CN107805297A - A kind of isocyanate-terminated polyethers for modified epoxy and preparation method thereof - Google Patents

A kind of isocyanate-terminated polyethers for modified epoxy and preparation method thereof Download PDF

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Publication number
CN107805297A
CN107805297A CN201711125537.0A CN201711125537A CN107805297A CN 107805297 A CN107805297 A CN 107805297A CN 201711125537 A CN201711125537 A CN 201711125537A CN 107805297 A CN107805297 A CN 107805297A
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CN
China
Prior art keywords
parts
isocyanate
diisocyanate
epoxy resin
terminated polyethers
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Pending
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CN201711125537.0A
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Chinese (zh)
Inventor
邓瑞
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Individual
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Individual
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Priority to CN201711125537.0A priority Critical patent/CN107805297A/en
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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
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/2805Compounds having only one group containing active hydrogen
    • C08G18/2815Monohydroxy compounds
    • C08G18/283Compounds containing ether groups, e.g. oxyalkylated monohydroxy compounds
    • C08G18/2835Compounds containing ether groups, e.g. oxyalkylated monohydroxy compounds having less than 5 ether groups
    • 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
    • C08G18/58Epoxy resins
    • 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
    • C08G18/7614Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring

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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)
  • Epoxy Resins (AREA)

Abstract

The present invention relates to a kind of isocyanate-terminated polyethers for modified epoxy and preparation method thereof, belong to epoxy resin modification technical field.The polyethers includes 20 30 parts of diethylene glycol monobutyl ether, toluene 2,40 50 parts of 4 diisocyanate, 50 100 parts of hexamethylene.The present invention is from epoxy resin structural feature, prepare the polyethers for only having one end to be isocyanate groups on main chain, isocyano in the polyethers can be with hydroxyl reaction in epoxy resin, on polyether grafting to epoxy resin side chain, improve the pliability of epoxy resin in itself, simultaneously because the change of epoxy resin structural, can improve the curing process of modified resin, widen the application field of epoxy resin.

Description

A kind of isocyanate-terminated polyethers for modified epoxy and preparation method thereof
Technical field
The present invention relates to a kind of polyethers and preparation method thereof, it is more particularly related to which a kind of be used for modified epoxy Isocyanate-terminated polyethers of resin and preparation method thereof, belong to epoxy resin modification technical field.
Background technology
Epoxy resin is to prepare one of important matrix material of high-performance composite materials, assigns composite good mechanics Performance and physical property, it is a kind of advanced composite material for being widely used in the fields such as space flight and aviation, automobile, machinery, electronics and building Material.But epoxy resin cured product resinousness is crisp, poor toughness, it is difficult to obtains higher mechanical property and physical property.For current This disadvantage of the epoxy resin used, is conducted extensive research to its curing system both at home and abroad.But these researchs often limit In the modification to epoxy curing agent, the research being directly modified to epoxy resin is less, greatly limit Its application field.
The content of the invention
A kind of present invention seek to address that the problems of the prior art, there is provided terminal isocyanate group for modified epoxy Polyethers, the polyethers improves the pliability of epoxy resin in itself, simultaneously because the change of epoxy resin structural, can improve modification The curing process of resin, the application field of epoxy resin is widened.
In order to realize foregoing invention purpose, its specific technical scheme is as follows:
A kind of isocyanate-terminated polyethers for modified epoxy, it is characterised in that:Including it is following in parts by weight Raw material:
Diethylene glycol monobutyl ether 20-30 parts
Toluene-2,4-diisocyanate, 4- diisocyanate 40-50 parts
Hexamethylene 50-100 parts.
Preferably, a kind of isocyanate-terminated polyethers for modified epoxy, it is characterised in that:Including below according to The raw material of parts by weight meter:
21 parts of diethylene glycol monobutyl ether
43 parts of Toluene-2,4-diisocyanate, 4- diisocyanate
80 parts of hexamethylene.
A kind of preparation method of isocyanate-terminated polyethers for modified epoxy, it is characterised in that:Including following Processing step:
A, diethylene glycol monobutyl ether, Toluene-2,4-diisocyanate, 4- diisocyanate and hexamethylene are weighed by recipe requirements, and add one there is electricity In the four round flask for moving stirring, condenser pipe, charge door and nitrogen mouth, it is uniformly mixed;
B, temperature of reaction system is risen to 65-70 DEG C, reacts 3-4h;Temperature of reaction system will be risen to 70-75 DEG C again, react 3- 4h;
C, the isocyanate content of reaction product is measured by sampling, reaches and stops reaction after reaction requires, quick cooling reaction System is to room temperature;Pour out reaction product and solvent hexamethylene is removed under vacuum condition, obtain isocyanate-terminated polyethers.
The advantageous effects that the present invention is brought:
The present invention prepares the polyethers for only having one end to be isocyanate groups on main chain, is somebody's turn to do from epoxy resin structural feature Isocyano in polyethers, on polyether grafting to epoxy resin side chain, can improve epoxy with hydroxyl reaction in epoxy resin The pliability of resin in itself, simultaneously because the change of epoxy resin structural, can improve the curing process of modified resin, widen The application field of epoxy resin.
Embodiment
Embodiment 1
A kind of isocyanate-terminated polyethers for modified epoxy, including following raw materials by weight:
20 parts of diethylene glycol monobutyl ether
40 parts of Toluene-2,4-diisocyanate, 4- diisocyanate
50 parts of hexamethylene.
Embodiment 2
A kind of isocyanate-terminated polyethers for modified epoxy, including following raw materials by weight:
30 parts of diethylene glycol monobutyl ether
50 parts of Toluene-2,4-diisocyanate, 4- diisocyanate
100 parts of hexamethylene.
Embodiment 3
A kind of isocyanate-terminated polyethers for modified epoxy, including following raw materials by weight:
25 parts of diethylene glycol monobutyl ether
45 parts of Toluene-2,4-diisocyanate, 4- diisocyanate
75 parts of hexamethylene.
Embodiment 4
A kind of preparation method of isocyanate-terminated polyethers for modified epoxy, is comprised the following steps that:
A, diethylene glycol monobutyl ether, Toluene-2,4-diisocyanate, 4- diisocyanate and hexamethylene are weighed by recipe requirements, and add one there is electricity In the four round flask for moving stirring, condenser pipe, charge door and nitrogen mouth, it is uniformly mixed;
B, temperature of reaction system is risen to 65 DEG C, reacts 3h;Temperature of reaction system will be risen to 70 DEG C again, react 3h;
C, the isocyanate content of reaction product is measured by sampling, reaches and stops reaction after reaction requires, quick cooling reaction System is to room temperature;Pour out reaction product and solvent hexamethylene is removed under vacuum condition, obtain isocyanate-terminated polyethers.
Embodiment 5
A kind of preparation method of isocyanate-terminated polyethers for modified epoxy, is comprised the following steps that:
A, diethylene glycol monobutyl ether, Toluene-2,4-diisocyanate, 4- diisocyanate and hexamethylene are weighed by recipe requirements, and add one there is electricity In the four round flask for moving stirring, condenser pipe, charge door and nitrogen mouth, it is uniformly mixed;
B, temperature of reaction system is risen to 70 DEG C, reacts 4h;Temperature of reaction system will be risen to 75 DEG C again, react 4h;
C, the isocyanate content of reaction product is measured by sampling, reaches and stops reaction after reaction requires, quick cooling reaction System is to room temperature;Pour out reaction product and solvent hexamethylene is removed under vacuum condition, obtain isocyanate-terminated polyethers.
Embodiment 6
A kind of preparation method of isocyanate-terminated polyethers for modified epoxy, is comprised the following steps that:
A, diethylene glycol monobutyl ether, Toluene-2,4-diisocyanate, 4- diisocyanate and hexamethylene are weighed by recipe requirements, and add one there is electricity In the four round flask for moving stirring, condenser pipe, charge door and nitrogen mouth, it is uniformly mixed;
B, temperature of reaction system is risen to 67.5 DEG C, reacts 3.5h;Temperature of reaction system will be risen to 72.5 DEG C again, reaction 3.5h;
C, the isocyanate content of reaction product is measured by sampling, reaches and stops reaction after reaction requires, quick cooling reaction System is to room temperature;Pour out reaction product and solvent hexamethylene is removed under vacuum condition, obtain isocyanate-terminated polyethers.

Claims (3)

  1. A kind of 1. isocyanate-terminated polyethers for modified epoxy, it is characterised in that:Including below according to parts by weight The raw material of meter:
    Diethylene glycol monobutyl ether 20-30 parts
    Toluene-2,4-diisocyanate, 4- diisocyanate 40-50 parts
    Hexamethylene 50-100 parts.
  2. A kind of 2. isocyanate-terminated polyethers for modified epoxy according to claim 1, it is characterised in that:Bag Include following raw materials by weight:
    21 parts of diethylene glycol monobutyl ether
    43 parts of Toluene-2,4-diisocyanate, 4- diisocyanate
    80 parts of hexamethylene.
  3. 3. a kind of preparation method of isocyanate-terminated polyethers for modified epoxy according to claim 1, its It is characterised by:Comprise the following steps that:
    A, diethylene glycol monobutyl ether, Toluene-2,4-diisocyanate, 4- diisocyanate and hexamethylene are weighed by recipe requirements, and add one there is electricity In the four round flask for moving stirring, condenser pipe, charge door and nitrogen mouth, it is uniformly mixed;
    B, temperature of reaction system is risen to 65-70 DEG C, reacts 3-4h;Temperature of reaction system will be risen to 70-75 DEG C again, react 3- 4h;
    C, the isocyanate content of reaction product is measured by sampling, reaches and stops reaction after reaction requires, quick cooling reaction System is to room temperature;Pour out reaction product and solvent hexamethylene is removed under vacuum condition, obtain isocyanate-terminated polyethers.
CN201711125537.0A 2017-11-14 2017-11-14 A kind of isocyanate-terminated polyethers for modified epoxy and preparation method thereof Pending CN107805297A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711125537.0A CN107805297A (en) 2017-11-14 2017-11-14 A kind of isocyanate-terminated polyethers for modified epoxy and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711125537.0A CN107805297A (en) 2017-11-14 2017-11-14 A kind of isocyanate-terminated polyethers for modified epoxy and preparation method thereof

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Publication Number Publication Date
CN107805297A true CN107805297A (en) 2018-03-16

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116426123A (en) * 2023-06-14 2023-07-14 北京爱思达航天科技有限公司 Bismaleimide resin composition, composite material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116426123A (en) * 2023-06-14 2023-07-14 北京爱思达航天科技有限公司 Bismaleimide resin composition, composite material and preparation method thereof
CN116426123B (en) * 2023-06-14 2023-09-12 北京爱思达航天科技有限公司 Bismaleimide resin composition, composite material and preparation method thereof

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Application publication date: 20180316