CN114957967B - Thermoplastic polyurethane elastomer for charging pile sheath and preparation method thereof - Google Patents

Thermoplastic polyurethane elastomer for charging pile sheath and preparation method thereof Download PDF

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CN114957967B
CN114957967B CN202111400732.6A CN202111400732A CN114957967B CN 114957967 B CN114957967 B CN 114957967B CN 202111400732 A CN202111400732 A CN 202111400732A CN 114957967 B CN114957967 B CN 114957967B
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long
butanediol
charging pile
mass ratio
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CN114957967A (en
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蔡建国
龙双林
张曦
徐震华
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Shanghai Lejoin High Molecular Material Co ltd
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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
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes
    • C08L75/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
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    • C08G18/3206—Polyhydroxy compounds aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4202—Two or more polyesters of different physical or chemical nature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633—Compounds of group C08G18/42
    • C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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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
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
    • 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
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/60—Other road transportation technologies with climate change mitigation effect
    • Y02T10/70—Energy storage systems for electromobility, e.g. batteries
    • 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
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/60—Other road transportation technologies with climate change mitigation effect
    • Y02T10/7072—Electromobility specific charging systems or methods for batteries, ultracapacitors, supercapacitors or double-layer capacitors

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  • Compositions Of Macromolecular Compounds (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

The application relates to the field of C08L75/04, in particular to a thermoplastic polyurethane elastomer for a charging pile sheath and a preparation method thereof. The application adopts diphenylmethane diisoacid ester to react with a polyol compound, adopts poly (1, 4-butanediol adipate), poly (1, 4-butanediol adipate) glycol and poly (ethylene succinate) glycol as long-chain polyol compounds, adopts 1, 4-butanediol and polyethylene glycol 200 as small-molecule chain extenders, and controls the mass ratio of the long-chain polyol compounds to the small-molecule chain extenders to be (4-6): 1, under the synergistic effect of the nano filler and the protective agent, the hardness and softness of the thermoplastic polyurethane elastomer can be improved to the greatest extent, so that the prepared thermoplastic polyurethane elastomer is moderate in hardness and higher in tear resistance, elongation at break and tensile strength, has excellent flame retardance and ageing resistance, and meets the higher practical application requirements of the charging pile protective sleeve.

Description

Thermoplastic polyurethane elastomer for charging pile sheath and preparation method thereof
Technical Field
The application relates to the field of C08L75/04, in particular to a thermoplastic polyurethane elastomer for a charging pile sheath and a preparation method thereof.
Background
Polyurethanes are prepolymers formed from the reaction of a diisocyanate with a polyester or polyether containing a polyol in the structure, long chain polyols and short chain polyols are both used to synthesize the polyurethane, wherein the long chain polyols provide soft domains or segments in the polyurethane, while the short chain polyols generally act as chain extenders and combine with isocyanates to form hard segments in the polyurethane to shape the resin.
At present, the preparation raw materials of the charging pile protective sleeve mainly comprise thermoplastic elastomer and polyvinyl chloride, chinese patent CN104530625A discloses a halogen-free flame-retardant insulating cable material for an electric automobile charging pile and a preparation method thereof, and the cable material obtained by taking hydrogenated polystyrene-ethylene/butylene-styrene segmented copolymer as the main raw materials and taking polyester elastomer and polyolefin resin as matrix materials has higher elongation at break, but has lower tearing strength and cannot meet the actual application requirements; chinese patent CN108148327a discloses a PVC charging pile cable material and a preparation method thereof, comprising using polyvinyl chloride as a matrix material, the obtained PVC charging pile cable material has higher tensile strength, but the elongation at break is only about 120%, the texture is hard and easy to break; notably, the first standard (GB/T33594) for charging pile cables, which has increased the requirement for tear strength of the charging pile sheath, was formally released in 2017 in China.
Therefore, the polyurethane thermoplastic elastomer with moderate hardness, high elongation at break, high tensile strength and high tearing strength is provided, and meanwhile, the polyurethane thermoplastic elastomer is excellent in flame retardance and ageing resistance, can meet the higher practical application requirements of the charging pile protective sleeve, and has important practical research and application significance.
Disclosure of Invention
The application provides a thermoplastic polyurethane elastomer for a charging pile sheath, which at least comprises the following components in parts by weight: 40 to 60 parts of isocyanate, 60 to 90 parts of polyalcohol compounds, 1 to 6 parts of nano-filler, 5 to 10 parts of protective agent and 0.1 to 0.5 part of compatilizer;
as a preferable technical scheme, the isocyanate is at least one selected from toluene diisocyanate, diphenylmethane diisoacid ester, dicyclohexylmethane diisocyanate and hexamethylene diisocyanate; as the thermoplastic elastomer for the charging pile protective sleeve has higher requirements on tearing strength, flexibility and chemical stability, the isocyanate is diphenylmethane diisoacid ester, and the nano filler, the protective agent and the compatilizer in the synergistic system are controlled by controlling the mass ratio of the diphenylmethane diisoacid ester to the polyalcohol compound to obtain the thermoplastic polyurethane elastomer with moderate hardness, high tearing strength, high tensile strength and high elongation at break, and meanwhile, the provided polyurethane elastomer has excellent flame retardance and ageing resistance, so that the practical application requirement of the charging pile protective sleeve is met;
the CAS number of the diphenylmethane diisoacid ester is 101-68-8, and the diphenylmethane diisoacid ester is purchased from Shanghai Ala Biochemical technology Co., ltd;
as a preferable technical scheme, the polyol compound at least comprises a long-chain polyol compound and a small-molecule chain extender; the charging pile protection sleeve protects the charging pile from the influence of external acting force, environmental conditions and the like, so that the charging pile is inevitably required to be exposed to ultraviolet rays, high temperature and the like for a long time, and therefore, the requirements on the hardness, flexibility, ageing resistance and the like of the material are high, and as a preferable technical scheme, the mass ratio of the long-chain polyol compound to the small-molecule chain extender is (4-6): 1, the soft segment can be formed in polyurethane through the long-chain polyol compound to the greatest extent, and the hard segment can be formed in polyurethane through the small-molecule chain extender, so that the prepared thermoplastic polyurethane elastomer meets the requirement of serving as a protective sleeve of the charging pile;
in the preparation process of the long-chain polyol compound actually applied to the polyurethane thermoplastic elastomer, different long-chain polyol compounds are selected according to different application fields of the polyurethane thermoplastic elastomer; as a preferable technical scheme, the long-chain polyol compound is saturated aliphatic polyester polyol with the number average molecular weight in the range of 500-2000, and although the saturated aliphatic polyester polyol is widely applied to the production of polyurethane thermoplastic elastomer, the number average molecular weight of the saturated aliphatic polyester polyol is controlled in the range of 500-2000, so that the production period can be shortened and the production efficiency of the product can be improved on the premise of ensuring that the product is easy to process and has high yield;
as a preferable technical scheme, the saturated aliphatic polyester polyol is at least one selected from poly (1, 4-butanediol adipate), poly (ethylene succinate), poly (1, 4-butanediol adipate) glycol and poly (ethylene glycol adipate);
the poly (1, 4-butanediol adipate) is widely applied to the production of polyurethane, but the hardness of the poly (1, 4-butanediol adipate) needs to be regulated to a certain extent to ensure that the poly (1, 4-butanediol adipate) is better suitable for the protective sleeve of the charging pile, and as a preferable technical scheme, the saturated aliphatic polyester polyol is the combination of the poly (1, 4-butanediol adipate), the poly (1, 4-butanediol adipate) glycol and the poly (ethylene succinate) glycol, the poly (1, 4-butanediol adipate) glycol has certain crystallinity, and the existence of the poly (ethylene succinate) glycol can avoid the excessive crystallization of the poly (ethylene succinate) glycol to cause the hardness of the obtained polyurethane thermoplastic elastomer to be too high; the inventors have unexpectedly found that when the mass ratio of the poly (1, 4-butylene adipate), the poly (1, 4-butylene adipate) glycol and the poly (ethylene succinate) is controlled to be (1-3): 1:0.8, the hardness and softness of the polyurethane thermoplastic elastomer can be improved to the greatest extent, and the balance of the hardness and the flexibility of the polyurethane thermoplastic elastomer is realized under the action of the small molecule chain extender;
the number average molecular weight of the poly (1, 4-butanediol adipate) is 2000, the CAS number is 150923-12-9, and the poly (1, 4-butanediol adipate) is purchased from Shanghai Michelin Biochemical technology Co., ltd; the number average molecular weight of the poly (1, 4-butanediol adipate) glycol is 1000, the model is HY-1022, and the poly (1, 4-butanediol adipate) glycol is purchased from Xuzhou bright Huiyang New material Co., ltd; the number average molecular weight of the polyethylene glycol succinate is 500, the CAS number is 25777-14-4, and the polyethylene glycol succinate is purchased from Beijing carboline science and technology Co., ltd;
the small molecular chain extender is a small molecular compound containing amino or hydroxyl on a molecular chain, and is a glycol compound with the number average molecular weight range of 80-200 as a preferable technical scheme;
as a preferable technical scheme, the dihydric alcohol compound is at least one selected from 1, 4-butanediol, polyethylene glycol 200 and 1, 4-pentanediol; preferably, the dihydric alcohol compound is 1, 4-butanediol and polyethylene glycol 200, so that the hardness and flexibility of the polyurethane thermoplastic elastomer can be fully balanced, and the obtained product has moderate hardness, higher tensile strength and tensile elongation and tear resistance; the inventors have unexpectedly found that when the mass ratio of the glycol compound to 1, 4-butanediol to polyethylene glycol 200 is controlled to be (1-2): 1, the dispersibility of the system is improved, the compatibility among substances in the system is improved, and the stability of the system is further facilitated;
the CAS number of the 1, 4-butanediol is 110-63-4, and the 1, 4-butanediol is purchased from Shanghai Ala Biochemical technology Co., ltd;
the polyethylene glycol 200 has a CAS number of 25322-68-3, purchased from Sigma Aldrich trade Inc.;
the nano-particles have larger specific surface area and surface activity, so that the nano-particles have good compatibility with resin, and as a preferable technical scheme, the nano-filler is at least one selected from nano-silica, nano-titania, nano-zinc oxide, carbon nano-tubes and graphene; preferably, the nano-filler is a combination of nano-silica and nano-titania; the inventors have unexpectedly found that by controlling the mass ratio of the nano silicon dioxide to the nano titanium dioxide to be (0.8-1.2): (1-1.5) not only can be used as an ultraviolet screening agent, but also can help to improve the dispersibility of the system, and can also improve the toughness of the obtained thermoplastic polyurethane, which is probably caused by the fact that the polyurethane elastomer has improved dispersibility and absorbability of impact energy due to the existence of nano silicon dioxide and nano titanium dioxide, so that the toughness is improved;
the CAS number of the nano silicon dioxide is 7631-86-9, the grain diameter is 20nm, and the specific surface area is 145-160m 2 And/g, model XFI03, purchased from Jiangsu Xianfeng nanomaterials science and technology Co., ltd;
the CAS number of the nano titanium dioxide is 13463-67-7, the grain diameter is 20-40nm, and the specific surface area is 77.37m 2 And/g, model XFI02, purchased from Jiangsu Xianfeng nanomaterials science and technology Co., ltd;
although the ageing resistance of the polyurethane elastomer is closely related to the hard segment content of the polyurethane elastomer, in order to meet the needs of practical application, a protective agent is added on the basis of balancing the hardness and the flexibility of the polyurethane, and the protective agent at least comprises a flame retardant, an antioxidant and an ultraviolet absorber as a preferable technical scheme; preferably, the mass ratio of the flame retardant, the antioxidant and the ultraviolet absorber is (1-1.5): (0.8-1.2): 0.8, fully protecting the polyurethane elastomer, avoiding the safety problem caused by ultraviolet oxidation, high-temperature oxidation or flame retardation intolerance, and limiting the application of the polyurethane elastomer in the field of charging pile protection sleeves;
as a preferable technical scheme, the flame retardant is at least one of chlorinated paraffin, decabromodiphenyl ether, trichloroethyl phosphate and ammonium polyphosphate;
as a preferable technical scheme, the flame retardant is a composition of chlorinated paraffin and trichloroethyl phosphate; the mass ratio of the chlorinated paraffin to the trichloroethyl phosphate is 1: (1.2-1.8), phosphorus and chlorine coexist, the generated phosphorus chloride has larger vapor density, can cover the flame surface to isolate oxygen and dilute combustibles, and meanwhile, the generated hydrogen chloride can capture active free radicals to effectively improve the flame retardant property of the polyurethane elastomer;
preferably, the chlorinated paraffin is chlorinated paraffin with chlorine content of 50%, CAS number is 106232-86-4, purchased from Jinan Jinbang environmental protection technology Co., ltd;
the CAS number of the trichloroethyl phosphate is 115-96-8, and the trichloroethyl phosphate is purchased from Techniaria (Shanghai) chemical industry development Co., ltd;
as a preferable technical scheme, the antioxidant is at least one selected from antioxidant 1076, antioxidant BHT, antioxidant 626 and antioxidant 1010;
preferably, the antioxidant is antioxidant 1076, and can cooperate with a flame retardant and an ultraviolet absorber in a system to protect the polyurethane elastomer to the greatest extent, so that the polyurethane elastomer is better suitable for a charging pile protective sleeve;
the antioxidant 1076 has CAS number 2082-79-3 and is purchased from Hefeijian chemical company;
as a preferable embodiment, the ultraviolet absorber is at least one selected from the group consisting of ultraviolet absorber UV-531, ultraviolet absorber UV-9, ultraviolet absorber UVP-327, and ultraviolet absorber RMB;
preferably, the ultraviolet absorber is ultraviolet absorber UV-531, has good compatibility with various substances in a system, is nontoxic and easy to process, can absorb 240-340 nanometers of ultraviolet light, delays yellowing of the polyurethane elastomer and protects the polyurethane elastomer from physical property loss caused by ultraviolet oxidation;
the CAS number of the ultraviolet absorber UV-531 is 1843-05-6, and the ultraviolet absorber UV-531 is purchased from Hubei Makesi refinement technology Co., ltd;
as a preferable technical scheme, the compatilizer is polyethylene glycol with a hydroxyl value of 120-600mg KOH/g;
as a preferable technical scheme, the polyethylene glycol is at least one selected from polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and polyethylene glycol 800;
preferably, the polyethylene glycol is polyethylene glycol-400, which is helpful for improving the dispersibility and compatibility of the system, maintaining the stability of the system and ensuring the application of the polyurethane elastomer;
the application also provides a preparation method of the thermoplastic polyurethane elastomer for the charging pile sheath, which at least comprises the following steps:
s1, according to the weight parts or the proportion, adding a long-chain polyol compound and a protective agent comprising a flame retardant, an antioxidant and an ultraviolet absorbent into a reaction kettle, mixing, controlling the rotating speed to be 1000-1500rpm, and stirring for 20-40min to obtain a long-chain polyol mixture;
s2, controlling the temperature to be 90-110 ℃, adding isocyanate, nano filler and compatilizer into a reaction kettle, and reacting with the long-chain polyol mixture obtained in the step S1 to prepare polyurethane prepolymer;
s3, putting the polyurethane prepolymer prepared in the step S2 and the micromolecular chain extender into a double-screw extruder according to the proportion, reacting, controlling the reaction temperature to be 150-200 ℃, controlling the screw rotation speed to be 300-400rpm, extruding, granulating and underwater granulating after reacting for 50-80 seconds, dehumidifying and drying for 4-7 hours at 60-80 ℃, and finally packaging to obtain the thermoplastic polyurethane elastomer for the charging pile sheath.
The beneficial effects are that:
1. the application provides a thermoplastic polyurethane elastomer for a charging pile sheath, which not only has proper hardness, high tearing strength, high tensile strength and high elongation at break, but also has excellent flame retardance and ageing resistance, and meets the higher practical application requirement of the charging pile sheath;
2. the polyol compound and the diphenylmethane diisoacid ester are adopted to react, and the mass ratio of the long-chain polyol compound to the small-molecule chain extender is controlled to be (4-6): 1, the soft segment can be formed in polyurethane through the long-chain polyol compound to the greatest extent, and the hard segment can be formed in polyurethane through the small-molecule chain extender, so that the prepared thermoplastic polyurethane elastomer has moderate hardness and higher tear resistance, elongation at break and tensile strength;
3. the saturated aliphatic polyester polyol with the number average molecular weight ranging from 500 to 2000 is adopted as a long-chain polyol compound, so that the production period can be shortened and the production efficiency of the product can be improved on the premise of ensuring that the product is easy to process and high in yield; and the mass ratio of the poly (1-3) adipic acid-1, 4-butanediol ester, the poly (1, 4-butanediol adipate) glycol and the poly (ethylene succinate) is controlled to be: 1:0.8, the hardness and softness of the polyurethane thermoplastic elastomer can be improved to the greatest extent, and the balance of the hardness and the flexibility of the polyurethane thermoplastic elastomer is realized under the action of the small molecule chain extender;
4. the combination of nano silicon dioxide and nano titanium dioxide is adopted as nano filler, and the mass ratio of the nano silicon dioxide to the nano titanium dioxide is controlled to be (0.8-1.2): (1-1.5) not only can be used as an ultraviolet screening agent, but also can help to improve the dispersibility of the system and can also increase the toughness of the obtained thermoplastic polyurethane;
5. flame retardant, antioxidant and ultraviolet absorbent are adopted as protective agents, and the mass ratio of the flame retardant, the antioxidant and the ultraviolet absorbent is controlled to be (1-1.5): (0.8-1.2): and 0.8, the polyurethane elastomer is fully protected, and the safety problem caused by ultraviolet oxidation, high-temperature oxidation or flame retardation is avoided, so that the obtained polyurethane elastomer is better suitable for the field of charging pile protection sleeves.
Detailed Description
Examples
Example 1
In one aspect, embodiment 1 of the application provides a thermoplastic polyurethane elastomer for a charging pile sheath, which comprises the following components in parts by weight: 50 parts of isocyanate, 80 parts of polyalcohol compounds, 3 parts of nanofiller, 8 parts of protective agent and 0.3 part of compatilizer;
the isocyanate is diphenyl methane diisoacid ester;
the CAS number of the diphenylmethane diisoacid ester is 101-68-8, and the diphenylmethane diisoacid ester is purchased from Shanghai Ala Biochemical technology Co., ltd;
the polyalcohol compound comprises a long-chain polyalcohol compound and a small-molecule chain extender; the mass ratio of the long-chain polyol compound to the small-molecule chain extender is 5:1, a step of;
the long chain polyol compound is a saturated aliphatic polyester polyol with a number average molecular weight ranging from 500 to 2000;
the saturated aliphatic polyester polyol is a combination of poly (1, 4-butanediol adipate), poly (1, 4-butanediol adipate) glycol and poly (ethylene succinate);
the mass ratio of the poly (1, 4-butanediol adipate) to the poly (1, 4-butanediol adipate) glycol to the poly (ethylene succinate) is 2:1:0.8;
the number average molecular weight of the poly (1, 4-butanediol adipate) is 2000, the CAS number is 150923-12-9, and the poly (1, 4-butanediol adipate) is purchased from Shanghai Michelin Biochemical technology Co., ltd; the number average molecular weight of the poly (1, 4-butanediol adipate) glycol is 1000, the model is HY-1022, and the poly (1, 4-butanediol adipate) glycol is purchased from Xuzhou bright Huiyang New material Co., ltd; the number average molecular weight of the polyethylene glycol succinate is 500, the CAS number is 25777-14-4, and the polyethylene glycol succinate is purchased from Beijing carboline science and technology Co., ltd;
the small molecular chain extender is a dihydric alcohol compound with the number average molecular weight range of 80-200;
the dihydric alcohol compound is 1, 4-butanediol and polyethylene glycol 200; the mass ratio of the 1, 4-butanediol to the polyethylene glycol 200 is 1.5:1, a step of;
the CAS number of the 1, 4-butanediol is 110-63-4, and the 1, 4-butanediol is purchased from Shanghai Ala Biochemical technology Co., ltd;
the polyethylene glycol 200 has a CAS number of 25322-68-3, purchased from Sigma Aldrich trade Inc.;
the nano-filler is a combination of nano-silica and nano-titania; the mass ratio of the nano silicon dioxide to the nano titanium dioxide is 1:1.2;
the CAS number of the nano silicon dioxide is 7631-86-9, the grain diameter is 20nm, and the specific surface area is 145-160m 2 And/g, model XFI03, purchased from Jiangsu Xianfeng nanomaterials science and technology Co., ltd; the CAS number of the nano titanium dioxide is 13463-67-7, the grain diameter is 20-40nm, and the specific surface area is 77.37m 2 And/g, model XFI02, purchased from Jiangsu Xianfeng nanomaterials science and technology Co., ltd;
the protective agent comprises a flame retardant, an antioxidant and an ultraviolet absorber; the mass ratio of the flame retardant to the antioxidant to the ultraviolet absorber is 1.3:1.1:0.8;
the flame retardant is a composition of chlorinated paraffin and trichloroethyl phosphate; the mass ratio of the chlorinated paraffin to the trichloroethyl phosphate is 1:1.6;
the chlorinated paraffin is chlorinated paraffin with chlorine content of 50%, CAS number is 106232-86-4, purchased from Jinan Jinbang environmental protection technology Co., ltd; the CAS number of the trichloroethyl phosphate is 115-96-8, and the trichloroethyl phosphate is purchased from Techniaria (Shanghai) chemical industry development Co., ltd;
the antioxidant is an antioxidant 1076, the CAS number of the antioxidant 1076 is 2082-79-3, and the antioxidant is purchased from Hefeijian Tianjian chemical company;
the ultraviolet absorber is ultraviolet absorber UV-531, wherein the CAS number of the ultraviolet absorber UV-531 is 1843-05-6, and the ultraviolet absorber is purchased from the company of Mechikus refinement science and technology, inc. of Hubei;
the compatilizer is polyethylene glycol with a hydroxyl value of 120-600mg KOH/g;
the polyethylene glycol is polyethylene glycol-400, the CAS number is 25322-68-3, and the polyethylene glycol is purchased from sigma Aldrich trade company;
the embodiment 1 of the application provides a preparation method of a thermoplastic polyurethane elastomer for a charging pile sheath, which comprises the following steps:
s1, according to the weight parts or the proportion, adding a long-chain polyol compound and a protective agent comprising a flame retardant, an antioxidant and an ultraviolet absorbent into a reaction kettle, mixing, controlling the rotating speed to 1200rpm, and stirring for 30min to obtain a long-chain polyol mixture;
s2, controlling the temperature to be 100 ℃, adding isocyanate, nano filler and compatilizer into a reaction kettle, and reacting with the long-chain polyol mixture obtained in the step S1 to prepare polyurethane prepolymer;
s3, putting the polyurethane prepolymer prepared in the step S2 and the micromolecular chain extender into a double-screw extruder according to the proportion, reacting, controlling the reaction temperature to be 180 ℃, controlling the screw rotation speed to be 360rpm, extruding, granulating and underwater granulating after 60S of reaction, dehumidifying and drying for 5h at 70 ℃, and finally packaging to obtain the thermoplastic polyurethane elastomer for the charging pile sheath.
Example 2
In one aspect, embodiment 2 of the application provides a thermoplastic polyurethane elastomer for a charging pile sheath, which comprises the following components in parts by weight: 60 parts of isocyanate, 90 parts of polyalcohol compounds, 6 parts of nanofiller, 10 parts of protective agent and 0.5 part of compatilizer;
the isocyanate is diphenyl methane diisoacid ester;
the CAS number of the diphenylmethane diisoacid ester is 101-68-8, and the diphenylmethane diisoacid ester is purchased from Shanghai Ala Biochemical technology Co., ltd;
the polyalcohol compound comprises a long-chain polyalcohol compound and a small-molecule chain extender; the mass ratio of the long-chain polyol compound to the small-molecule chain extender is 6:1, a step of;
the long chain polyol compound is a saturated aliphatic polyester polyol with a number average molecular weight ranging from 500 to 2000;
the saturated aliphatic polyester polyol is a combination of poly (1, 4-butanediol adipate), poly (1, 4-butanediol adipate) glycol and poly (ethylene succinate);
the mass ratio of the poly (1, 4-butanediol adipate) to the poly (1, 4-butanediol adipate) glycol to the poly (ethylene succinate) is 3:1:0.8;
the number average molecular weight of the poly (1, 4-butanediol adipate) is 2000, the CAS number is 150923-12-9, and the poly (1, 4-butanediol adipate) is purchased from Shanghai Michelin Biochemical technology Co., ltd; the number average molecular weight of the poly (1, 4-butanediol adipate) glycol is 1000, the model is HY-1022, and the poly (1, 4-butanediol adipate) glycol is purchased from Xuzhou bright Huiyang New material Co., ltd; the number average molecular weight of the polyethylene glycol succinate is 500, the CAS number is 25777-14-4, and the polyethylene glycol succinate is purchased from Beijing carboline science and technology Co., ltd;
the small molecular chain extender is a dihydric alcohol compound with the number average molecular weight range of 80-200;
the dihydric alcohol compound is 1, 4-butanediol and polyethylene glycol 200; the mass ratio of the 1, 4-butanediol to the polyethylene glycol 200 is 2:1, a step of;
the CAS number of the 1, 4-butanediol is 110-63-4, and the 1, 4-butanediol is purchased from Shanghai Ala Biochemical technology Co., ltd;
the polyethylene glycol 200 has a CAS number of 25322-68-3, purchased from Sigma Aldrich trade Inc.;
the nano-filler is a combination of nano-silica and nano-titania; the mass ratio of the nano silicon dioxide to the nano titanium dioxide is 1.2:1.5;
the CAS number of the nano silicon dioxide is 7631-86-9, the grain diameter is 20nm, and the specific surface area is 145-160m 2 And/g, model XFI03, purchased from Jiangsu Xianfeng nanomaterials science and technology Co., ltd; the CAS number of the nano titanium dioxide is 13463-67-7, the grain diameter is 20-40nm, and the specific surface area is 77.37m 2 And/g, model XFI02, purchased from Jiangsu Xianfeng nanomaterials science and technology Co., ltd;
the protective agent comprises a flame retardant, an antioxidant and an ultraviolet absorber; the mass ratio of the flame retardant to the antioxidant to the ultraviolet absorber is 1.5:1.2:0.8;
the flame retardant is a composition of chlorinated paraffin and trichloroethyl phosphate; the mass ratio of the chlorinated paraffin to the trichloroethyl phosphate is 1:1.8;
the chlorinated paraffin is chlorinated paraffin with chlorine content of 50%, CAS number is 106232-86-4, purchased from Jinan Jinbang environmental protection technology Co., ltd; the CAS number of the trichloroethyl phosphate is 115-96-8, and the trichloroethyl phosphate is purchased from Techniaria (Shanghai) chemical industry development Co., ltd;
the antioxidant is an antioxidant 1076, the CAS number of the antioxidant 1076 is 2082-79-3, and the antioxidant is purchased from Hefeijian Tianjian chemical company;
the ultraviolet absorber is ultraviolet absorber UV-531, wherein the CAS number of the ultraviolet absorber UV-531 is 1843-05-6, and the ultraviolet absorber is purchased from the company of Mechikus refinement science and technology, inc. of Hubei;
the compatilizer is polyethylene glycol with a hydroxyl value of 120-600mg KOH/g;
the polyethylene glycol is polyethylene glycol-400, the CAS number is 25322-68-3, and the polyethylene glycol is purchased from sigma Aldrich trade company;
the embodiment 2 of the application provides a preparation method of a thermoplastic polyurethane elastomer for a charging pile sheath, which comprises the following steps:
s1, according to the weight parts or the proportion, adding a long-chain polyol compound and a protective agent comprising a flame retardant, an antioxidant and an ultraviolet absorbent into a reaction kettle, mixing, controlling the rotating speed to 1200rpm, and stirring for 30min to obtain a long-chain polyol mixture;
s2, controlling the temperature to be 100 ℃, adding isocyanate, nano filler and compatilizer into a reaction kettle, and reacting with the long-chain polyol mixture obtained in the step S1 to prepare polyurethane prepolymer;
s3, putting the polyurethane prepolymer prepared in the step S2 and the micromolecular chain extender into a double-screw extruder according to the proportion, reacting, controlling the reaction temperature to be 180 ℃, controlling the screw rotation speed to be 360rpm, extruding, granulating and underwater granulating after 60S of reaction, dehumidifying and drying for 5h at 70 ℃, and finally packaging to obtain the thermoplastic polyurethane elastomer for the charging pile sheath.
Example 3
In one aspect, embodiment 3 of the application provides a thermoplastic polyurethane elastomer for a charging pile sheath, which comprises the following components in parts by weight: 40 parts of isocyanate, 60 parts of polyalcohol compounds, 1 part of nano filler, 5 parts of protective agent and 0.1 part of compatilizer;
the isocyanate is diphenyl methane diisoacid ester;
the CAS number of the diphenylmethane diisoacid ester is 101-68-8, and the diphenylmethane diisoacid ester is purchased from Shanghai Ala Biochemical technology Co., ltd;
the polyalcohol compound comprises a long-chain polyalcohol compound and a small-molecule chain extender; the mass ratio of the long-chain polyol compound to the small-molecule chain extender is 4:1, a step of;
the long chain polyol compound is a saturated aliphatic polyester polyol with a number average molecular weight ranging from 500 to 2000;
the saturated aliphatic polyester polyol is a combination of poly (1, 4-butanediol adipate), poly (1, 4-butanediol adipate) glycol and poly (ethylene succinate);
the mass ratio of the poly (1, 4-butanediol adipate) to the poly (1, 4-butanediol adipate) glycol to the poly (ethylene succinate) is 1:1:0.8;
the number average molecular weight of the poly (1, 4-butanediol adipate) is 2000, the CAS number is 150923-12-9, and the poly (1, 4-butanediol adipate) is purchased from Shanghai Michelin Biochemical technology Co., ltd; the number average molecular weight of the poly (1, 4-butanediol adipate) glycol is 1000, the model is HY-1022, and the poly (1, 4-butanediol adipate) glycol is purchased from Xuzhou bright Huiyang New material Co., ltd; the number average molecular weight of the polyethylene glycol succinate is 500, the CAS number is 25777-14-4, and the polyethylene glycol succinate is purchased from Beijing carboline science and technology Co., ltd;
the small molecular chain extender is a dihydric alcohol compound with the number average molecular weight range of 80-200;
the dihydric alcohol compound is 1, 4-butanediol and polyethylene glycol 200; the mass ratio of the 1, 4-butanediol to the polyethylene glycol 200 is 1:1, a step of;
the CAS number of the 1, 4-butanediol is 110-63-4, and the 1, 4-butanediol is purchased from Shanghai Ala Biochemical technology Co., ltd;
the polyethylene glycol 200 has a CAS number of 25322-68-3, purchased from Sigma Aldrich trade Inc.;
the nano-filler is a combination of nano-silica and nano-titania; the mass ratio of the nano silicon dioxide to the nano titanium dioxide is 0.8:1, a step of;
the CAS number of the nano silicon dioxide is 7631-86-9, the grain diameter is 20nm, and the specific surface area is 145-160m 2 And/g, model XFI03, purchased from Jiangsu Xianfeng nanomaterials science and technology Co., ltd; the CAS number of the nano titanium dioxide is 13463-67-7, the grain diameter is 20-40nm, and the specific surface area is 77.37m 2 And/g, model XFI02, purchased from Jiangsu Xianfeng nanomaterials science and technology Co., ltd;
the protective agent comprises a flame retardant, an antioxidant and an ultraviolet absorber; the mass ratio of the flame retardant to the antioxidant to the ultraviolet absorber is 1:0.8:0.8;
the flame retardant is a composition of chlorinated paraffin and trichloroethyl phosphate; the mass ratio of the chlorinated paraffin to the trichloroethyl phosphate is 1:1.2;
the chlorinated paraffin is chlorinated paraffin with chlorine content of 50%, CAS number is 106232-86-4, purchased from Jinan Jinbang environmental protection technology Co., ltd; the CAS number of the trichloroethyl phosphate is 115-96-8, and the trichloroethyl phosphate is purchased from Techniaria (Shanghai) chemical industry development Co., ltd;
the antioxidant is an antioxidant 1076, the CAS number of the antioxidant 1076 is 2082-79-3, and the antioxidant is purchased from Hefeijian Tianjian chemical company;
the ultraviolet absorber is ultraviolet absorber UV-531, wherein the CAS number of the ultraviolet absorber UV-531 is 1843-05-6, and the ultraviolet absorber is purchased from the company of Mechikus refinement science and technology, inc. of Hubei;
the compatilizer is polyethylene glycol with a hydroxyl value of 120-600mg KOH/g;
the polyethylene glycol is polyethylene glycol-400, the CAS number is 25322-68-3, and the polyethylene glycol is purchased from sigma Aldrich trade company;
the embodiment 3 of the application provides a preparation method of a thermoplastic polyurethane elastomer for a charging pile sheath, which comprises the following steps:
s1, according to the weight parts or the proportion, adding a long-chain polyol compound and a protective agent comprising a flame retardant, an antioxidant and an ultraviolet absorbent into a reaction kettle, mixing, controlling the rotating speed to 1200rpm, and stirring for 30min to obtain a long-chain polyol mixture;
s2, controlling the temperature to be 100 ℃, adding isocyanate, nano filler and compatilizer into a reaction kettle, and reacting with the long-chain polyol mixture obtained in the step S1 to prepare polyurethane prepolymer;
s3, putting the polyurethane prepolymer prepared in the step S2 and the micromolecular chain extender into a double-screw extruder according to the proportion, reacting, controlling the reaction temperature to be 180 ℃, controlling the screw rotation speed to be 360rpm, extruding, granulating and underwater granulating after 60S of reaction, dehumidifying and drying for 5h at 70 ℃, and finally packaging to obtain the thermoplastic polyurethane elastomer for the charging pile sheath.
Comparative example 1
The comparative example 1 of the present application provides a thermoplastic polyurethane elastomer for a charging pile sheath, and the specific embodiment of the thermoplastic polyurethane elastomer is the same as example 1, wherein the mass ratio of the long-chain polyol compound to the small-molecule chain extender is 3:1.
comparative example 2
Comparative example 2 of the present application provides a thermoplastic polyurethane elastomer for a charging pile cover, which has the same specific embodiment as example 1, except that the saturated aliphatic polyester polyol is poly (1, 4-butylene adipate).
Comparative example 3
Comparative example 3 of the present application provides a thermoplastic polyurethane elastomer for a charging pile cover, and its specific embodiment is the same as example 1, except that the glycol compound is 1, 4-butanediol.
Comparative example 4
Comparative example 4 of the present application provides a thermoplastic polyurethane elastomer for a charging pile cover, which is different from example 1 in that the thermoplastic polyurethane elastomer is prepared from raw materials not including nanofillers.
Comparative example 5
Comparative example 5 of the present application provides a thermoplastic polyurethane elastomer for a charging pile sheath, and its specific embodiment is the same as example 1, except that the flame retardant is chlorinated paraffin.
Performance test method
(1) Shore hardness: the Shore hardness of the polyurethane thermoplastic elastomers prepared in examples and comparative examples was measured with reference to ASTM D2240;
(2) Tensile strength: tensile strength performance tests were performed on the polyurethane thermoplastic elastomers prepared in examples and comparative examples, with reference to ASTM D412;
(3) Elongation at break: the elongation at break of the polyurethane thermoplastic elastomers prepared in examples and comparative examples was measured with reference to ASTM D412;
(4) Tear strength: the tear strength of the polyurethane thermoplastic elastomers prepared in examples and comparative examples was measured with reference to ASTM D624;
(5) Flame retardant properties: limiting oxygen index characterization the limiting oxygen index of the polyurethane thermoplastic elastomers prepared in the examples and comparative examples was measured according to the GB/T2406-1993 standard method.
Performance test data
The polyurethane thermoplastic elastomers prepared in examples 1 to 3 and comparative examples 1 to 5 were subjected to performance evaluation.
Referring to Table 1, table 1 shows the performance test data of the polyurethane thermoplastic elastomers prepared in examples 1 to 3 and comparative examples 1 to 5.

Claims (2)

1. The thermoplastic polyurethane elastomer for the charging pile sheath is characterized by comprising the following preparation raw materials in parts by weight: 40 to 60 parts of isocyanate, 60 to 90 parts of polyalcohol compounds, 1 to 6 parts of nano-filler, 5 to 10 parts of protective agent and 0.1 to 0.5 part of compatilizer;
the isocyanate is diphenyl methane diisoacid ester;
the polyol compound at least comprises a long-chain polyol compound and a small-molecule chain extender, wherein the mass ratio of the long-chain polyol compound to the small-molecule chain extender is (4-6): 1, a step of;
the long chain polyol compound is a saturated aliphatic polyester polyol with a number average molecular weight ranging from 500 to 2000; the saturated aliphatic polyester polyol is a combination of poly (1, 4-butanediol adipate), poly (1, 4-butanediol adipate) glycol and poly (ethylene succinate), and the mass ratio of the poly (1, 4-butanediol adipate), the poly (1, 4-butanediol adipate) glycol to the poly (ethylene succinate) is (1-3): 1:0.8;
the small molecular chain extender is a dihydric alcohol compound with the number average molecular weight range of 80-200, the dihydric alcohol compound is a combination of 1, 4-butanediol and polyethylene glycol 200, and the mass ratio of the 1, 4-butanediol to the polyethylene glycol 200 is (1-2): 1, a step of;
the nano filler is a combination of nano silicon dioxide and nano titanium dioxide, and the mass ratio of the nano silicon dioxide to the nano titanium dioxide is (0.8-1.2): (1-1.5);
the protective agent is a combination of a flame retardant, an antioxidant and an ultraviolet absorber, and the mass ratio of the flame retardant to the antioxidant to the ultraviolet absorber is (1-1.5): (0.8-1.2): 0.8; the flame retardant is a composition of chlorinated paraffin and trichloroethyl phosphate; the mass ratio of the chlorinated paraffin to the trichloroethyl phosphate is 1: (1.2-1.8); the antioxidant is antioxidant 1076, and the ultraviolet absorbent is ultraviolet absorbent UV-531.
2. A method for preparing a thermoplastic polyurethane elastomer for a charging pile sheath according to claim 1, comprising at least the following steps:
s1, according to the weight parts or the proportion, putting a long-chain polyol compound and a protective agent into a reaction kettle for mixing, controlling the rotating speed to be 1000-1500rpm, and stirring for 20-40min to obtain a long-chain polyol mixture;
s2, controlling the temperature to be 90-110 ℃, adding isocyanate, nano filler and compatilizer into a reaction kettle, and reacting with the long-chain polyol mixture obtained in the step S1 to prepare polyurethane prepolymer;
s3, putting the polyurethane prepolymer and the micromolecular chain extender which are preliminarily prepared in the step S2 into a double-screw extruder for reaction according to the proportion, controlling the reaction temperature to be 150-200 ℃, controlling the screw rotation speed to be 300-400rpm, extruding, granulating and underwater granulating after the reaction for 50-80S, dehumidifying and drying for 4-7h at 60-80 ℃, and finally packaging to obtain the thermoplastic polyurethane elastomer for the charging pile sheath.
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Denomination of invention: A thermoplastic polyurethane elastomer for charging pile cover and its preparation method

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