CN108034125B - Novel heat-shrinkable tube material and preparation method thereof - Google Patents
Novel heat-shrinkable tube material and preparation method thereof Download PDFInfo
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- CN108034125B CN108034125B CN201711318077.3A CN201711318077A CN108034125B CN 108034125 B CN108034125 B CN 108034125B CN 201711318077 A CN201711318077 A CN 201711318077A CN 108034125 B CN108034125 B CN 108034125B
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- 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
- C08L23/10—Homopolymers or copolymers of propene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/44—Preparation of metal salts or ammonium salts
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/12—Shape memory
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/05—Polymer mixtures characterised by other features containing polymer components which can react with one another
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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
- C08L2312/00—Crosslinking
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- Polymers & Plastics (AREA)
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Abstract
The invention provides a novel heat-shrinkable tube material and a preparation method thereof, wherein the heat-shrinkable tube material is prepared from the following raw materials in parts by weight: 85-95 parts of polypropylene, 1-5 parts of acrylic acid, 2-10 parts of acrylate, 1-5 parts of metal oxide, 0.01-0.1 part of cross-linking agent and 0.01-0.1 part of auxiliary agent. The novel heat-shrinkable tube material and the preparation method thereof have the characteristics of recoverability, simple processing technology and the like, have good economic applicability, heat resistance, electrical insulation performance and mechanical performance, and can be applied to the field of circuit joint protection and sealing.
Description
Technical Field
The invention belongs to the technical field of polymer modification, and particularly relates to a novel heat-shrinkable tube material and a preparation method thereof.
Background
Currently, the main materials for producing heat shrinkable tubes include: olefin polymer or copolymer; rubber material or thermoplastic elastomer styrene-butadiene-styrene block copolymer (SBS) and styrene-isoprene block copolymer (SIS); (iii) other auxiliary materials. The processing process needs chemical and radiation crosslinking, the processing technology is complex, the material can not be recycled, and the processing cost is high.
It was found that the carboxylic acid salts are formed by the in situ polymerization of acrylic acid and acrylic esters in a twin screw and further by the reaction thereof with metal oxides and are homogeneously dispersed in the mixture. The carboxylate has strong polarity, so that a relatively stable network structure is formed in a material system, and when the carboxylate is uniformly dispersed in a polypropylene system, metal ions serve as physical cross-linking bonds in the material system and play a role in fixing the shape. In conclusion, the composition system obtains excellent shape memory function through stable physical crosslinking points formed by the metal salt in the polypropylene organism. The heat-shrinkable tube prepared by the method is a shape polymer with a physical crosslinking structure, can be directly formed by injection molding after being extruded and granulated, does not need complex processes such as chemistry or radiation and the like, and is simple and easy to obtain.
Disclosure of Invention
In view of the above, the present invention is directed to a novel heat shrinkable tube material and a preparation method thereof, wherein the heat shrinkable tube material has good economic applicability, heat resistance, electrical insulation property and mechanical property, and can be applied to the field of circuit joint protection and sealing.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a novel heat-shrinkable tube material is prepared from the following raw materials in parts by weight: 85-95 parts of polypropylene, 1-5 parts of acrylic acid, 2-10 parts of acrylate, 1-5 parts of metal oxide, 0.01-0.1 part of cross-linking agent and 0.01-0.1 part of auxiliary agent.
Preferably, the polypropylene is a homo-polypropylene and/or a co-polypropylene.
Preferably, the purity of the acrylic acid is more than or equal to 98.5%, and the acrylic ester is one or more of ethyl acrylate, butyl acrylate and glycidyl acrylate.
Preferably, the acrylic acid accounts for 1-3.5 parts by weight, and the acrylate accounts for 2-9.5 parts by weight.
Preferably, the metal oxide is one or more of zinc oxide, magnesium oxide, iron oxide and aluminum oxide.
Preferably, the metal oxide is present in an amount of 1 to 4 parts by weight.
Preferably, the cross-linking agent is one or more of benzoyl peroxide, lauroyl peroxide, cumene hydroperoxide, tert-butyl hydroperoxide, di-tert-butyl peroxide, dicumyl peroxide, tert-butyl peroxybenzoate, tert-butyl peroxypivalate, methyl ethyl ketone peroxide, cyclohexanone peroxide, diisopropyl peroxydicarbonate and dicyclohexyl peroxydicarbonate.
Preferably, the weight portion of the cross-linking agent is 0.01-0.08.
The preparation method of the novel heat-shrinkable tube material comprises the following steps:
the first step is as follows: uniformly mixing the raw materials to obtain a premix;
the second step is that: extruding and granulating the premix prepared in the first step in an extruder at the temperature of 200-320 ℃;
the third step: extruding the granules prepared in the second step into a required specific shape through an extruder;
the fourth step: and (3) expanding the extruded special shape prepared in the third step by heating, cooling and shaping to prepare the novel heat-shrinkable tube material.
The preparation method of the novel heat-shrinkable tube material comprises extrusion granulation, extrusion molding and direct heat expansion, does not need chemical crosslinking, and fixes the required shape through the physical crosslinking effect formed by the metal salt of the copolymer in a system.
The novel heat shrinkable tube disclosed by the invention has the following principle: a certain amount of in-situ generated acrylate/acrylate copolymer dispersed phase is uniformly dispersed in polypropylene resin, meanwhile, an acrylate chain segment can play a toughening role, the whole ductility of the material is improved, meanwhile, hydrogen bonds on carbon atoms connected with methyl groups of the polypropylene have certain activity, and under the condition that free radicals exist, the acrylic acid/acrylate is grafted to the chain segment of the polypropylene, so that in-situ generated metal salt is more uniformly dispersed in the resin. Because polypropylene has a certain melting point, and ionic bonds between acrylates exist stably in a certain stable range without being damaged, when the blend is heated to a certain temperature, the polypropylene resin is in a molten state, and the ionic bonds formed by the acrylate/acrylate copolymer still exist, and can be used as physical crosslinking points to exist in the blend to record the original shape of the material; when the temperature is reduced to be lower than the melting point of the polypropylene, the polypropylene is in a crystalline state and can fix the shape at high temperature; when the temperature is raised above the melting point of the polypropylene, the original shape is restored, due to the presence of the physical crosslinks at this time. Due to the characteristics of the composition, the heat shrinkable tube material can be applied to the field of heat shrinkable tube materials.
Compared with the prior art, the novel heat-shrinkable tube material and the preparation method thereof have the following advantages:
the novel heat-shrinkable tube material and the preparation method thereof have the characteristics of recoverability, simple processing technology and the like, have good economic applicability, heat resistance, electrical insulation performance and mechanical performance, and can be applied to the field of circuit joint protection and sealing.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
The crosslinking agents used in the examples and comparative examples were dicumyl peroxide (DCP); the used auxiliary agents are antioxidant and lubricant.
Example 1
A novel heat-shrinkable tube material is prepared from the following raw materials in parts by weight: 90.3 parts of polypropylene, 2 parts of acrylic acid, 6 parts of butyl acrylate, 1 part of zinc oxide, 0.05 part of cross-linking agent, 0.2 part of antioxidant and 0.5 part of lubricant.
The preparation method of the novel heat-shrinkable tube material comprises the following steps:
the first step is as follows: uniformly mixing the raw materials to obtain a premix;
the second step is that: extruding and granulating the premix prepared in the first step in an extruder at the temperature of 200-320 ℃;
the third step: extruding the granules prepared in the second step into a required specific shape through an extruder;
the fourth step: and (3) expanding the extruded special shape prepared in the third step by heating, cooling and shaping to prepare the novel heat-shrinkable tube material.
Example 2
A novel heat-shrinkable tube material is prepared from the following raw materials in parts by weight: 86.3 parts of polypropylene, 3 parts of acrylic acid, 8 parts of butyl acrylate, 2 parts of zinc oxide, 0.06 part of cross-linking agent, 0.2 part of antioxidant and 0.5 part of lubricant.
The preparation method of the novel heat-shrinkable tube material comprises the following steps:
the first step is as follows: uniformly mixing the raw materials to obtain a premix;
the second step is that: extruding and granulating the premix prepared in the first step in an extruder at the temperature of 200-320 ℃;
the third step: extruding the granules prepared in the second step into a required specific shape through an extruder;
the fourth step: and (3) expanding the extruded special shape prepared in the third step by heating, cooling and shaping to prepare the novel heat-shrinkable tube material.
Example 3
A novel heat-shrinkable tube material is prepared from the following raw materials in parts by weight: 85.0 parts of polypropylene, 3.5 parts of acrylic acid, 8.3 parts of butyl acrylate, 2.5 parts of zinc oxide, 0.08 part of cross-linking agent, 0.2 part of antioxidant and 0.5 part of lubricant.
The preparation method of the novel heat-shrinkable tube material comprises the following steps:
the first step is as follows: uniformly mixing the raw materials to obtain a premix;
the second step is that: extruding and granulating the premix prepared in the first step in an extruder at the temperature of 200-320 ℃;
the third step: extruding the granules prepared in the second step into a required specific shape through an extruder;
the fourth step: and (3) expanding the extruded special shape prepared in the third step by heating, cooling and shaping to prepare the novel heat-shrinkable tube material.
Comparative example 1
A heat-shrinkable tube material is prepared from the following raw materials in parts by weight: 75.3 parts of polypropylene, 8 parts of acrylic acid, 10 parts of butyl acrylate, 6 parts of zinc oxide, 0.12 part of cross-linking agent, 0.2 part of antioxidant and 0.5 part of lubricant.
The preparation method of the heat shrinkable tube material comprises the following steps:
the first step is as follows: uniformly mixing the raw materials to obtain a premix;
the second step is that: extruding and granulating the premix prepared in the first step in an extruder at the temperature of 200-320 ℃;
the third step: extruding the granules prepared in the second step into a required specific shape through an extruder;
the fourth step: and (4) heating and expanding the extruded specific shape prepared in the third step, and cooling and shaping to prepare the heat shrinkable tube material.
Comparative example 2
A heat-shrinkable tube material is prepared from the following raw materials in parts by weight: 86.3 parts of polypropylene, 3 parts of acrylic acid, 8 parts of butyl acrylate, 1.5 parts of zinc oxide, 0.2 part of antioxidant and 0.5 part of lubricant.
The preparation method of the heat shrinkable tube material comprises the following steps:
the first step is as follows: uniformly mixing the raw materials to obtain a premix;
the second step is that: extruding and granulating the premix prepared in the first step in an extruder at the temperature of 200-320 ℃;
the third step: extruding the granules prepared in the second step into a required specific shape through an extruder;
the fourth step: and (4) heating and expanding the extruded specific shape prepared in the third step, and cooling and shaping to prepare the heat shrinkable tube material.
Comparative example 3
A heat-shrinkable tube material is prepared from the following raw materials in parts by weight: 86.3 parts of polypropylene, 11 parts of polyacrylate toughening agent, 2 parts of zinc oxide, 0.05 part of crosslinking agent, 0.2 part of antioxidant and 0.5 part of lubricant.
The preparation method of the heat shrinkable tube material comprises the following steps:
the first step is as follows: uniformly mixing the raw materials to obtain a premix;
the second step is that: extruding and granulating the premix prepared in the first step in an extruder at the temperature of 200-320 ℃;
the third step: extruding the granules prepared in the second step into a required specific shape through an extruder;
the fourth step: and (4) heating and expanding the extruded specific shape prepared in the third step, and cooling and shaping to prepare the heat shrinkable tube material.
The shape fixing rate and the shape recovery rate of the heat shrinkable tube materials prepared in examples 1 to 3 and comparative examples 1 to 3 were measured under the following conditions:
the shape memory properties of the sample were first heated to 160 ℃ and stretched at this temperature to a strain (. epsilon.m) of 100% or 50%;
then cooling to normal temperature and unloading. After unloading, part of the strain (. epsilon.m-. epsilon.u) is recovered instantaneously, leaving an unrecovered strain (. epsilon.u).
The sample was then heated again at a loading temperature of 160 ℃ for strain recovery, resulting in a permanent strain (. epsilon.p). The above three steps complete a simple thermomechanical cycle. The shape fixation ratio (SF) and shape recovery ratio (SR) are defined as follows:
the test results are shown in table 1:
TABLE 1 concrete compounding ratios of respective compositions in examples 1 to 3 and comparative examples 1 to 3 and their test properties
From the test data in the above table, it can be seen that the shape fixation rate and the shape recovery rate of the heat shrinkable tube material of the present invention are both greatly improved as compared with the comparative examples.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A heat shrinkable tube material is characterized in that: the heat shrinkable tube material is prepared from the following raw materials in parts by weight: 85-95 parts of polypropylene, 1-5 parts of acrylic acid, 2-10 parts of acrylate, 1-5 parts of metal oxide, 0.01-0.08 part of cross-linking agent and 0.01-0.1 part of auxiliary agent; the polypropylene is homo-polypropylene and/or co-polypropylene.
2. A heat shrinkable tube material as set forth in claim 1, wherein: the purity of the acrylic acid is more than or equal to 98.5 percent, and the acrylic acid is one or more of ethyl acrylate, butyl acrylate and glycidyl acrylate.
3. A heat shrinkable tube material as set forth in claim 2, wherein: the weight portion of the acrylic acid is 1-3.5, and the weight portion of the acrylate is 2-9.5.
4. A heat shrinkable tube material as set forth in claim 1, wherein: the metal oxide is one or more of zinc oxide, magnesium oxide, iron oxide and aluminum oxide.
5. A heat shrinkable tube material as set forth in claim 1, wherein: the weight portion of the metal oxide is 1-4 portions.
6. A heat shrinkable tube material as set forth in claim 1, wherein: the cross-linking agent is one or more of benzoyl peroxide, lauroyl peroxide, cumene hydroperoxide, tert-butyl hydroperoxide, di-tert-butyl peroxide, dicumyl peroxide, tert-butyl peroxybenzoate, tert-butyl peroxypivalate, methyl ethyl ketone peroxide, cyclohexanone peroxide, diisopropyl peroxydicarbonate and dicyclohexyl peroxydicarbonate.
7. The method of making a heat shrinkable tube material of any of claims 1-6, wherein: the method comprises the following steps:
the first step is as follows: uniformly mixing the raw materials to obtain a premix;
the second step is that: extruding and granulating the premix prepared in the first step in an extruder at the temperature of 200-320 ℃;
the third step: extruding the granules prepared in the second step into a required specific shape through an extruder;
the fourth step: and (4) heating and expanding the extruded specific shape prepared in the third step, and cooling and shaping to prepare the heat shrinkable tube material.
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| CN103524682B (en) * | 2013-10-04 | 2016-05-04 | 浙江大学 | Reaction is extruded and is prepared the method for high melt strength, propylene from aggressiveness |
| CN103554655B (en) * | 2013-10-04 | 2016-01-20 | 浙江大学 | Reactive extrursion prepares the method for Polypropylene Ionomers |
| CN104927149B (en) * | 2015-05-12 | 2017-12-08 | 天津金发新材料有限公司 | A kind of polyethylene/polyester heat-shrink tube and preparation method thereof |
| CN106317557A (en) * | 2016-08-18 | 2017-01-11 | 苏州泰斯拓伟机电设备有限公司 | Insulating heat shrink tube for high-speed railway track and preparation method of tube |
| CN106832142B (en) * | 2016-12-27 | 2019-05-03 | 天津金发新材料有限公司 | A kind of filling PC composition |
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