar organic solvent to the organic acid of the S1 is (18-22): 1.
Further, the water-soluble polar organic solvent is N, N-dimethylformamide, and the organic acid is acetic acid.
The preferable technical proposal is that the temperature of the conveying section of the double screw extruder in S4 is 100-170 ℃ and the temperature of the melting section is 170-190 ℃; the temperature of the homogenizing section is 190-220 ℃.
The invention has the advantages and beneficial effects that:
the reinforced polyethylene pipe adopts two reinforcing fillers of mica powder and rod-shaped zinc oxide, wherein the mica powder has a two-dimensional lamellar structure, the rod-shaped zinc oxide has a short rod structure, and the mica powder and the rod-shaped zinc oxide are treated by using a silane coupling agent containing epoxy groups and an acrylic ester monomer to prepare composite powder;
the reinforced master batch is prepared by blending the composite powder with the high-density polyethylene and polyethylene octene co-elastomer, and the interaction of the rod-shaped zinc oxide in the composite powder and the mica powder is beneficial to load transmission and transfer, so that the strength of the polyethylene composite material is improved to a certain extent, and the strength and low-temperature impact resistance of the high-density polyethylene pipe are improved.
Detailed Description
The following describes the invention in further detail with reference to examples. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
The main components of the reinforced polyethylene pipe are obtained by blending high-density polyethylene and reinforced master batches, and besides the main components, the reinforced polyethylene pipe also comprises auxiliary agents such as a lubricant, an antioxidant, a flame retardant, an antibacterial agent and the like, namely the auxiliary agents can be directly added into extrusion inlet materials of the polyethylene pipe or added into the reinforced master batches. In comparison, the addition of the above additives to the reinforcing masterbatch is more advantageous for the uniform distribution of the additives in the tubing.
The epoxy acrylate monomer is selected from at least one of glycidyl acrylate and glycidyl acrylate.
The high density polyethylene, (3-epoxypropylpropoxy) trimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyl trimethoxysilane, glycidyl methacrylate and the like used in the following examples are all commercially available, and the medicines used for preparing the composite powder of N, N-dimethylformamide, isopropanol, acetic acid, sodium hydroxide, zinc chloride, isopropanol and the like are all commercially analytically pure;
mica powder: 270 meshes, and the diameter-thickness ratio is 30-50 (corresponding to the particle size of 53 μm);
rod-shaped zinc oxide: self-making by adopting a direct precipitation method, wherein the molar ratio of the solute in the zinc chloride solution to the solute in the sodium hydroxide solution is 1:10, dropwise adding the zinc chloride solution into the sodium hydroxide solution, fully stirring, placing the mixed solution in an oven at 80 ℃ for 24 hours, filtering, washing and filtering the obtained solid, centrifuging and drying; the rod-shaped zinc oxide has the diameter of 200-400 nm and the length of 8-10 nm.
Example 1
Preparation of modified powder
S1: dropwise adding acetic acid into N, N-dimethylformamide, wherein the volume ratio of the N, N-dimethylformamide to the acetic acid is 20:1; dispersing 15 parts of mica powder in a mixed solution according to a mass-volume ratio of 2g/10ml, adding 0.06 part of glycidyl methacrylate monomer under the protection of ultrasonic vibration and inert gas, heating to 90 ℃ for reaction for 8 hours, cooling to room temperature, filtering the mica powder, cleaning and drying to constant weight, and obtaining pretreated mica powder;
s2: 28 parts of rod-shaped zinc oxide is dispersed in an isopropanol solution containing 0.6 part of (3-epoxypropylpropoxy) trimethoxysilane, and the volume ratio of the mass of the rod-shaped zinc oxide to the isopropanol is 1.67g/10ml; and (3) carrying out ultrasonic vibration mixing and heating to 70 ℃ for reaction for 3 hours, cooling to room temperature, adding 15.06 parts of S1 pretreated mica powder and deionized water into a reaction system, wherein the addition amount of the deionized water is 8% of the volume of isopropanol, regulating the pH to 6 by acetic acid, heating to 50 ℃ for reaction for 1 hour, cooling, filtering out powder, drying to constant weight, crushing and sieving to obtain modified powder.
Preparing reinforced master batch
Mixing and drying 7 parts of high-density polyethylene, 5 parts of polyethylene octene co-elastomer, 43.66 parts of modified powder, 2.735 parts of polyethylene wax and 1.825 parts of antioxidant at a high speed in proportion, and carrying out melt extrusion by a double-screw extruder, wherein the temperature of a conveying section of the double-screw extruder is 100-170 ℃, and the temperature of a melting section is 170-190 ℃; the homogenization section temperature is 190-220 ℃, and the reinforced master batch is obtained after granulating and drying.
Preparation of reinforced polyethylene pipe
The high-density polyethylene and the reinforced master batch are fed into a double-screw extruder according to the mass ratio of 3:1, and the reaction temperature of each section of screw is as follows: 170 ℃, 180 ℃, 190 ℃, 195 ℃, 200 ℃, 210 ℃, 200 ℃, 190 ℃, and cooling to obtain the reinforced polyethylene pipe, and preparing a standard sample by an injection method.
Example 2
S1 of example 2 is the same as example 1;
s2: 28 parts of rod-shaped zinc oxide is dispersed in an isopropanol solution containing 0.4 part of (3-epoxypropylpropoxy) trimethoxysilane and 0.2 part of 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, and the volume ratio of the mass of the rod-shaped zinc oxide to the isopropanol is 1.67g/10ml; mixing by ultrasonic oscillation, heating to 70 ℃ for reaction for 3 hours, cooling to room temperature, adding 15.06 parts of pretreated mica powder of S1 and deionized water into a reaction system, wherein the addition amount of the deionized water is 8% of the volume of isopropanol, regulating the pH to 6 by acetic acid, heating to 50 ℃ for reaction for 1 hour, cooling, filtering out powder, drying to constant weight, crushing and sieving to obtain modified powder;
the modified powder of S2 and the production process of example 1 are used for preparing the reinforced polyethylene pipe standard sample.
Example 3
S1 of example 3 is the same as example 1;
s2: 28 parts of rod-shaped zinc oxide is dispersed in an isopropanol solution containing 0.2 part of (3-epoxypropylpropoxy) trimethoxysilane and 0.4 part of 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, and the volume ratio of the mass of the rod-shaped zinc oxide to the isopropanol is 1.67g/10ml; mixing by ultrasonic oscillation, heating to 70 ℃ for reaction for 3 hours, cooling to room temperature, adding 15.06 parts of pretreated mica powder of S1 and deionized water into a reaction system, wherein the addition amount of the deionized water is 8% of the volume of isopropanol, regulating the pH to 6 by acetic acid, heating to 50 ℃ for reaction for 1 hour, cooling, filtering out powder, drying to constant weight, crushing and sieving to obtain modified powder;
the modified powder of S2 and the production process of example 1 are used for preparing the reinforced polyethylene pipe standard sample.
Example 4
The high-density polyethylene and the reinforced masterbatch of the embodiment 1 are fed into a double-screw extruder according to the mass ratio of 2.5:1, and are subjected to melt extrusion and cooling to obtain a reinforced polyethylene pipe, and the reinforced polyethylene pipe is prepared into a standard sample by an injection method.
Example 5
The amount of S2 deionized water added in example 5 was 12% by volume of isopropyl alcohol, and other process parameters were the same as in example 1.
Comparative example 1
Mixing 187 parts of high-density polyethylene, 5 parts of polyethylene octene co-elastomer, (3-epoxypropyl propoxy) trimethoxy silane 0.6 parts, glycidyl methacrylate 0.06 parts, mica powder 15 parts, rod-shaped zinc oxide 28 parts, polyethylene wax 2.375 parts and antioxidant 1.825 parts at a high speed; based on the extrusion process of example 1, the blend was fed to a twin screw extruder to obtain reinforced polyethylene tubing, which was made into standard samples using an injection method.
Comparative example 2
Mixing 187 parts of high-density polyethylene, 5 parts of polyethylene octene co-elastomer, 0.4 part of (3-epoxypropyl propoxy) trimethoxy silane, 0.2 part of 2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane, 15 parts of mica powder, 28 parts of rod-shaped zinc oxide, 2.375 parts of polyethylene wax and 1.825 parts of antioxidant at a high speed; based on the extrusion process of example 1, the blend was fed to a twin screw extruder to obtain reinforced polyethylene tubing, which was made into standard samples using an injection method.
Detection of a standard sample:
1. determination of tensile Properties of plastics according to GB/T1040.1-2006 part 1: general rules test tensile strength and elongation at break were carried out on standard test specimens, the tensile rate being 50mm/min, and the test results for the test specimens of examples and comparative examples are shown in the following table:
tensile breaking strength/MPa | Elongation at break/% | |
Example 1 | 36.21 | 762 |
Example 2 | 37.38 | 785 |
Example 3 | 34.73 | 743 |
Example 4 | 38.34 | 794 |
Example 5 | 30.95 | 729 |
Comparative example 1 | 27.75 | 707 |
Comparative example 2 | 28.62 | 701 |
2. The impact properties of standard samples were tested according to GB/T1843-2008 "determination of impact Strength of Plastic cantilever", the test results of the samples of examples and comparative examples are shown in the following Table:
impact strength of cantilever beam/KJ/m 2 | |
Example 1 | 37.4 |
Example 2 | 40.1 |
Example 3 | 36.0 |
Example 4 | 42.8 |
Example 5 | 34.3 |
Comparative example 1 | 31.7 |
Comparative example 2 | 30.5 |
The silane coupling agent and filler of comparative examples 1 and 2 were added directly to the pipe feed, wherein example 1 contrasted with comparative example and example 2 contrasted with comparative example 2 (comparative example 2 does not contain glycidyl methacrylate); the result shows that the composite powder prepared by pre-treating the mica powder and the rod-shaped zinc oxide is beneficial to improving the tensile breaking strength, the breaking elongation and the impact strength of the standard sample;
in the preparation process of the mica powder and the rod-shaped zinc oxide composite powder, the epoxy group of the epoxy acrylate monomer is opened and reacts with the hydroxyl on the surface of the mica surface to obtain the epoxy acrylate monomer modified mica powder; the alkoxy of the epoxy silane coupling agent is hydrolyzed into alkoxy, the alkoxy is oriented to the surface of rod-shaped zinc oxide, the hydrolysis polycondensation reaction is carried out with the hydroxyl on the surface of the zinc oxide, the epoxy group at the other end of the epoxy silane coupling agent is oriented to the surface of mica powder modified by epoxy acrylate monomers under the acidic condition, and the epoxy acrylate monomers are oriented to polyethylene, so that the interface between the composite powder and the polyethylene has sufficient adhesive force. The composite powder of the platy mica powder and the rod-shaped zinc oxide filler with different forms is dispersed in the polyethylene base material, and when the application of force to the composite material, the composite powder structure can effectively transfer and disperse load.
Example 1, example 2 and example 3 form a control of the content of 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane; the tensile breaking strength, elongation at break and impact strength of the test pieces of example 2 are superior to those of examples 1 and 3; the steric effect of the cyclohexyl in the 2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane structure is beneficial to improving the uniformity of the distribution of the silane coupling agent modified zinc oxide on the mica surface, but the excessive content of the 2- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane is unfavorable for the compounding of the flaky mica powder and the rod-shaped zinc oxide, so that the reinforcing effect of the compound powder is weakened.
Example 1 and example 4 form a control of the blending ratio of the high density polyethylene and the modified masterbatch, and the test results show that the tensile breaking strength, the elongation at break and the impact resistance of the polyethylene composite material are improved with the content of the modified masterbatch within the preferred ranges.
Example 1 and example 5 form a comparison of the added amount of S2 deionized water, and on the basis of the preferred added amount of deionized water, if the added amount of deionized water is too large, the alcohol content in the reaction system is reduced, silanol condensation is increased under heating conditions, and the generation of composite powder is not facilitated.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the scope of the invention.
Claims (10)
1. The reinforced polyethylene pipe is characterized in that the main components are prepared from high-density polyethylene and reinforced master batches according to the mass ratio of (2-4.5): 1, blending to obtain the product;
the reinforcing master batch comprises the following main components in parts by mass: 7 parts of high-density polyethylene, 3.5-6 parts of polyethylene octene co-elastomer, 0.2-0.8 part of epoxy silane coupling agent, 0.03-0.09 part of epoxy acrylate monomer, 10-20 parts of mica powder and 20-35 parts of rod-shaped zinc oxide.
2. The reinforced polyethylene pipe of claim 1, wherein the mica powder has a particle size of 10 to 200 μm; the diameter of the rod-shaped zinc oxide is 200-400 nm, and the length is 8-10 nm.
3. The reinforced polyethylene pipe according to claim 1, wherein the epoxysilane coupling agent is composed of a combination of (3-epoxypropylpropoxy) trimethoxysilane and 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, and the mass ratio of (3-epoxypropylpropoxy) trimethoxysilane to 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane is (1.7-2.5): 1.
4. The reinforced polyethylene pipe of claim 1, wherein the reinforced masterbatch further comprises at least one of a lubricant, an antioxidant, a flame retardant, and an antimicrobial agent.
5. A method for producing reinforced polyethylene pipe, characterized in that it is based on any one of claims 1 to 4, comprising the steps of:
s1: dispersing mica powder in a mixed solution of a water-soluble polar organic solvent and an organic acid, adding an epoxy acrylate monomer under the protection of ultrasonic oscillation and inert gas, heating to 80-100 ℃ for reacting for at least 5 hours, cooling to room temperature, filtering out the mica powder, cleaning and drying to constant weight to obtain pretreated mica powder;
s2: dispersing rod-shaped zinc oxide in an alcohol solution of an epoxy silane coupling agent, carrying out ultrasonic oscillation, mixing and heating to 50-80 ℃ for reaction for at least 30min, cooling to room temperature, adding S1 pretreatment mica powder and deionized water into a reaction system, regulating pH to 5.5-6.5, carrying out heating reaction for 0.5-1 h, cooling, filtering out powder, drying to constant weight, crushing and sieving to obtain modified powder;
s3: blending and drying the modified powder of the S2 and the high-density polyethylene and polyethylene octene co-elastomer in proportion, and carrying out melt extrusion and pelleting by a double-screw extruder to obtain reinforced master batch;
s4: and (3) feeding the reinforced master batch of the S3 and the high-density polyethylene into a pipe extruder, and obtaining the reinforced polyethylene pipe through melt extrusion, cooling, traction and cutting.
6. The method for producing reinforced polyethylene pipe according to claim 5, wherein the mass concentration of the solute in the epoxy silane coupling agent solution in S2 is 1% to 2%.
7. The method for producing reinforced polyethylene pipe according to claim 5, wherein the pretreated mica powder in S2 is added into the reaction system and then heated to 45-55 ℃.
8. The method for producing reinforced polyethylene pipe according to claim 6, wherein the solvent of the epoxy silane coupling agent is isopropyl alcohol; the addition amount of deionized water in S2 is 4-10% of the volume of the solvent.
9. The method according to claim 5, wherein the volume ratio of the S1 water-soluble polar organic solvent to the organic acid is (15-25): 1, and the volume ratio of the mass of the mica powder to the volume ratio of the mixed solution is 1.5-2.5 g/10ml.
10. The method for producing reinforced polyethylene pipe according to claim 5, wherein the conveying section temperature of the twin-screw extruder in S4 is 100 to 170 ℃ and the melting section temperature is 170 to 190 ℃; the temperature of the homogenizing section is 190-220 ℃.
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