CN111393609A - Pouring type polyurethane elastomer and preparation method thereof - Google Patents

Pouring type polyurethane elastomer and preparation method thereof Download PDF

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Publication number
CN111393609A
CN111393609A CN202010139811.5A CN202010139811A CN111393609A CN 111393609 A CN111393609 A CN 111393609A CN 202010139811 A CN202010139811 A CN 202010139811A CN 111393609 A CN111393609 A CN 111393609A
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component
molecular weight
polyurethane elastomer
temperature
polycaprolactone polyol
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王雨露
李留罐
刘勇
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Suzhou Cpugl Roller Co ltd
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Suzhou Cpugl Roller Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C08G18/7671Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08Processes
    • C08G18/10Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/38Low-molecular-weight compounds having heteroatoms other than oxygen
    • C08G18/3802Low-molecular-weight compounds having heteroatoms other than oxygen having halogens
    • C08G18/3814Polyamines
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/42Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4266Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
    • C08G18/4269Lactones
    • C08G18/4277Caprolactone and/or substituted caprolactone

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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)

Abstract

The invention discloses a pouring type polyurethane elastomer and a preparation method thereof, and belongs to the technical field of materials. According to the invention, the prepolymer with NCO% of about 8.0% is prepared, and the MOCA proportion is adjusted by using polyols with different molecular weights, so that the defects that the MOCA has an overhigh melting point (MOCA melting point is 98 ℃, MOCA and polyester polyol are fused to reduce the pouring temperature), and the MOCA is easy to crystallize in low-temperature pouring are overcome, and the production safety is facilitated; the invention increases the rigidity of the polyurethane elastomer and greatly improves the tensile strength of the polyurethane elastomer.

Description

Pouring type polyurethane elastomer and preparation method thereof
Technical Field
The invention relates to a pouring type polyurethane elastomer and a preparation method thereof, belonging to the technical field of materials.
Background
Polyurethane elastomer is a high molecular material based between plastic and rubber. The polyurethane elastomer has excellent performances of wear resistance, good elasticity, impact resistance, oil resistance, acid resistance, alkali resistance, ray radiation resistance and the like. Because of its outstanding performance, it is widely used in many fields of national economy: light industry, chemical industry, electronics, textile, medical treatment, building materials, automobiles, national defense, aerospace, aviation, machinery, traffic, oil field and mine, printing machine rollers, solid wheels, sports and other fields. The MDI100 molecular structure contains two benzene rings, has a symmetrical molecular structure, and the prepared polyurethane elastomer has good mechanical properties. The MDI100 is mainly applied to the manufacture of various polyurethane elastomers and is mainly used for producing thermoplastic polyurethane elastomers.
However, in the prior art, MDI100 prepolymers are all prepared into elastomers by using 1, 4-Butanediol (BDO) as a chain extender. Compared with MOCA chain extension, BDO has lower tensile strength and cannot meet the use field of high load, and the MOCA chain extension can improve the rigidity of the elastomer, increase the tensile strength of the elastomer and be used under some high load requirements.
Disclosure of Invention
In order to solve the problems, the invention provides a pouring type polyurethane elastomer and a preparation method thereof, wherein prepolymer with NCO% of about 8.0% is prepared, and polyol with different molecular weights is used for adjusting the MOCA ratio, so that the defects of overhigh melting point of MOCA and easy crystallization in low-temperature pouring are overcome. The method has the advantages of simple production process, time saving and easy operation.
The first purpose of the invention is to provide a preparation method of a pouring type polyurethane elastomer, which comprises the following steps:
s1, preparation of the component A: dehydrating and vacuumizing polycaprolactone polyol with the molecular weight of 800-1200 at the temperature of 100-105 ℃, cooling to 50-60 ℃, adding 1/3-2/3 polycaprolactone polyol with the molecular weight of 800-1200 into diphenylmethane diisocyanate (MDI100) at the temperature of 50-60 ℃, adjusting the temperature to 75-85 ℃, adding the remaining polycaprolactone polyol with the molecular weight of 800-1200, and reacting until the content of isocyanate groups is 7% -10% to obtain a component A;
s2, preparation of a component B: polycaprolactone polyol with the molecular weight of 1800-2200, 3-dichloro-4, 4Diaminodiphenylmethane (MOCA), color paste, defoaming agent and catalyst are dehydrated and vacuumized at the temperature of 110 ℃ and 105 ℃, and the temperature is reduced to 75-80 ℃ to obtain a component B;
s3, preparation of polyurethane elastomer: mixing the component A and the component B according to the proportion that the isocyanate index R is 0.95-1, stirring and mixing at 75-85 ℃ under a vacuum condition, injecting into a mold, demolding after molding, and curing to prepare a polyurethane elastomer;
the component A and the component B respectively comprise the following components in parts by weight:
the component A comprises:
diphenylmethane diisocyanate: 50 to 60 portions of
Polycaprolactone polyol with molecular weight of 800-1200: 90 to 110 portions of
And B component:
polycaprolactone polyol with molecular weight of 1800-2200: 50 to 60 portions of
3,3 '-dichloro-4, 4' -diaminodiphenylmethane: 40 to 50 portions of
And (3) defoaming agent: 0.2 to 0.5 portion
Color paste: 0.2 to 1 portion
Catalyst: 0.2 to 0.5 portion.
Further, the catalyst is an organic tin catalyst.
Further, the defoaming agent is an organosilicon surfactant.
Further, in the step of S1 or the step of S2, the dehydration vacuum pumping time is 30 to 40 minutes.
Further, in the step S3, the degree of vacuum under vacuum is 0.098MPa to 0.10 MPa.
Further, in the step of S1, the reaction time is 2 to 4 hours.
Further, in the steps of S1 and S2, the prepared a component and B component are sealed and preserved by filling nitrogen gas.
Further, in the step S3, the stirring and mixing time is 2-5 min.
Further, in the step S3, the temperature of the mold is 110-130 ℃, the mold is pre-vulcanized in the mold for 20-30 min and then is demoulded, and the demolding is carried out, and then the vulcanization is carried out for 10-15 hours at 85-95 ℃ to obtain the polyurethane elastomer.
The second purpose of the invention is to provide a casting polyurethane elastomer prepared by the method.
The invention has the beneficial effects that:
according to the invention, the prepolymer with NCO% of about 8.0% is prepared, and the MOCA proportion is adjusted by using polyols with different molecular weights, so that the defects that the MOCA has an overhigh melting point (MOCA melting point is 98 ℃, MOCA and polyester polyol are fused to reduce the pouring temperature), and the MOCA is easy to crystallize in low-temperature pouring are overcome, and the production safety is facilitated; the invention increases the rigidity of the polyurethane elastomer and greatly improves the tensile strength of the polyurethane elastomer.
Detailed Description
The present invention is further described below in conjunction with specific examples to enable those skilled in the art to better understand the present invention and to practice it, but the examples are not intended to limit the present invention.
Example 1:
weighing raw materials:
weighing the following components in parts by weight: weighing 95 parts of polycaprolactone polyol with the molecular weight of 1000; 55 parts of polycaprolactone polyol with the molecular weight of 2000; diphenylmethane diisocyanate (MID 100), 50 parts; 3,3, -dichloro-4, 4, -diaminodiphenylmethane (MOCA), 40 parts; silicone surfactant defoamer: 0.5 part; color paste: 1 part; organotin catalyst: 0.5 part.
The preparation method of the pouring type polyurethane elastomer comprises the following steps:
(1) adding weighed diphenylmethane diisocyanate (MDI100) into a three-neck flask, heating in a water bath at 50 ℃ to melt the weighed diphenylmethane diisocyanate, and filling nitrogen for storage after melting;
(2) putting 1000 molecular weight polycaprolactone polyol into a three-neck flask according to a certain weight, heating to 105 ℃, dehydrating, vacuumizing for 30min, cooling to 60 ℃ after vacuumizing, and filling nitrogen for storage.
(3) Adding dehydrated polycaprolactone polyol with the molecular weight of 1000 at 60 ℃ into MDI100 with the molecular weight of 50 ℃ in batches, stirring and reacting for 30min, cooling to 60 ℃ after stopping heating, continuously adding the rest polycaprolactone polyol with the molecular weight of 1000 for reacting, and keeping the temperature at 80 ℃.
(4) Fully stirring and mixing for reaction, reacting for 2.0-2.5 hours at the temperature of 80-85 ℃, then vacuumizing, and reacting for 1.0-1.5 hours in a vacuum state to obtain the prepolymer.
(5) And (3) determining the percentage content of the isocyanate group (NCO) in the prepolymer, stopping the reaction when the percentage content of the isocyanate group (NCO) is 7.8-8.0%, obtaining the prepolymer meeting the requirement, and filling nitrogen into the prepolymer for sealed storage for the next step.
(6) Weighing a certain part of polycaprolactone polyol with molecular weight of 2000 and 3,3, -dichloro-4, 4, -diaminodiphenylmethane (MOCA) according to a ratio of 15:13, fully stirring and mixing, heating to 105 ℃, dehydrating and vacuumizing for 60 min.
(7) After the vacuum pumping is finished, the temperature is reduced to 80 ℃.
(8) Adding an organic tin catalyst, color paste and a defoaming agent into a mixture of 2000 molecular weight polycaprolactone polyol and MOCA, fully stirring, heating to 105 ℃, dehydrating, vacuumizing for 30min, cooling to 75 ℃, filling nitrogen, and hermetically sealing for storage.
(9) And (3) fully stirring and mixing the prepolymer prepared in the step (5) and the mixture prepared in the step (8) at the isocyanate index R of 0.98 under vacuum at 80 ℃ for 2 mm, and then putting the mixture into a 120 ℃ mold.
(10) Then precuring for 20min at 120 ℃ and demoulding.
(11) After demoulding, the polyurethane elastomer of the MDI-MOCA system can be obtained after vulcanization for 12h at the temperature of 90 ℃.
The polyurethane elastomer prepared in this example had a hardness of 95A and a tensile strength of 51.9 MPa.
Example 2:
weighing raw materials:
weighing the following components in parts by weight: weighing 90 parts of polycaprolactone polyol with the molecular weight of 1000; 50 parts of polycaprolactone polyol with the molecular weight of 2000; diphenylmethane diisocyanate (MID 100), 50 parts; 3,3, -dichloro-4, 4, -diaminodiphenylmethane (MOCA), 40 parts; silicone surfactant defoamer: 0.2 part; color paste: 0.2 part; organotin catalyst: 0.2 part.
The preparation method of the pouring type polyurethane elastomer comprises the following steps:
(1) adding weighed diphenylmethane diisocyanate (MDI100) into a three-neck flask, heating in a water bath at 50 ℃ to melt the weighed diphenylmethane diisocyanate, and filling nitrogen for storage after melting;
(2) putting 1000 molecular weight polycaprolactone polyol into a three-neck flask according to a certain weight, heating to 105 ℃, dehydrating, vacuumizing for 30min, cooling to 60 ℃ after vacuumizing, and filling nitrogen for storage.
(3) Adding dehydrated polycaprolactone polyol with the molecular weight of 1000 at 60 ℃ into MDI100 with the molecular weight of 50 ℃ in batches, stirring and reacting for 30min, cooling to 60 ℃ after stopping heating, continuously adding the rest polycaprolactone polyol with the molecular weight of 1000 for reacting, and keeping the temperature at 80 ℃.
(4) Fully stirring and mixing for reaction, reacting for 2.0-2.5 hours at the temperature of 80-85 ℃, then vacuumizing, and reacting for 1.0-1.5 hours in a vacuum state to obtain the prepolymer.
(5) And (3) determining the percentage content of the isocyanate group (NCO) in the prepolymer, stopping the reaction when the percentage content of the isocyanate group (NCO) is 7.8-8.0%, obtaining the prepolymer meeting the requirement, and filling nitrogen into the prepolymer for sealed storage for the next step.
(6) Weighing a certain part of polycaprolactone polyol with molecular weight of 2000 and 3,3, -dichloro-4, 4, -diaminodiphenylmethane (MOCA) according to a ratio of 15:13, fully stirring and mixing, heating to 105 ℃, dehydrating and vacuumizing for 60 min.
(7) After the vacuum pumping is finished, the temperature is reduced to 80 ℃.
(8) Adding an organic tin catalyst, color paste and a defoaming agent into a mixture of 2000 molecular weight polycaprolactone polyol and MOCA, fully stirring, heating to 105 ℃, dehydrating, vacuumizing for 30min, cooling to 75 ℃, filling nitrogen, and hermetically sealing for storage.
(9) And (3) fully stirring and mixing the prepolymer prepared in the step (5) and the mixture prepared in the step (8) at the isocyanate index R of 0.98 under vacuum at 80 ℃ for 2 mm, and then putting the mixture into a 120 ℃ mold.
(10) Then precuring for 20min at 120 ℃ and demoulding.
(11) After demoulding, the polyurethane elastomer of the MDI-MOCA system can be obtained after vulcanization for 12h at the temperature of 90 ℃.
The hardness of the polyurethane elastomer prepared in this example was 95A, and the tensile strength was 48.9 MPa.
Example 3:
weighing raw materials:
weighing the following components in parts by weight: weighing 100 parts of polycaprolactone polyol with the molecular weight of 1000; 55 parts of polycaprolactone polyol with the molecular weight of 2000; diphenylmethane diisocyanate (MID 100), 55 parts; 3,3, -dichloro-4, 4, -diaminodiphenylmethane (MOCA), 45 parts; silicone surfactant defoamer: 0.3 part; color paste: 0.5 part; organotin catalyst: 0.3 part.
The preparation method of the pouring type polyurethane elastomer comprises the following steps:
(1) adding weighed diphenylmethane diisocyanate (MDI100) into a three-neck flask, heating in a water bath at 50 ℃ to melt the weighed diphenylmethane diisocyanate, and filling nitrogen for storage after melting;
(2) putting 1000 molecular weight polycaprolactone polyol into a three-neck flask according to a certain weight, heating to 105 ℃, dehydrating, vacuumizing for 30min, cooling to 60 ℃ after vacuumizing, and filling nitrogen for storage.
(3) Adding dehydrated polycaprolactone polyol with the molecular weight of 1000 at 60 ℃ into MDI100 with the molecular weight of 50 ℃ in batches, stirring and reacting for 30min, cooling to 60 ℃ after stopping heating, continuously adding the rest polycaprolactone polyol with the molecular weight of 1000 for reacting, and keeping the temperature at 80 ℃.
(4) Fully stirring and mixing for reaction, reacting for 2.0-2.5 hours at the temperature of 80-85 ℃, then vacuumizing, and reacting for 1.0-1.5 hours in a vacuum state to obtain the prepolymer.
(5) And (3) determining the percentage content of the isocyanate group (NCO) in the prepolymer, stopping the reaction when the percentage content of the isocyanate group (NCO) is 7.8-8.0%, obtaining the prepolymer meeting the requirement, and filling nitrogen into the prepolymer for sealed storage for the next step.
(6) Weighing a certain part of polycaprolactone polyol with molecular weight of 2000 and 3,3, -dichloro-4, 4, -diaminodiphenylmethane (MOCA) according to a ratio of 15:13, fully stirring and mixing, heating to 105 ℃, dehydrating and vacuumizing for 60 min.
(7) After the vacuum pumping is finished, the temperature is reduced to 80 ℃.
(8) Adding an organic tin catalyst, color paste and a defoaming agent into a mixture of 2000 molecular weight polycaprolactone polyol and MOCA, fully stirring, heating to 105 ℃, dehydrating, vacuumizing for 30min, cooling to 75 ℃, filling nitrogen, and hermetically sealing for storage.
(9) And (3) fully stirring and mixing the prepolymer prepared in the step (5) and the mixture prepared in the step (8) at the isocyanate index R of 0.98 under vacuum at 80 ℃ for 2 mm, and then putting the mixture into a 120 ℃ mold.
(10) Then precuring for 20min at 120 ℃ and demoulding.
(11) After demoulding, the polyurethane elastomer of the MDI-MOCA system can be obtained after vulcanization for 12h at the temperature of 90 ℃.
The hardness of the polyurethane elastomer prepared in this example was 95A, and the tensile strength was 54.4 MPa.
Example 4:
weighing raw materials:
weighing the following components in parts by weight: weighing 110 parts of polycaprolactone polyol with the molecular weight of 1000; 60 parts of polycaprolactone polyol with the molecular weight of 2000; diphenylmethane diisocyanate (MID 100), 60 parts; 3,3, -dichloro-4, 4, -diaminodiphenylmethane (MOCA), 50 parts; silicone surfactant defoamer: 0.5 part; color paste: 1 part; organotin catalyst: 0.5 part.
The preparation method of the pouring type polyurethane elastomer comprises the following steps:
(1) adding weighed diphenylmethane diisocyanate (MDI100) into a three-neck flask, heating in a water bath at 50 ℃ to melt the weighed diphenylmethane diisocyanate, and filling nitrogen for storage after melting;
(2) putting 1000 molecular weight polycaprolactone polyol into a three-neck flask according to a certain weight, heating to 105 ℃, dehydrating, vacuumizing for 30min, cooling to 60 ℃ after vacuumizing, and filling nitrogen for storage.
(3) Adding dehydrated polycaprolactone polyol with the molecular weight of 1000 at 60 ℃ into MDI100 with the molecular weight of 50 ℃ in batches, stirring and reacting for 30min, cooling to 60 ℃ after stopping heating, continuously adding the rest polycaprolactone polyol with the molecular weight of 1000 for reacting, and keeping the temperature at 80 ℃.
(4) Fully stirring and mixing for reaction, reacting for 2.0-2.5 hours at the temperature of 80-85 ℃, then vacuumizing, and reacting for 1.0-1.5 hours in a vacuum state to obtain the prepolymer.
(5) And (3) determining the percentage content of the isocyanate group (NCO) in the prepolymer, stopping the reaction when the percentage content of the isocyanate group (NCO) is 7.8-8.0%, obtaining the prepolymer meeting the requirement, and filling nitrogen into the prepolymer for sealed storage for the next step.
(6) Weighing a certain part of polycaprolactone polyol with molecular weight of 2000 and 3,3, -dichloro-4, 4, -diaminodiphenylmethane (MOCA) according to a ratio of 15:13, fully stirring and mixing, heating to 105 ℃, dehydrating and vacuumizing for 60 min.
(7) After the vacuum pumping is finished, the temperature is reduced to 80 ℃.
(8) Adding an organic tin catalyst, color paste and a defoaming agent into a mixture of 2000 molecular weight polycaprolactone polyol and MOCA, fully stirring, heating to 105 ℃, dehydrating, vacuumizing for 30min, cooling to 75 ℃, filling nitrogen, and hermetically sealing for storage.
(9) Mixing the prepolymer prepared in the step (5) and the mixture prepared in the step (8) according to a ratio of 50: 22.5 in a proportion of 80 ℃ under vacuum, fully stirring and mixing for 2mim, and then placing into a 120 ℃ mold.
(10) Then precuring for 20min at 120 ℃ and demoulding.
(11) After demoulding, the polyurethane elastomer of the MDI-MOCA system can be obtained after vulcanization for 12h at the temperature of 90 ℃.
The polyurethane elastomer prepared in this example had a hardness of 95A and a tensile strength of 53.7 MPa.
Comparative example 1:
polyurethane elastomers were prepared according to conventional methods using 1, 4-Butanediol (BDO) as the chain extender. The tensile strength of the polyurethane elastomer with the hardness of 95A is 38-45 MPa, and the tensile strength can be different but not more than 45MPa by adopting different raw material dosages.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.

Claims (10)

1. The preparation method of the pouring type polyurethane elastomer is characterized by comprising the following steps:
s1, preparation of the component A: dehydrating and vacuumizing polycaprolactone polyol with the molecular weight of 800-1200 at the temperature of 100-105 ℃, cooling to 50-60 ℃, adding 1/3-2/3 polycaprolactone polyol with the molecular weight of 800-1200 into diphenylmethane diisocyanate (MDI100) at the temperature of 50-60 ℃, adjusting the temperature to 75-85 ℃, adding the remaining polycaprolactone polyol with the molecular weight of 800-1200, and reacting until the content of isocyanate groups is 7% -10% to obtain a component A;
s2, preparation of a component B: polycaprolactone polyol with the molecular weight of 1800-2200, 3-dichloro-4, 4Diaminodiphenylmethane (MOCA), color paste, defoaming agent and catalyst are dehydrated and vacuumized at the temperature of 110 ℃ and 105 ℃, and the temperature is reduced to 75-80 ℃ to obtain a component B;
s3, preparation of polyurethane elastomer: mixing the component A and the component B according to the proportion that the isocyanate index R is 0.95-1, stirring and mixing at 75-85 ℃ under a vacuum condition, injecting into a mold, demolding after molding, and curing to prepare a polyurethane elastomer;
the component A and the component B respectively comprise the following components in parts by weight:
the component A comprises:
diphenylmethane diisocyanate: 50 to 60 portions of
Polycaprolactone polyol with molecular weight of 800-1200: 90 to 110 portions of
And B component:
polycaprolactone polyol with molecular weight of 1800-2200: 50 to 60 portions of
3,3-dichloro-4, 4Diaminodiphenylmethane: 40 to 50 portions of
And (3) defoaming agent: 0.2 to 0.5 portion
Color paste: 0.2 to 1 portion
Catalyst: 0.2 to 0.5 portion.
2. The method of claim 1, wherein the catalyst is an organotin catalyst.
3. The method of claim 1 wherein said defoamer is a silicone surfactant.
4. The method as claimed in claim 1, wherein the dehydrating evacuation time is 30 to 40 minutes at the step of S1 or the step of S2.
5. The method as claimed in claim 1, wherein the degree of vacuum of the vacuum condition is 0.098MPa to 0.10MPa in the S3 step.
6. The method according to claim 1, wherein the reaction time in the step of S1 is 2 to 4 hours.
7. The method of claim 1, wherein the prepared A-component and B-component are sealed and preserved by filling nitrogen gas in the steps of S1 and S2.
8. The method according to claim 1, wherein the stirring and mixing time in the step of S3 is 2-5 min.
9. The method according to claim 1, wherein in the step S3, the temperature of the mold is 110-130 ℃, the mold is pre-vulcanized in the mold for 20-30 min and then is demolded, and the demolding is followed by post-vulcanization at 85-95 ℃ for 10-15 hours to obtain the polyurethane elastomer.
10. A cast polyurethane elastomer prepared by the method of any one of claims 1 to 9.
CN202010139811.5A 2020-03-03 2020-03-03 Pouring type polyurethane elastomer and preparation method thereof Pending CN111393609A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114560991A (en) * 2022-03-25 2022-05-31 华南理工大学 Polyurethane material with dynamic performance and damping performance and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504182A (en) * 2011-10-27 2012-06-20 山东东大一诺威聚氨酯有限公司 Preparation method of rigid polyurethane

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504182A (en) * 2011-10-27 2012-06-20 山东东大一诺威聚氨酯有限公司 Preparation method of rigid polyurethane

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114560991A (en) * 2022-03-25 2022-05-31 华南理工大学 Polyurethane material with dynamic performance and damping performance and preparation method thereof
CN114560991B (en) * 2022-03-25 2023-10-20 华南理工大学 Polyurethane material with dynamic performance and damping performance and preparation method thereof

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Application publication date: 20200710