CN109679061B - Thermoplastic polyurethane elastomer for flexible electrothermal film and preparation method thereof - Google Patents
Thermoplastic polyurethane elastomer for flexible electrothermal film and preparation method thereof Download PDFInfo
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- CN109679061B CN109679061B CN201811581617.1A CN201811581617A CN109679061B CN 109679061 B CN109679061 B CN 109679061B CN 201811581617 A CN201811581617 A CN 201811581617A CN 109679061 B CN109679061 B CN 109679061B
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- thermoplastic polyurethane
- polyurethane elastomer
- electrothermal film
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- 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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- 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
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to the field of synthesis of high polymer materials, and particularly relates to a thermoplastic polyurethane elastomer for a flexible electrothermal film and a preparation method thereof. The thermoplastic polyurethane elastomer for the flexible electrothermal film is prepared from the following raw materials in percentage by mass and a catalyst: 52-61% of polyester polyol; 20-29% of diisocyanate; 4.5-7.0% of a chain extender; 0.1-0.5% of antioxidant; 0.1-0.5% of light stabilizer; 0.1-0.5% of a lubricant; 9-15% of a flame retardant; 0.1-0.5% of hydrolysis resistant agent; the dosage of the catalyst is 0.001-0.01% of the total mass of the raw materials; the flame retardant has high mechanical strength, stable high-temperature performance, excellent flame retardance, hydrolysis resistance and high voltage resistance; the preparation method has the advantages of simple and easy operation, low cost and no pollution.
Description
Technical Field
The invention belongs to the field of synthesis of high polymer materials, and particularly relates to a thermoplastic polyurethane elastomer for a flexible electrothermal film and a preparation method thereof.
Background
The flexible electric heating film is a planar heating film heating element, is suitable for all construction environments of common electric heating films due to good flexibility, conductivity and safety, can be directly laid on sofas, Simmons mattresses and the like, and can be used as heating bodies of heating mattresses, carbon fiber jade mattresses, automobile heating cushions, heating table and chair cushions, heating ground mats, heating foot pads, heating clothes and the like. The industrial field can also be used for mechanical heat preservation, water pipeline and oil field oil pipeline heat preservation. And snow melting and heat preservation of highways, ramps, curves, stadiums, airport runways and the like.
At present, an insulating material bottom die used by a flexible electric heating film comprises three types, namely silica gel, PI (polyimide) and PET (polyester), and the silica gel material has poor heat conductivity, so that local overheating and the absolute temperature of a heating body is overhigh to cause the aging of the insulating material; the PET material can resist the temperature of only 70 ℃ and can only be applied to low-temperature heating; the PI material has poor mechanical property and low mechanical strength. The three types of soft heating elements have the problems of no high temperature resistance, easy aging, easy hydrolysis or low mechanical strength due to the problems of the structure and the material, so that potential safety hazards exist in the use process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a thermoplastic polyurethane elastomer for a flexible electrothermal film, which has higher mechanical strength, stable high-temperature performance, excellent flame retardance, hydrolysis resistance and high voltage resistance; meanwhile, the invention also provides a preparation method of the compound, which is simple and easy to operate, low in cost and free of pollution.
The invention relates to a thermoplastic polyurethane elastomer for a flexible electric heating film, which is prepared from the following raw materials in percentage by mass and a catalyst:
the dosage of the catalyst is 0.001-0.01% of the total mass of the raw materials;
the polyester polyol is polyester diol, and the molecular weight of the polyester polyol is 1000-3000.
The polyester polyol is one, two or more of polyethylene glycol adipate glycol, polybutylene glycol adipate glycol or polyhexamethylene glycol adipate glycol, and the two or more of the two or more of the two or the two of the two or more of the two or the two of the two or the two of the two or the two of the two or the two of the two or the two of.
The diisocyanate is one of 4,4 '-diphenylmethane diisocyanate, phenylene-1, 4-diisocyanate, toluene diisocyanate, 1, 4-cyclohexyl-diisocyanate or decane-1, 10-diisocyanate, and is preferably 4,4' -diphenylmethane diisocyanate (MDI-100).
The chain extender is one, two or more of 1, 4-butanediol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 2-methyl-1, 3-propylene glycol or 1, 6-hexanediol, and the two or more can be mixed in any proportion.
The antioxidant is one, two or more of hindered phenol antioxidant, phosphite antioxidant or sulfur-containing antioxidant, and the two or more can be mixed at any ratio, preferably the antioxidant 1010, 1076, 168, 626, DLTDP or DMTDP.
The light stabilizer is one, two or more of Tinuvin770, Tinuvin234 or Tinuvin571, and the two or more of the Tinuvin770, the Tinuvin234 and the Tinuvin571 can be mixed in any proportion.
The lubricant is one, two or more of oleamide, erucamide, glycerin monostearate, polyethylene wax or montan wax, and the two or more of the oleamide, the erucamide, the glycerin monostearate, the polyethylene wax or the montan wax can be mixed at any ratio, and preferably E wax or OP wax produced by the Clariant company.
The flame retardant is a halogen-free environment-friendly flame retardant taking phosphorus and nitrogen as flame retardant elements, and preferably EPFR-400A produced by Puseofur company.
The hydrolysis resistant agent is one or two of monocarbodiimide or polycarbodiimide which are mixed in any proportion, preferably Stabaxol P200.
The catalyst is organic bismuth, organic tin or titanate catalyst.
The invention relates to a preparation method of a thermoplastic polyurethane elastomer for a flexible electrothermal film, which comprises the following steps:
(1) adding polyester polyol, an antioxidant, a light stabilizer, a lubricant, an anti-hydrolysis agent and a catalyst into a reaction kettle A, and uniformly mixing, wherein the set temperature is 100-115 ℃;
(2) adding diisocyanate into the reaction kettle B, and setting the temperature to be 65-75 ℃; adding the chain extender into a C reaction kettle, and setting the temperature to be 60-70 ℃;
(3) when the materials in each reaction kettle are uniformly stirred and the temperature is stable, raw materials in A, B and C reaction kettles are injected into a feeding port of a double-screw extruder through a filling system with accurate measurement, a flame retardant with accurate measurement is injected into the feeding port of the double-screw extruder, the mixture is uniformly reacted and plasticized in a cylinder of the double-screw extruder, and the mixture is cut into particles by an underwater granulator to obtain the thermoplastic polyurethane elastomer for the flexible electrothermal film.
Compared with the prior art, the invention has the following beneficial effects:
(1) the thermoplastic polyurethane elastomer for the flexible electrothermal film prepared by the invention has good flame retardant effect, the flame retardant grade can reach V0 grade, and the safe and practical requirements of the flexible electrothermal film are met;
(2) the thermoplastic polyurethane elastomer for the flexible electrothermal film prepared by the invention has stronger hydrolytic resistance, and ensures the use safety under the high humidity and heat condition;
(3) the thermoplastic polyurethane elastomer for the flexible electrothermal film, prepared by the invention, has lower deformation rate under the high-temperature condition, high-temperature aging resistance, no deterioration and stable performance, and prolongs the service life;
(4) the thermoplastic polyurethane elastomer for the flexible electrothermal film, prepared by the invention, has high voltage resistance, can bear a test voltage of 3500V without damage, and has higher mechanical strength;
(5) the preparation method provided by the invention is simple and feasible to operate, low in cost and free of pollution.
Detailed Description
The present invention will be further described with reference to the following examples.
All the starting materials used in the examples are commercially available, except where otherwise indicated.
Example 1
A thermoplastic polyurethane elastomer for a flexible electrothermal film is prepared from the following raw materials in percentage by weight and a catalyst:
the dosage of the catalyst stannous octoate (T-9) is 0.005 percent of the total mass of the used raw materials;
the molecular weight of the polybutylene adipate glycol is 2000.
The preparation method comprises the following steps:
(1) adding polybutylene adipate glycol, an antioxidant 1010, an antioxidant 626, Tinuvin770, E wax, OP wax, Stabaxol P200 and T-9 into a reaction kettle A, and uniformly mixing, wherein the set temperature is 100 ℃;
(2) adding MDI-100 into a reaction kettle B, and setting the temperature to 65 ℃; adding 1, 6-hexanediol into a C reaction kettle, and setting the temperature to be 60 ℃;
(3) when the materials in each reaction kettle are uniformly stirred and the temperature is stable, raw materials in A, B and C reaction kettles are injected into a feeding port of a double-screw extruder through a filling system with accurate measurement, EPFR-400A with accurate measurement is injected into the feeding port of the double-screw extruder, the mixture is uniformly reacted and plasticized in a cylinder of the double-screw extruder, and the mixture is cut into particles by an underwater granulator to obtain the thermoplastic polyurethane elastomer for the flexible electrothermal film.
Example 2
A thermoplastic polyurethane elastomer for a flexible electrothermal film is prepared from the following raw materials in percentage by weight and a catalyst:
the dosage of the catalyst stannous octoate (T-9) is 0.005 percent of the total mass of the used raw materials;
the molecular weight of the polybutylene adipate glycol is 1000.
The preparation method comprises the following steps:
(1) adding polybutylene adipate glycol, an antioxidant 1010, an antioxidant 626, Tinuvin770, E wax, OP wax, Stabaxol P200 and T-9 into a reaction kettle A, and uniformly mixing, wherein the set temperature is 105 ℃;
(2) adding MDI-100 into a reaction kettle B, and setting the temperature to be 75 ℃; adding 1, 6-hexanediol into a C reaction kettle, and setting the temperature to 65 ℃;
(3) when the materials in each reaction kettle are uniformly stirred and the temperature is stable, raw materials in A, B and C reaction kettles are injected into a feeding port of a double-screw extruder through a filling system with accurate measurement, EPFR-400A with accurate measurement is injected into the feeding port of the double-screw extruder, the mixture is uniformly reacted and plasticized in a cylinder of the double-screw extruder, and the mixture is cut into particles by an underwater granulator to obtain the thermoplastic polyurethane elastomer for the flexible electrothermal film.
Example 3
A thermoplastic polyurethane elastomer for a flexible electrothermal film is prepared from the following raw materials in percentage by weight and a catalyst:
the dosage of the catalyst stannous octoate (T-9) is 0.005 percent of the total mass of the used raw materials;
the molecular weight of the polybutylene adipate glycol is 3000.
The preparation method comprises the following steps:
(1) adding polybutylene adipate glycol, an antioxidant 1010, an antioxidant 626, Tinuvin770, E wax, OP wax, Stabaxol P200 and T-9 into a reaction kettle A, and uniformly mixing, wherein the set temperature is 110 ℃;
(2) adding MDI-100 into a reaction kettle B, and setting the temperature to be 70 ℃; adding 1, 4-butanediol into a C reaction kettle, and setting the temperature to be 70 ℃;
(3) when the materials in each reaction kettle are uniformly stirred and the temperature is stable, raw materials in A, B and C reaction kettles are injected into a feeding port of a double-screw extruder through a filling system with accurate measurement, EPFR-400A with accurate measurement is injected into the feeding port of the double-screw extruder, the mixture is uniformly reacted and plasticized in a cylinder of the double-screw extruder, and the mixture is cut into particles by an underwater granulator to obtain the thermoplastic polyurethane elastomer for the flexible electrothermal film.
Example 4
A thermoplastic polyurethane elastomer for a flexible electrothermal film is prepared from the following raw materials in percentage by weight and a catalyst:
the dosage of the catalyst stannous octoate (T-9) is 0.005 percent of the total mass of the used raw materials;
the molecular weight of the polybutylene adipate glycol is 1000.
The preparation method comprises the following steps:
(1) adding polybutylene adipate glycol, an antioxidant 1010, an antioxidant 626, Tinuvin770, E wax, OP wax, Stabaxol P200 and T-9 into a reaction kettle A, and uniformly mixing, wherein the set temperature is 115 ℃;
(2) adding MDI-100 into a reaction kettle B, and setting the temperature to be 70 ℃; adding 1, 4-butanediol into a C reaction kettle, and setting the temperature to 65 ℃;
(3) when the materials in each reaction kettle are uniformly stirred and the temperature is stable, raw materials in A, B and C reaction kettles are injected into a feeding port of a double-screw extruder through a filling system with accurate measurement, EPFR-400A with accurate measurement is injected into the feeding port of the double-screw extruder, the mixture is uniformly reacted and plasticized in a cylinder of the double-screw extruder, and the mixture is cut into particles by an underwater granulator to obtain the thermoplastic polyurethane elastomer for the flexible electrothermal film.
Comparative example
A thermoplastic polyurethane elastomer for a flexible electrothermal film is prepared from the following raw materials in percentage by weight and a catalyst:
the dosage of the catalyst stannous octoate (T-9) is 0.005 percent of the total mass of the used raw materials;
the molecular weight of the polybutylene adipate glycol is 1000.
The preparation method comprises the following steps:
(1) adding polybutylene adipate glycol, an antioxidant 1010, Tinuvin770 and T-9 into a reaction kettle A, and uniformly mixing, wherein the temperature is set to be 115 ℃;
(2) adding MDI-100 into a reaction kettle B, and setting the temperature to be 70 ℃; adding 1, 4-butanediol into a C reaction kettle, and setting the temperature to 65 ℃;
(3) and after the materials in each reaction kettle are uniformly stirred and the temperature is stable, injecting the raw materials in the A, B and C reaction kettles into a feeding port of a double-screw extruder through a filling system with accurate measurement, uniformly reacting and plasticizing in a cylinder of the double-screw extruder, and granulating by an underwater granulator to obtain the thermoplastic polyurethane elastomer for the flexible electrothermal film.
Thermoplastic polyurethane elastomer performance detection for flexible electrothermal film
The performance of the thermoplastic polyurethane elastomer for the flexible electrothermal film prepared in the embodiments 1 to 4 and the comparative example was tested, and the test results are shown in table 1.
Remarking: the hydrolysis conditions were 85 ℃ and 85% RH for 28 days.
TABLE 1
As can be seen from the data in Table 1, the thermoplastic polyurethane elastomer for the flexible electrothermal film prepared by the invention has higher mechanical strength, stable high-temperature performance and excellent flame retardance and hydrolysis resistance, is not damaged by a 3500V high-voltage breakdown test, and can meet the use requirement of the flexible electrothermal film.
Claims (6)
1. A thermoplastic polyurethane elastomer for a flexible electrothermal film, characterized in that: the catalyst is prepared from the following raw materials in percentage by mass and a catalyst, wherein the raw materials comprise:
52 to 61 percent of polyester polyol
20-29% of diisocyanate
Chain extender 4.5-7.0%
0.1 to 0.5 percent of antioxidant
0.1 to 0.5 percent of light stabilizer
0.1 to 0.5 percent of lubricant
9-15% of flame retardant
0.1-0.5% of hydrolysis resistant agent;
the dosage of the catalyst is 0.001-0.01% of the total mass of the raw materials;
the polyester polyol is polyester diol, and the molecular weight of the polyester polyol is 1000-3000;
the lubricant is E wax and OP wax;
the flame retardant is EPFR-400A;
the hydrolysis resistant agent is Stabaxol P200;
the preparation method of the thermoplastic polyurethane elastomer for the flexible electrothermal film comprises the following steps:
(1) adding polyester polyol, an antioxidant, a light stabilizer, a lubricant, an anti-hydrolysis agent and a catalyst into a reaction kettle A, and setting the temperature to be 100-115 ℃;
(2) adding diisocyanate into the reaction kettle B, and setting the temperature to be 65-75 ℃; adding the chain extender into a C reaction kettle, and setting the temperature to be 60-70 ℃;
(3) and (3) adding the raw materials in the A, B and the C reaction kettle into a double-screw extruder, simultaneously adding the flame retardant into the double-screw extruder for reaction and plasticization, and granulating by using an underwater granulator to obtain the thermoplastic polyurethane elastomer for the flexible electrothermal film.
2. The thermoplastic polyurethane elastomer for a flexible electrothermal film according to claim 1, wherein: the polyester polyol is one or more of polyethylene glycol adipate glycol, polybutylene glycol adipate glycol or polyhexamethylene glycol adipate glycol.
3. The thermoplastic polyurethane elastomer for a flexible electrothermal film according to claim 1, wherein: the diisocyanate is 4,4' -diphenylmethane diisocyanate, phenylene-1, 4-diisocyanate, toluene diisocyanate, 1, 4-cyclohexyl-diisocyanate or decane-1, 10-diisocyanate.
4. The thermoplastic polyurethane elastomer for a flexible electrothermal film according to claim 1, wherein: the chain extender is one or more of 1, 4-butanediol, ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 2-methyl-1, 3-propylene glycol or 1, 6-hexanediol; the antioxidant is one or more of hindered phenol antioxidant, phosphite antioxidant or sulfur-containing antioxidant.
5. The thermoplastic polyurethane elastomer for a flexible electrothermal film according to claim 1, wherein: the light stabilizer is one or more of Tinuvin770, Tinuvin234 or Tinuvin 571.
6. The thermoplastic polyurethane elastomer for a flexible electrothermal film according to claim 1, wherein: the catalyst is organic bismuth, organic tin or titanate catalyst.
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CN110845694A (en) * | 2019-11-08 | 2020-02-28 | 浙江华峰热塑性聚氨酯有限公司 | Thermoplastic polyurethane capable of carrying out light transmission and preparation method thereof |
CN112375202A (en) * | 2020-11-30 | 2021-02-19 | 山东一诺威聚氨酯股份有限公司 | Thermoplastic polyurethane elastomer for light guide strip and preparation method thereof |
CN112574678A (en) * | 2020-11-30 | 2021-03-30 | 山东一诺威聚氨酯股份有限公司 | High-temperature-resistant water-washing TPU (thermoplastic polyurethane) hot melt adhesive film and preparation method thereof |
CN115141479B (en) * | 2022-09-01 | 2023-01-31 | 山东一诺威聚氨酯股份有限公司 | Modified TPU for encapsulating PC and preparation method thereof |
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