CN109679061A - Thermoplastic polyurethane elastomer and preparation method thereof for flexible electrothermal membrane - Google Patents
Thermoplastic polyurethane elastomer and preparation method thereof for flexible electrothermal membrane Download PDFInfo
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- CN109679061A CN109679061A CN201811581617.1A CN201811581617A CN109679061A CN 109679061 A CN109679061 A CN 109679061A CN 201811581617 A CN201811581617 A CN 201811581617A CN 109679061 A CN109679061 A CN 109679061A
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- Prior art keywords
- thermoplastic polyurethane
- polyurethane elastomer
- electrothermal membrane
- flexible electrothermal
- diisocyanate
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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
-
- 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
-
- 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 synthesis of polymer material fields, and in particular to a kind of thermoplastic polyurethane elastomer and preparation method thereof for flexible electrothermal membrane.The thermoplastic polyurethane elastomer for flexible electrothermal membrane is made: polyester polyol 52~61% of the raw material extra catalyst of following mass percent;Diisocyanate 20~29%;Chain extender 4.5~7.0%;Antioxidant 0.1~0.5%;Light stabilizer 0.1~0.5%;Lubricant 0.1~0.5%;Fire retardant 9~15%;Anti-hydrolysis agent 0.1~0.5%;The dosage of the catalyst is the 0.001~0.01% of above-mentioned raw materials used gross mass;Mechanical strength with higher, stable high-temperature behavior, excellent fire-retardant, hydrolysis and high voltage withstanding performance;The preparation method, operation is simple, at low cost, pollution-free.
Description
Technical field
The invention belongs to synthesis of polymer material fields, and in particular to a kind of thermoplastic polyurethane for flexible electrothermal membrane
Elastomer and preparation method thereof.
Background technique
Flexible electrothermal membrane is a kind of thin-film heating element of planar heating, because of its good flexibility, electric conductivity and peace
Full property is suitable for all construction environments of common Electric radiant Heating Film, can directly be layed in sofa, padding for spring bed etc., can be heating bed
Pad, carbon fiber jade mattress, automobile heating seat cushion, heating chair cushion, heating ground cushion, heating foot pad, heated clothing etc., which are done, to generate heat
Body.Industrial circle can also do mechanical heat preservation, waterpipe, the heat preservation of oil pipeline road.And highway, ramp, bend, sport
, snow melt heat preservation of airfield runway etc. etc..
Currently, insulating materials bed die used in flexible electrothermal membrane includes three categories, i.e. silica gel, PI (polyimides), PET
(polyester) three categories, silica gel material poor thermal conductivity easily cause hot-spot and heater absolute temperature are excessively high leads to insulating materials
Aging;PET material heatproof is only 70 DEG C, can only be in low-temperature heat application;The PI mechanical property of materials is poor, and mechanical strength is low.This three
The soft heating element of class, because there are non-refractories the problem of structure and material, easy to aging, facile hydrolysis or mechanical strength are low
The problem of, lead in use process that there are security risks.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of thermoplastic polyurethanes for flexible electrothermal membrane
Elastomer, mechanical strength with higher, stable high-temperature behavior, excellent fire-retardant, hydrolysis and high voltage withstanding performance;Simultaneously
The present invention also provides preparation methods, and operation is simple, at low cost, pollution-free.
Thermoplastic polyurethane elastomer of the present invention for flexible electrothermal membrane, by the raw material of following mass percent
Extra catalyst is made:
The dosage of the catalyst is the 0.001~0.01% of above-mentioned raw materials used gross mass;
The polyester polyol is polyester-diol, and molecular weight is 1000~3000.
The polyester polyol is polyethylene glycol adipate glycol, polybutylene glyool adipate or polyadipate
One of hexylene glycol esterdiol, two or more, two or more when can arbitrary proportion mixing.
The diisocyanate is 4,4'- methyl diphenylene diisocyanate, phenylene -1,4- diisocyanate, first
Phenylene diisocyanate, Isosorbide-5-Nitrae-one of cyclohexyl-diisocyanate or decane -1,10- diisocyanate, preferably 4,4'- bis-
Methylenebis phenyl isocyanate (MDI-100).
The chain extender is 1,4- butanediol, ethylene glycol, 1,2- propylene glycol, 1,3- propylene glycol, 2- methyl-1,3- the third two
Alcohol or 1, one of 6- hexylene glycol, two or more, two or more when can arbitrary proportion mixing.
The antioxidant be one of Hinered phenols antioxidant, phosphite ester antioxidant or sulfur-bearing antioxidant,
Two or more, two or more when can arbitrary proportion mixing, preferably antioxidant 1010,1076,168,626, DLTDP or
DMTDP。
The light stabilizer be one of Tinuvin770, Tinuvin234 or Tinuvin571, two or more,
Two or more when can arbitrary proportion mixing.
The lubricant is one in oleamide, erucyl amide, glycerin monostearate, polyethylene wax or montanin wax
Kind, two or more, two or more when can arbitrary proportion mixing, preferably Clariant Corporation production E wax or OP wax.
The fire retardant is using phosphorus, nitrogen as the halogen-free environment-friendly fire retardant of ignition-proof element, and preferably Pu Sai furan company is raw
The EPFR-400A of production.
The anti-hydrolysis agent is that one or both of single second carbide imine or polycarbodiimide are mixed with arbitrary proportion
It closes, preferably Stabaxol P200.
The catalyst is organo-bismuth, organotin or titanate ester catalyst.
Method for preparing thermoplastic polyurethane elastomer of the present invention for flexible electrothermal membrane, including following step
It is rapid:
(1) polyester polyol, antioxidant, light stabilizer, lubricant, anti-hydrolysis agent and catalyst are added to A reaction
It is uniformly mixed in kettle, setting temperature is 100~115 DEG C;
(2) diisocyanate is added in B reaction kettle, setting temperature is 65~75 DEG C;Chain extender is added to C reaction kettle
In, setting temperature is 60~70 DEG C;
(3) uniform to each reaction kettle material stirring, temperature is stablized, by having the perfusion system of accurate measurement, by A, B and
Raw material in C reaction kettle injects double screw extruder spout, and the fire retardant of accurate measurement injects double screw extruder spout,
Mixture homogeneous reaction, plasticizing in twin screw extruder barrel body, through underwater pelletizer pelletizing to get for flexible electrothermal membrane
Thermoplastic polyurethane elastomer.
Compared with prior art, beneficial effects of the present invention are as follows:
(1) thermoplastic polyurethane elastomer prepared by the present invention for flexible electrothermal membrane, good flame retardation effect, fire-retardant rank
It can reach V0 grades, meet the safe and practical requirement of flexible electrothermal membrane;
(2) thermoplastic polyurethane elastomer prepared by the present invention for flexible electrothermal membrane has stronger hydrolytic resistance
Can, it ensure that the safety used under high wet heat condition;
(3) thermoplastic polyurethane elastomer prepared by the present invention for flexible electrothermal membrane, under the high temperature conditions have compared with
Low deformation ratio, high-temperature aging resisting never degenerate, performance stabilization, extend service life;
(4) thermoplastic polyurethane elastomer prepared by the present invention for flexible electrothermal membrane has high voltage withstanding performance, can
The test voltage of 3500V is withstood up to without breakage, while having both higher mechanical strength;
(5) preparation method of the present invention, operation is simple, at low cost, pollution-free.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
All raw materials used in embodiment are commercially available unless otherwise specified.
Embodiment 1
A kind of thermoplastic polyurethane elastomer for flexible electrothermal membrane, by the additional catalysis of the raw material of following weight percent
Agent is made:
The dosage of octoate catalyst stannous (T-9) is the 0.005% of total mass of raw material used above;
The polybutylene glyool adipate molecular weight is 2000.
Preparation method:
(1) by polybutylene glyool adipate, antioxidant 1010, antioxidant 626, Tinuvin770, E wax, OP wax,
Stabaxol P200 and T-9 are added in A reaction kettle and are uniformly mixed, and setting temperature is 100 DEG C;
(2) MDI-100 is added in B reaction kettle, setting temperature is 65 DEG C;1,6- hexylene glycol is added in C reaction kettle,
It is 60 DEG C that temperature, which is arranged,;
(3) uniform to each reaction kettle material stirring, temperature is stablized, by having the perfusion system of accurate measurement, by A, B and
Raw material in C reaction kettle injects double screw extruder spout, and the EPFR-400A of accurate measurement injects double screw extruder feeding
Mouthful, mixture homogeneous reaction, plasticizing in twin screw extruder barrel body are used for flexible electric heating through underwater pelletizer pelletizing
The thermoplastic polyurethane elastomer of film.
Embodiment 2
A kind of thermoplastic polyurethane elastomer for flexible electrothermal membrane, by the additional catalysis of the raw material of following weight percent
Agent is made:
The dosage of octoate catalyst stannous (T-9) is the 0.005% of total mass of raw material used above;
The polybutylene glyool adipate molecular weight is 1000.
Preparation method:
(1) by polybutylene glyool adipate, antioxidant 1010, antioxidant 626, Tinuvin770, E wax, OP wax,
Stabaxol P200 and T-9 are added in A reaction kettle and are uniformly mixed, and setting temperature is 105 DEG C;
(2) MDI-100 is added in B reaction kettle, setting temperature is 75 DEG C;1,6- hexylene glycol is added in C reaction kettle,
It is 65 DEG C that temperature, which is arranged,;
(3) uniform to each reaction kettle material stirring, temperature is stablized, by having the perfusion system of accurate measurement, by A, B and
Raw material in C reaction kettle injects double screw extruder spout, and the EPFR-400A of accurate measurement injects double screw extruder feeding
Mouthful, mixture homogeneous reaction, plasticizing in twin screw extruder barrel body are used for flexible electric heating through underwater pelletizer pelletizing
The thermoplastic polyurethane elastomer of film.
Embodiment 3
A kind of thermoplastic polyurethane elastomer for flexible electrothermal membrane, by the additional catalysis of the raw material of following weight percent
Agent is made:
The dosage of octoate catalyst stannous (T-9) is the 0.005% of total mass of raw material used above;
The polybutylene glyool adipate molecular weight is 3000.
Preparation method:
(1) by polybutylene glyool adipate, antioxidant 1010, antioxidant 626, Tinuvin770, E wax, OP wax,
Stabaxol P200 and T-9 are added in A reaction kettle and are uniformly mixed, and setting temperature is 110 DEG C;
(2) MDI-100 is added in B reaction kettle, setting temperature is 70 DEG C;1,4-butanediol is added in C reaction kettle,
It is 70 DEG C that temperature, which is arranged,;
(3) uniform to each reaction kettle material stirring, temperature is stablized, by having the perfusion system of accurate measurement, by A, B and
Raw material in C reaction kettle injects double screw extruder spout, and the EPFR-400A of accurate measurement injects double screw extruder feeding
Mouthful, mixture homogeneous reaction, plasticizing in twin screw extruder barrel body are used for flexible electric heating through underwater pelletizer pelletizing
The thermoplastic polyurethane elastomer of film.
Embodiment 4
A kind of thermoplastic polyurethane elastomer for flexible electrothermal membrane, by the additional catalysis of the raw material of following weight percent
Agent is made:
The dosage of octoate catalyst stannous (T-9) is the 0.005% of total mass of raw material used above;
The polybutylene glyool adipate molecular weight is 1000.
Preparation method:
(1) by polybutylene glyool adipate, antioxidant 1010, antioxidant 626, Tinuvin770, E wax, OP wax,
Stabaxol P200 and T-9 are added in A reaction kettle and are uniformly mixed, and setting temperature is 115 DEG C;
(2) MDI-100 is added in B reaction kettle, setting temperature is 70 DEG C;1,4-butanediol is added in C reaction kettle,
It is 65 DEG C that temperature, which is arranged,;
(3) uniform to each reaction kettle material stirring, temperature is stablized, by having the perfusion system of accurate measurement, by A, B and
Raw material in C reaction kettle injects double screw extruder spout, and the EPFR-400A of accurate measurement injects double screw extruder feeding
Mouthful, mixture homogeneous reaction, plasticizing in twin screw extruder barrel body are used for flexible electric heating through underwater pelletizer pelletizing
The thermoplastic polyurethane elastomer of film.
Comparative example
A kind of thermoplastic polyurethane elastomer for flexible electrothermal membrane, by the additional catalysis of the raw material of following weight percent
Agent is made:
The dosage of octoate catalyst stannous (T-9) is the 0.005% of total mass of raw material used above;
The polybutylene glyool adipate molecular weight is 1000.
Preparation method:
(1) polybutylene glyool adipate, antioxidant 1010, Tinuvin770 and T-9 are added in A reaction kettle
It is uniformly mixed, setting temperature is 115 DEG C;
(2) MDI-100 is added in B reaction kettle, setting temperature is 70 DEG C;1,4-butanediol is added in C reaction kettle,
It is 65 DEG C that temperature, which is arranged,;
(3) uniform to each reaction kettle material stirring, temperature is stablized, by having the perfusion system of accurate measurement, by A, B and
Raw material in C reaction kettle injects double screw extruder spout, homogeneous reaction, plasticizing in twin screw extruder barrel body, through water
Lower pelletizing machine-cut grain is to get the thermoplastic polyurethane elastomer for flexible electrothermal membrane.
Thermoplastic polyurethane elastomer performance detection for flexible electrothermal membrane
To the thermoplastic polyurethane elastomer progressive for being used for flexible electrothermal membrane prepared by Examples 1 to 4 and comparison example
It can detect, testing result is shown in Table 1.
Remarks: hydrolysising condition is to be kept for 28 days at 85 DEG C, 85%RH.
Table 1
It can be seen from the data in Table 1 that the thermoplastic polyurethane elastomer prepared by the present invention for flexible electrothermal membrane has
There are higher mechanical strength, stable high-temperature behavior, excellent fire-retardant and anti-hydrolytic performance, and is surveyed by 3500V high-voltage breakdown
Examination has no breakage, can meet the requirement of flexible electrothermal membrane.
Claims (10)
1. a kind of thermoplastic polyurethane elastomer for flexible electrothermal membrane, it is characterised in that: by the original of following mass percent
Material extra catalyst is made:
The dosage of the catalyst is the 0.001~0.01% of above-mentioned raw materials used gross mass;
The polyester polyol is polyester-diol, and molecular weight is 1000~3000.
2. the thermoplastic polyurethane elastomer according to claim 1 for flexible electrothermal membrane, it is characterised in that: described
Polyester polyol is in polyethylene glycol adipate glycol, polybutylene glyool adipate or polyhexamethylene adipate glycol
One kind, two or more.
3. the thermoplastic polyurethane elastomer according to claim 1 for flexible electrothermal membrane, it is characterised in that: described
Diisocyanate be 4,4'- methyl diphenylene diisocyanate, phenylene -1,4- diisocyanate, toluene di-isocyanate(TDI), 1,
4- cyclohexyl-diisocyanate or decane -1,10- diisocyanate.
4. the thermoplastic polyurethane elastomer according to claim 1 for flexible electrothermal membrane, it is characterised in that: described
Chain extender is 1,4- butanediol, ethylene glycol, 1,2- propylene glycol, 1,3- propylene glycol, 2- methyl-1,3-propanediol or 1,6-HD
One of, two or more;The antioxidant is Hinered phenols antioxidant, phosphite ester antioxidant or sulfur-bearing antioxygen
One of agent, two or more.
5. the thermoplastic polyurethane elastomer according to claim 1 for flexible electrothermal membrane, it is characterised in that: described
Light stabilizer be one of Tinuvin770, Tinuvin234 or Tinuvin571, two or more.
6. the thermoplastic polyurethane elastomer according to claim 1 for flexible electrothermal membrane, it is characterised in that: described
Lubricant be one of oleamide, erucyl amide, glycerin monostearate, polyethylene wax or montanin wax, two or more.
7. the thermoplastic polyurethane elastomer according to claim 1 for flexible electrothermal membrane, it is characterised in that: described
Fire retardant is using phosphorus, nitrogen as the halogen-free environment-friendly fire retardant of ignition-proof element.
8. the thermoplastic polyurethane elastomer according to claim 1 for flexible electrothermal membrane, it is characterised in that: described
Anti-hydrolysis agent is one or both of single second carbide imine or polycarbodiimide.
9. the thermoplastic polyurethane elastomer according to claim 1 for flexible electrothermal membrane, it is characterised in that: described
Catalyst is organo-bismuth, organotin or titanate ester catalyst.
10. a kind of method for preparing thermoplastic polyurethane elastomer described in claim 1 for flexible electrothermal membrane, feature
It is: the following steps are included:
(1) polyester polyol, antioxidant, light stabilizer, lubricant, anti-hydrolysis agent and catalyst are added in A reaction kettle,
It is 100~115 DEG C that temperature, which is arranged,;
(2) diisocyanate is added in B reaction kettle, setting temperature is 65~75 DEG C;Chain extender is added in C reaction kettle,
It is 60~70 DEG C that temperature, which is arranged,;
(3) raw material in A, B and C reaction kettle is added to double screw extruder, while fire retardant is added to twin-screw extrusion
Machine is reacted, is plasticized, through underwater pelletizer pelletizing to get the thermoplastic polyurethane elastomer for flexible electrothermal membrane.
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Cited By (4)
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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 |
CN115141479A (en) * | 2022-09-01 | 2022-10-04 | 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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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 |
CN115141479A (en) * | 2022-09-01 | 2022-10-04 | 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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