CN113292784A - Formula, preparation method, product and test method of high-rate heat-shrinkable tubing - Google Patents
Formula, preparation method, product and test method of high-rate heat-shrinkable tubing Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000010998 test method Methods 0.000 title claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 69
- 239000002184 metal Substances 0.000 claims abstract description 69
- 238000012360 testing method Methods 0.000 claims abstract description 57
- 238000004132 cross linking Methods 0.000 claims abstract description 23
- 239000000314 lubricant Substances 0.000 claims abstract description 21
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 14
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 12
- -1 polyethylene Polymers 0.000 claims abstract description 11
- 239000004595 color masterbatch Substances 0.000 claims abstract description 9
- 239000004698 Polyethylene Substances 0.000 claims abstract description 8
- 229920000573 polyethylene Polymers 0.000 claims abstract description 8
- 238000010894 electron beam technology Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 230000005251 gamma ray Effects 0.000 claims abstract description 5
- 238000007719 peel strength test Methods 0.000 claims abstract description 5
- 229920003023 plastic Polymers 0.000 claims description 44
- 239000004033 plastic Substances 0.000 claims description 44
- 238000001125 extrusion Methods 0.000 claims description 25
- 239000011241 protective layer Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- 230000032683 aging Effects 0.000 claims description 11
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 10
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 8
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 8
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 7
- 229920000098 polyolefin Polymers 0.000 claims description 7
- 150000008365 aromatic ketones Chemical class 0.000 claims description 6
- 238000006073 displacement reaction Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000004605 External Lubricant Substances 0.000 claims description 4
- 239000004610 Internal Lubricant Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000009472 formulation Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 150000004665 fatty acids Chemical class 0.000 claims description 3
- 125000000623 heterocyclic group Chemical group 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 239000012948 isocyanate Substances 0.000 claims description 3
- 150000002513 isocyanates Chemical class 0.000 claims description 3
- 150000001451 organic peroxides Chemical class 0.000 claims description 3
- 238000011056 performance test Methods 0.000 claims description 3
- 150000002989 phenols Chemical class 0.000 claims description 3
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 claims description 3
- 229920000768 polyamine Polymers 0.000 claims description 3
- 239000000344 soap Substances 0.000 claims description 3
- 150000005846 sugar alcohols Polymers 0.000 claims description 3
- 150000007970 thio esters Chemical class 0.000 claims description 3
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 2
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- 230000000694 effects Effects 0.000 description 10
- 238000007789 sealing Methods 0.000 description 9
- 229920001112 grafted polyolefin Polymers 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 230000001788 irregular Effects 0.000 description 4
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- 238000005452 bending Methods 0.000 description 3
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- 230000003679 aging effect Effects 0.000 description 2
- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 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 description 1
- 239000004831 Hot glue Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
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- 239000003063 flame retardant Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
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- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 238000003466 welding Methods 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
- C08L23/08—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C61/00—Shaping by liberation of internal stresses; Making preforms having internal stresses; Apparatus therefor
- B29C61/02—Thermal shrinking
- B29C61/025—Thermal shrinking for the production of hollow or tubular articles
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/06—Crosslinking by radiation
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Thermal Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
Abstract
The application provides a formula, a preparation method, a product and a test method of a high-rate heat-shrinkable tube. Every 100 weight parts of raw materials comprise the following components in parts by weight: 60-89 parts of polyethylene; 5-35 parts of a copolymer compatilizer; 2-4 parts of an antioxidant; 1-5 parts of a sensitizer; 0.1-5 parts of a lubricant; 1-5 parts of color master batch. The raw materials are blended, granulated and extruded by an extruder to prepare a front expanding tube; performing electron beam or gamma ray irradiation crosslinking modification on the tube before expansion; and expanding the front expanding tube to form a finished product, wherein the expansion multiplying power is more than 4 times. And (3) sleeving the high-rate heat-shrinkable sleeve on the metal pipe, and baking to firmly adhere the heat-shrinkable sleeve and the metal pipe. The cross section of the high-magnification heat-shrinkable sleeve is matched with that of the metal pipe. The test methods include a pull-off force test and a peel strength test for testing the adhesive properties. This application has kept high expansion rate and the viscidity of heat shrinkage bush through reducing the irradiation dose when energy saving and process time, is applicable to the tubular metal resonator protection.
Description
Technical Field
The application relates to the technical field of heat-shrinkable sleeves, in particular to a formula, a preparation method, a product and a test method of a high-rate heat-shrinkable sleeve.
Background
The heat-shrinkable sleeve has excellent flame-retardant and insulating properties, is flexible and elastic, has low shrinkage temperature and fast shrinkage, and can be widely applied to connection of electric wires, treatment of the end parts of the electric wires, protection of welding spots, wire harness identification, insulation protection of resistance and capacitance, anticorrosion protection of metal bars or pipes, protection of antennas and the like. Under the action of high-energy rays, the linear high polymer material forms a three-dimensional network cross-linked structure. The crosslinked polymer material has greatly improved mechanical strength, temperature resistance, chemical solvent resistance, aging resistance and the like, and particularly has greatly improved acid resistance and alkali resistance.
In the industrial fields of automobile parts, electronic components and the like, the heat-shrinkable sleeve is widely applied to the protection of metal and non-metal parts, but metal parts in the fields usually work in alternating cold and hot and humid environments, so that electrochemical corrosion is easy to occur, and the requirement on the sealing property of the heat-shrinkable sleeve is high. And because the metal pipeline may be a special-shaped piece, in order to be sleeved in and shrunk without wrinkling, a high-rate heat shrinkable tube is required, and good wear resistance and sealing property are maintained. To achieve sealing performance, the heat shrinkable sleeve is required to adhere well to the surface of the metal tube after shrinkage and to maintain the adhesion during use. The conventional method is to use a double-wall pipe to achieve the effect, but the inner layer of the double-wall pipe is hot melt adhesive, so that the cost is high, and the production and the processing have various limitations.
Therefore, the invention patent application with publication number CN112111097A provides a formula of a heat-shrinkable sleeve, which comprises polyethylene, maleic anhydride or methacrylic acid grafted polyolefin, an anti-aging agent and carbon black master batches, wherein the grafted polyolefin compatilizer in the formula improves the mechanical strength and the adhesion between the heat-shrinkable sleeve and a metal pipe, and the problem is solved to a certain extent by using the simplest formula. However, the technical scheme has the following defects found in actual production and experiments:
1. the copolymer compatilizer enables the extrusion speed in the extrusion process to be reduced while toughening and improving the viscosity;
2. when the irradiation dose is small, the crosslinking degree is insufficient, the crosslinking is not uniform, and the expansion with high magnification cannot be contracted to the original size due to insufficient memory effect; therefore, higher radiation dose is needed, energy consumption is increased, a wall deflection phenomenon is easily caused during high-rate expansion, and the yield is reduced;
3. the aging effect after the radiation dose is increased can also obviously reduce the effect of the copolymer compatilizer on improving the viscosity between the heat-shrinkable sleeve and the metal pipe, thereby influencing the sealing protection effect.
Disclosure of Invention
Aiming at the defects in the prior art, the application provides a high-rate heat-shrinkable tubing formula which improves the extrusion speed, reduces the irradiation dose and simultaneously improves the viscosity between the heat-shrinkable tubing and a metal tube under the high-rate expansion condition.
The formula of the high-magnification heat-shrinkable tubing provided by the application is suitable for heat-shrinkable tubing of an electron beam or gamma ray irradiation crosslinking process, and each 100 parts by weight of raw materials comprise the following components in parts by weight:
because the requirement of the heat-shrinkable tubing for metal protection on mechanical strength is not high, polyethylene which is easier to process, better in flexibility and better in low-temperature performance is adopted as basic resin. The maleic anhydride or methacrylic acid grafted polyolefin not only plays the roles of a copolymer compatilizer and a thermoplastic elastomer, but also plays the role of sensitizing polyethylene, and the requirement of irradiation dose is reduced to a certain extent; yet another important function of the composition in this application is to increase the adhesion between the heat shrink tubing and the metal tubing. The antioxidant is used for reducing irradiation oxidation and promoting smooth crosslinking, but the dosage of the antioxidant needs to be controlled, otherwise, the requirement of irradiation dose is increased.
Because the irradiation dose requirement of polyethylene, especially low density polyethylene, is high, although the addition of the copolymer compatilizer can reduce the irradiation dose required by crosslinking to a certain extent, the effect is limited, and therefore, a sensitizer needs to be added to further reduce the irradiation dose so as to save energy and reduce irradiation time. Yet another important synergistic effect of the sensitizers in the present application is: when the formula described in the reference is used, the aging effect of the higher radiation dose can obviously reduce the effect of the copolymer on increasing the viscosity between the heat-shrinkable sleeve and the metal tube, and the ratio of each component in the formula can not be obviously improved, so that the problem of the reduction of the viscosity can be solved while the effect of the sensitizer on reducing the radiation dose.
The lubricant is used for improving the flowability of the formula and reducing the friction force with the inner wall of the extrusion die, so that the extrusion speed of the formula at a lower extrusion temperature is increased. The color master batch is used for coloring and providing the function of ultraviolet aging resistance. Through a plurality of tests, the formula of the heat-shrinkable sleeve pipe uses relatively simple components, improves the extrusion speed, reduces the cross-linking irradiation amount and realizes higher viscosity between the heat-shrinkable sleeve pipe and the metal pipe.
Preferably, the polyethylene has a melt index of 2.1 to 9.0g/10 min; the monomer content of the maleic anhydride or methacrylic acid graft modified polyolefin is 1.1-4.9 wt%; the antioxidant is any one or a compound combination of amines, phenols, heterocycles, thioesters and phosphites; the sensitizer is one or a combination of more of isocyanate, polyamine, polyalcohol, acrylate, organic peroxide and aromatic ketone compounds; the lubricant comprises an external lubricant and an internal lubricant, and is a hydrocarbon, fatty acid, ester, alcohol, metal soap lubricant or composite lubricant.
Preferably, each 100 parts by weight of the raw materials comprises the following components in parts by weight: 62-89 parts of linear low-density polyethylene, 5-20 parts of maleic anhydride grafted modified polyolefin, 2-4 parts of antioxidant, 2-4 parts of aromatic ketone sensitizer, 0.1-5 parts of lubricant and 1-5 parts of color master batch. The linear low-density polyethylene maintains the good rheological property of the low-density polyethylene, improves the temperature resistance and the mechanical property, is suitable for being used as basic resin of a film and a sleeve formula, and is beneficial to realizing more than 4 times of expansion ratio when being used for a heat-shrinkable sleeve.
The application also provides a preparation method of the high-rate heat-shrinkable tubing, which comprises the following steps:
s01, preparing materials according to the formula of the high-rate heat-shrinkable sleeve;
s02, blending, granulating and extruding the mixture by an extruder to prepare a front expanding pipe, wherein the extrusion temperature of the extruder is 130-160 ℃, and the extrusion speed is 8-10 m/min;
s03, performing electron beam or gamma ray irradiation on the front expansion tube, wherein the irradiation dose is 50-200 kGy;
s04, expanding and forming the front expanding tube into a finished product, wherein the forming temperature is 150-230 ℃, and the expansion rate is more than 4 times.
By applying the formula of the application, higher extrusion speed can be realized, and the irradiation dose required by sufficient crosslinking is obviously lower than 150-300kGy required by a formula of a comparison document.
Preferably, in the step S03, the medium-energy electron beam irradiation is performed on the front expansion tube, and the irradiation dose is 100-140 kGy; in the step S04, the pre-expansion tube is subjected to air expansion molding, the molding temperature is 180-200 ℃, and the expansion ratio is 4 times. The air expansion forming can realize higher expansion multiplying power and thinner wall thickness.
The application also provides a high-rate heat-shrinkable sleeve for metal pipe protection, and the high-rate heat-shrinkable sleeve is prepared by the preparation method. The wall thickness of the front expanding pipe is 0.4-2.0mm, and the wall thickness of the finished product is 0.1-0.5 mm. The formula of the application overcomes the defect that the wall deviation is easy to occur due to insufficient or uneven cross-linking in a high expansion rate process in a formula of a comparison file, and can realize smooth expansion of a smaller wall thickness.
The application also provides a plastic-coated pipe which comprises a metal pipe and a plastic-coated protective layer, wherein the plastic-coated protective layer is formed by laying the high-rate heat-shrinkable sleeve to the surface of the metal pipe through a heat-shrinkable laying process so as to protect the metal pipe; the thermal shrinkage laying process comprises the following steps: sleeving the high-rate heat-shrinkable sleeve outside the metal pipe; and baking to ensure that the high-rate heat-shrinkable sleeve is heat-shrunk to the outer surface of the metal tube and is firmly adhered to the outer surface of the metal tube, wherein the baking temperature is 200-240 ℃.
Preferably, the cross section of the finished product is matched with that of the metal pipe. Through the matched arrangement of the extrusion die and the expansion die, the cross section of a finished product can be made to be matched with the cross section of the metal pipe to be protected, so that the sleeve pipe and the metal pipe after thermal shrinkage can be better attached, and particularly the cross section of the metal pipe is in an asymmetric or irregular condition.
Preferably, the metal pipe is a reducer pipe or a special pipe, and the special pipe comprises an elbow pipe, a special section pipe or a combination; the plastic-coated protective layer is formed by thermal shrinkage laying of the same high-magnification heat-shrinkable sleeve. Because the high expansion multiplying power is adopted, the heat-shrinkable sleeve is easy to sleeve and can adapt to the condition that the metal pipe has a certain degree of reducing, bending or irregular cross section, and the same high multiplying power heat-shrinkable sleeve is laid to form a plastic-coated protective layer.
The application also provides a high-rate heat-shrinkable tubing test method, which is used for carrying out a high-rate heat-shrinkable tubing adhesion performance test on the plastic-coated tube, and comprises a pull-off force test and a peel strength test.
The pull-out force test comprises the following steps:
s11, thermally shrinking and laying the high-rate heat-shrinkable sleeve to the metal pipe to form a plastic pipe test piece, wherein a traction part is extended out of one end of the metal pipe by the high-rate heat-shrinkable sleeve;
s12, intercepting the plastic-coated pipe test piece with a set length and reserving the traction part;
s13, carrying out IEC216 aging test pretreatment on the plastic-coated pipe test piece, and then placing the test piece to a set test temperature;
s14, pulling the plastic-coated protective layer off or to damage from the metal pipe through the pulling part on a pulling machine at a set first speed at the set test temperature;
and S15, recording a tension displacement curve.
The peel strength test comprises the following steps:
s21, carrying out IEC216 aging test pretreatment on the plastic-coated pipe test piece processed in the steps S11 and S12;
s22, cutting a strip extending along the radial direction of the metal pipe from the plastic-coated protective layer, wherein the adhesion state of the strip and the surface of the metal pipe is not damaged during operation;
s23, stripping the strip from the surface of the metal pipe in a direction of 90 degrees or 180 degrees on a tensile machine at a set second speed;
and S24, recording a tension displacement curve.
The pull-out force test is carried out by using an actual product after the pretreatment of the aging test, so that the actual effect of the formula in improving the viscosity can be effectively tested; the peeling force test is a test commonly used for testing the viscosity, the peeling force test is carried out on an actual product through the aging test pretreatment, the test result is closer to the actual effect, and the test result is more persuasive than the test by adopting a simple sample.
The technical effects of this application lie in:
1. by reasonably proportioning polyethylene and maleic anhydride or methacrylic acid grafted polyolefin and adding a lubricant, the heat-shrinkable tubing keeps the characteristic of easy processing while improving the heat-resistant chemical resistance and mechanical property, and can realize higher extrusion speed;
2. by adding the antioxidant and the sensitizer in a reasonable ratio, the irradiation dose required for realizing sufficient crosslinking and uniform crosslinking is greatly reduced, and the phenomenon of high-rate expansion and wall deviation is improved;
3. the high expansion ratio and the cross section of the heat-shrinkable sleeve matched with the metal pipe enable the heat-shrinkable sleeve to be better applied to the protection of various metal pipes, and the same high-ratio heat-shrinkable sleeve is used for protecting the metal pipe with a certain reducing, bending or irregular cross section;
4. by reducing the irradiation dose, the problem that the viscosity of the surfaces of the heat shrinkable sleeve and the metal pipe is reduced after high irradiation dose crosslinking is solved, and the sealing performance of the heat shrinkable sleeve is ensured;
5. through carrying out pull-off force test and peeling force test on the actual product after aging pretreatment, the viscosity of the surfaces of the heat-shrinkable sleeve and the metal pipe can be effectively tested, and data support is provided for improving the formula.
Detailed Description
In order to more clearly illustrate the technical solutions in the present application or the prior art, specific embodiments of the present application will be described below. The term "and/or" as used in this specification and the appended claims refers to and includes any and all possible combinations of one or more of the associated listed items. In this document, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; either directly or indirectly through intervening media, or both elements may be interconnected. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate. All the formulation components in the following examples are commercially available.
The first embodiment is as follows: a formula of a high-rate heat-shrinkable sleeve, a preparation method, the high-rate heat-shrinkable sleeve and a plastic-coated pipe.
The formula of the high-rate heat-shrinkable tubing of the embodiment is as follows: 81 parts of linear low-density polyethylene with the melt index of 4.0g/10min, 10 parts of maleic anhydride grafted modified polyolefin with the monomer content of 4.9 percent by weight, 2 parts of 1010 antioxidant, 2 parts of aromatic ketone sensitizer, 2 parts of EBS lubricant and 3 parts of yellow color master batch. Wherein the EBS lubricant functions as both an internal lubricant and an external lubricant.
The preparation method comprises the following steps: blending, granulating and extruding at 135 ℃ by an extruder at an extrusion speed of 10 m/min; crosslinking to 180% thermal elongation by 140kGy irradiation; and baking and softening the mixture in an oven at 180 ℃, and expanding the mixture by using air expansion equipment, wherein the expansion rate is 4 times, so that a finished high-rate heat-shrinkable sleeve is prepared. The wall thickness of the front expanding pipe is 1.0mm, and the wall thickness of the finished product is 0.25 mm. The embodiment can be used for production at a high extrusion speed, the required crosslinking degree can be achieved by using a low irradiation dose, and 4 times of high expansion rate can be smoothly realized.
And thermally shrinking the finished product with the inner diameter of 30mm, laying the finished product on an aluminum pipe with the diameter of 10mm, baking at the temperature of 200 ℃, and preparing the finished product into a plastic pipe. The pulling-out force of a plastic-coated protective layer on a plastic-coated pipe sample with the length of 25mm at 80 ℃ is more than 100N; a more desirable sealing performance can be achieved.
The following is a comparative formulation for this example: 84.9 parts of linear low-density polyethylene with the melt index of 4g/10min, 10 parts of maleic anhydride graft modified polyolefin with the monomer content of 4.9 percent by weight, 2 parts of 1010 antioxidant, 0.1 part of EBS lubricant and 3 parts of yellow color master batch. When the formula is blended, granulated and extruded at 135 ℃, the extrusion speed of normal production is 6 m/min; at an irradiation dose of 270kGy, the thermal elongation after irradiation was 300%, and sufficient crosslinking was not attained. When other processes are the same, the wall deviation is easy to occur when the expansion is carried out by using air expansion equipment, and the expansion cannot be stably carried out to 4 times to obtain a qualified finished product.
The thermal elongation of the formula is 180% under 400kGy of irradiation dose, and the high expansion rate of fully crosslinking and 4-time expansion can be achieved. However, under the same application conditions and test conditions, the pull-off force of the plastic-coated protective layer is less than 20N, and the formula cannot achieve the viscous performance.
Therefore, the formula provided by the application improves the extrusion speed, reduces the irradiation dose, and realizes the high expansion ratio of more than 4 times and the high viscosity with the metal tube by reasonable proportioning of the components and adding of a lubricant and a sensitizer.
Example two: a formula of a high-rate heat-shrinkable sleeve, a preparation method, the high-rate heat-shrinkable sleeve and a plastic-coated pipe.
The formula of the high-rate heat-shrinkable tubing of the embodiment is as follows: 60.9 parts of linear low-density polyethylene with the melt index of 2.1g/10min, 35 parts of maleic anhydride grafted modified polyolefin with the monomer content of 1.1 percent by weight, 2 parts of 1010 antioxidant, 1 part of aromatic ketone sensitizer, 0.1 part of EBS lubricant and 1 part of yellow color master batch. The preparation method comprises the following steps: blending, granulating and extruding at 130 ℃ by an extruder, wherein the extrusion speed is 8 m/min; crosslinking to 180% thermal elongation by 200kGy irradiation; and baking and softening the mixture in an oven at 150 ℃, and expanding the mixture by using air expansion equipment, wherein the expansion rate is 4 times, so that a finished product of the high-rate heat-shrinkable sleeve is prepared. The wall thickness of the front expanding pipe is 2.0mm, and the wall thickness of the finished product is 0.5 mm. The present embodiment can also be produced at a relatively high extrusion speed, and can achieve the required degree of crosslinking with a relatively low irradiation dose, and can smoothly achieve a high expansion ratio of 4 times.
And thermally shrinking the finished product with the inner diameter of 50mm, laying the finished product on an aluminum pipe with the diameter of 20mm, baking at 240 ℃ and preparing a plastic pipe. The pulling-out force of a plastic-coated protective layer on an aluminum pipe sample with the length of 25mm at 80 ℃ is more than 100N; a more desirable sealing performance can be achieved.
Example three: a formula of a high-rate heat-shrinkable sleeve, a preparation method, the high-rate heat-shrinkable sleeve and a plastic-coated pipe.
The formula of the high-rate heat-shrinkable tubing of the embodiment is as follows: 76 parts of linear low-density polyethylene with the melt index of 9.0g/10min, 5 parts of methacrylic acid grafted polyolefin with the monomer content of 3.0 percent by weight, 4 parts of 1010 antioxidant, 5 parts of aromatic ketone sensitizer, 5 parts of EBS lubricant and 5 parts of yellow color master batch. The preparation method comprises the following steps: blending, granulating and extruding at 160 ℃ by an extruder at an extrusion speed of 9 m/min; carrying out irradiation crosslinking to reach thermal elongation of 180% by 50 kGy; and baking and softening the mixture in an oven at 230 ℃, and expanding the mixture by using air expansion equipment, wherein the expansion rate is 4 times, so that a finished product of the high-rate heat-shrinkable sleeve is prepared. The wall thickness of the front expanding pipe is 0.4mm, and the wall thickness of the finished product is 0.1 mm. The present embodiment can also be produced at a relatively high extrusion speed, and can achieve the required degree of crosslinking with a very low irradiation dose, and can successfully achieve a high expansion ratio of 4 times.
And thermally shrinking the finished product with the inner diameter of 30mm, laying the finished product on an aluminum pipe with the diameter of 10mm, baking at 220 ℃ to prepare a plastic pipe. The pulling-out force of a plastic-coated protective layer on a plastic-coated pipe sample with the length of 25mm at 80 ℃ is more than 100N; a more desirable sealing performance can be achieved.
Example four: a formula of a high-rate heat-shrinkable sleeve, a preparation method, the high-rate heat-shrinkable sleeve and a plastic-coated pipe.
The formula of the high-rate heat-shrinkable tubing of the embodiment is as follows: 68 parts of linear low-density polyethylene with the melt index of 4.0g/10min, 20 parts of methacrylic acid grafted polyolefin with the monomer content of 4.9 percent by weight, 3 parts of 1010 antioxidant, 3 parts of aromatic ketone sensitizer, 3 parts of EBS lubricant and 3 parts of yellow color master batch. The preparation method comprises the following steps: blending, granulating and extruding at 135 ℃ by an extruder at an extrusion speed of 10 m/min; crosslinking to 180% thermal elongation by 100kGy irradiation; and baking and softening the mixture in an oven at 200 ℃, and expanding the mixture by using air expansion equipment, wherein the expansion rate is 4 times, so that a finished product of the high-rate heat-shrinkable sleeve is prepared. The wall thickness of the front expanding pipe is 0.4mm, and the wall thickness of the finished product is 0.1 mm. The present embodiment can also be produced at a relatively high extrusion speed, and can achieve the required degree of crosslinking with a very low irradiation dose, and can successfully achieve a high expansion ratio of 4 times.
And thermally shrinking the finished product with the inner diameter of 30mm, laying the finished product on an aluminum pipe with the diameter of 10mm, baking at 220 ℃ to prepare a plastic pipe. The pulling-out force of a plastic-coated protective layer on a plastic-coated pipe sample with the length of 25mm at 80 ℃ is more than 100N; a more desirable sealing performance can be achieved.
The antioxidant can also be selected from one or more of other amines, phenols, heterocycles, thioesters and phosphites; the lubricant can also be selected from other hydrocarbon, fatty acid, ester, alcohol, metal soap lubricant or composite lubricant, and the internal lubricant and the external lubricant can also be selected from different types for matching use; the sensitizer can also be selected from one or more of other isocyanate, polyamine, polyalcohol, acrylate, organic peroxide and aromatic ketone compounds; the proportion of each component is properly adjusted according to the performance difference of each component or limited tests.
When the tubular metal resonator is the reducing pipe, when the maximum diameter is within 2 times of minimum diameter, perhaps when having on the tubular metal resonator and not sharp-pointed protruding, only need the heat shrinkable bush of same root diameter to carry out the pyrocondensation and lay, when the diameter change was too big, then need adopt the multistage heat shrinkable bush of multiple diameter to protect. When the metal pipe is bent at a small angle, the metal pipe can be protected by only one heat-shrinkable sleeve, and when the bending angle is larger, a plurality of heat-shrinkable sleeves are needed. When the section of the metal pipe is polygonal, elliptical, oval or irregular, an extrusion die and an expansion die matched with the section can be used for producing a finished product heat-shrinkable tubing with the cross section matched with the section; when the dosage is not large, a circular sleeve with proper diameter can be selected, and a good protective layer is formed by utilizing the characteristics of high-rate expansion and high-rate contraction.
Example five: a high-rate heat-shrinkable tubing test method.
The embodiment is used for carrying out high-rate heat-shrinkable sleeve adhesion performance tests on the plastic-coated pipes in the first to fourth embodiments, and the tests comprise a pull-off force test and a peeling force test;
the pull-out force test comprises the following steps:
s11, laying the high-rate heat-shrinkable sleeve to the metal pipe to form a plurality of plastic-coated pipe test pieces, wherein the high-rate heat-shrinkable sleeve extends out of one end of the metal pipe to leave a traction part;
s12, cutting a 25mm test piece and reserving the traction part;
s13, carrying out IEC216 aging test pretreatment on the test piece, and then placing the test piece for 4 hours at 80 ℃;
s14, pulling the high-rate heat-shrinkable sleeve off or to the damage of the high-rate heat-shrinkable sleeve through the pulling part at 50mm/min on a tensile machine with a temperature box at 80 ℃;
and S15, recording a tension displacement curve, and calculating the average pull-out force according to the test results of more than 3 test pieces.
The peel force test comprises the following steps:
s21, carrying out IEC216 aging test pretreatment on the plastic-coated pipe test piece processed in the steps S11 and S12;
s22, cutting a strip extending along the radial direction of the metal pipe from the plastic-coated protective layer, wherein the adhesion state of the strip and the surface of the metal pipe is not damaged during operation; the length of the strip is 100mm, and the width is selected according to the pipe diameter of the metal pipe;
s23, testing a plurality of test pieces on a tensile machine at the speed of 30mm/min and in the directions of 90 degrees and 180 degrees, and stripping the strip from the surface of the metal pipe;
and S24, recording a tension displacement curve, and calculating the average peeling strength through the test results of more than 3 test pieces in each direction.
Through experimental design, the heat-shrinkable tubing with different formulas, different irradiation doses and different other process parameters is tested, the influence of each formula component can be found out, and a relatively better proportion can be found out.
The foregoing is only a preferred embodiment of the present application and the technical principles employed, and various obvious changes, rearrangements and substitutions may be made without departing from the spirit of the application. Other advantages and effects of the present application will be readily apparent to those skilled in the art from the disclosure herein. The present application is capable of other and different embodiments and its several details are capable of modifications and variations in various respects, all without departing from the spirit of the present application. The features in the above embodiments and embodiments may be combined with each other without conflict.
Claims (10)
1. A high-magnification heat-shrinkable tubing formula is used for heat-shrinkable tubing of electron beam or gamma ray irradiation crosslinking process, and is characterized in that each 100 parts by weight of raw materials comprise the following components in parts by weight:
2. the high-rate heat-shrinkable sleeve formulation of claim 1, wherein:
the melt index of the polyethylene is 2.1-9.0g/10 min;
the monomer content of the maleic anhydride or methacrylic acid graft modified polyolefin is 1.1-4.9 wt%;
the antioxidant is any one or a compound combination of amines, phenols, heterocycles, thioesters and phosphites;
the sensitizer is one or a combination of more of isocyanate, polyamine, polyalcohol, acrylate, organic peroxide and aromatic ketone compounds;
the lubricant comprises an external lubricant and an internal lubricant, and is a hydrocarbon, fatty acid, ester, alcohol, metal soap lubricant or composite lubricant.
3. The high-rate heat-shrinkable sleeve formulation of claim 2, wherein:
every 100 weight parts of raw materials comprise the following components in parts by weight: 62-89 parts of linear low-density polyethylene, 5-20 parts of maleic anhydride grafted modified polyolefin, 2-4 parts of antioxidant, 2-4 parts of aromatic ketone sensitizer, 0.1-5 parts of lubricant and 1-5 parts of color master batch.
4. A preparation method of a high-rate heat-shrinkable tubing is characterized by comprising the following steps:
s01, preparing materials according to the formula of the high-rate heat-shrinkable tubing claimed in claim 1, 2 or 3;
s02, blending, granulating and extruding the mixture by an extruder to prepare a front expanding pipe, wherein the extrusion temperature of the extruder is 130-160 ℃, and the extrusion speed is 8-10 m/min;
s03, performing electron beam or gamma ray irradiation on the front expansion tube, wherein the irradiation dose is 50-200 kGy;
s04, expanding and forming the front expanding tube into a finished product, wherein the forming temperature is 150-230 ℃, and the expansion rate is not less than 4 times.
5. The method of making a high-rate heat-shrinkable sleeve according to claim 4, wherein:
in the step S03, performing intermediate-energy electron beam irradiation on the front expansion tube, wherein the irradiation dose is 100-140 kGy;
in the step S04, the pre-expansion tube is subjected to air expansion molding, the molding temperature is 180-200 ℃, and the expansion ratio is 4 times.
6. The utility model provides a high magnification heat shrinkable tube for the protection of tubular metal resonator which characterized in that:
prepared by the high-rate heat-shrinkable tubing preparation method of claim 4 or 5;
the wall thickness of the front expanding pipe is 0.4-2.0mm, and the wall thickness of the finished product is 0.1-0.5 mm.
7. The utility model provides a plastic-coated pipe, moulds the protective layer including tubular metal resonator and package, its characterized in that:
the plastic-coated protective layer is formed by laying the high-rate heat-shrinkable sleeve pipe in claim 6 on the surface of the metal pipe through a heat-shrinkable laying process;
the thermal shrinkage laying process comprises the following steps: sleeving the high-rate heat-shrinkable sleeve outside the metal pipe; and baking to ensure that the high-rate heat-shrinkable sleeve is heat-shrunk to the outer surface of the metal tube and is firmly adhered to the outer surface of the metal tube, wherein the baking temperature is 200-240 ℃.
8. The plastic coated pipe according to claim 7, wherein:
the cross section of the finished product is matched with that of the metal pipe.
9. The plastic coated pipe according to claim 8, wherein:
the metal pipe is a reducer pipe or a special pipe, and the special pipe comprises an elbow pipe, a special-shaped section pipe or a combination;
the plastic-coated protective layer is formed by thermal shrinkage laying of the same high-magnification heat-shrinkable sleeve.
10. A high-rate heat-shrinkable tubing test method is characterized by comprising the following steps:
a high rate heat shrink tubing adhesion performance test for the plastic coated tubing of claim 7 or 8 or 9, comprising a pull-off force test and a peel strength test;
the pull-out force test comprises the following steps:
s11, thermally shrinking and laying the high-rate heat-shrinkable sleeve to the metal pipe to form a plastic pipe test piece, wherein a traction part is extended out of one end of the metal pipe by the high-rate heat-shrinkable sleeve;
s12, intercepting the plastic-coated pipe test piece with a set length and reserving the traction part;
s13, carrying out IEC216 aging test pretreatment on the plastic-coated pipe test piece, and then placing the test piece to a set test temperature;
s14, pulling the plastic-coated protective layer off or to damage from the metal pipe through the pulling part on a pulling machine at a set first speed at the set test temperature;
s15, recording a tension displacement curve;
the peel strength test comprises the following steps:
s21, carrying out IEC216 aging test pretreatment on the plastic-coated pipe test piece processed in the steps S11 and S12;
s22, cutting a strip extending along the radial direction of the metal pipe from the plastic-coated protective layer, wherein the adhesion state of the strip and the surface of the metal pipe is not damaged during operation;
s23, stripping the strip from the surface of the metal pipe in a direction of 90 degrees or 180 degrees on a tensile machine at a set second speed;
and S24, recording a tension displacement curve.
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Application publication date: 20210824 |