CN107722234A - A kind of isocyanate-terminated polyethers modified epoxy and preparation method thereof - Google Patents

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

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Publication number
CN107722234A
CN107722234A CN201711124494.4A CN201711124494A CN107722234A CN 107722234 A CN107722234 A CN 107722234A CN 201711124494 A CN201711124494 A CN 201711124494A CN 107722234 A CN107722234 A CN 107722234A
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CN
China
Prior art keywords
isocyanate
parts
epoxy resin
terminated polyethers
reaction
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201711124494.4A
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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 CN201711124494.4A priority Critical patent/CN107722234A/en
Publication of CN107722234A publication Critical patent/CN107722234A/en
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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
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • 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
    • C08G18/58—Epoxy resins
    • 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
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7614—Polyisocyanates 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 modified epoxy and preparation method thereof, belong to epoxy resin modification technical field.The modified epoxy includes 20 30 parts of isocyanate-terminated polyethers, 51 30 40 parts of epoxy resin E, 50 80 parts of dimethylbenzene, 20 30 parts of MEK；The present invention is from epoxy resin structural feature, prepare the polyethers for only having one end to be isocyanate groups on main chain, hydroxyl reaction in isocyano and epoxy resin in the polyethers, 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 modified epoxy and preparation method thereof
Technical field
The present invention relates to a kind of modified epoxy and preparation method thereof, it is more particularly related to which a kind of end is different Cyanic acid ester group polyether modified epoxy resin and preparation method thereof, belongs 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
Present invention seek to address that the problems of the prior art, there is provided a kind of isocyanate-terminated polyethers modified epoxy, Pliability of the epoxy resin itself is preferable, simultaneously because the change of epoxy resin structural, the curing process of modified resin obtains Improve, widened the application field of epoxy resin.
In order to realize foregoing invention purpose, its specific technical scheme is as follows：
A kind of isocyanate-terminated polyethers modified epoxy, it is characterised in that：Including following raw materials by weight：
Isocyanate-terminated polyethers 20-30 parts
Epoxy resin E-51 30-40 parts
Dimethylbenzene 50-80 parts
MEK 20-30 parts；
Wherein isocyanate-terminated polyethers include following raw materials by weight：
Diethylene glycol monobutyl ether 20-30 parts
Toluene-2,4-diisocyanate, 4- diisocyanate 40-50 parts
Hexamethylene 50-100 parts.
A kind of preparation method of isocyanate-terminated polyethers modified epoxy, it is characterised in that：Walked including following technique Suddenly：
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；
D, in another four round flask with electric stirring, condenser pipe, charge door and nitrogen mouth, recipe requirements amount is added Epoxy resin E-51, while add reaction dissolvent dimethylbenzene and MEK；
E, stirring is started to be sufficiently mixed the epoxy resin E-51 and solvent of above-mentioned addition uniformly；Terminal isocyanate group is added to gather Ether, reaction temperature is risen to 70-80 DEG C under nitrogen protection, react 2-3h, obtain isocyanate-terminated polyethers modified epoxy.
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 Hydroxyl reaction in isocyano and epoxy resin in polyethers, on polyether grafting to epoxy resin side chain, improve asphalt mixtures modified by epoxy resin The pliability of fat 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 modified epoxy, including following raw materials by weight：
20 parts of isocyanate-terminated polyethers
30 parts of epoxy resin E-51
50 parts of dimethylbenzene
20 parts of MEK；
Wherein isocyanate-terminated polyethers include 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 modified epoxy, including following raw materials by weight：
30 parts of isocyanate-terminated polyethers
40 parts of epoxy resin E-51
80 parts of dimethylbenzene
30 parts of MEK；
Wherein isocyanate-terminated polyethers include 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 modified epoxy, including following raw materials by weight：
25 parts of isocyanate-terminated polyethers
35 parts of epoxy resin E-51
65 parts of dimethylbenzene
25 parts of MEK；
Wherein isocyanate-terminated polyethers include 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 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；
D, in another four round flask with electric stirring, condenser pipe, charge door and nitrogen mouth, recipe requirements amount is added Epoxy resin E-51, while add reaction dissolvent dimethylbenzene and MEK；
E, stirring is started to be sufficiently mixed the epoxy resin E-51 and solvent of above-mentioned addition uniformly；Terminal isocyanate group is added to gather Ether, reaction temperature is risen to 70 DEG C under nitrogen protection, react 2h, obtain isocyanate-terminated polyethers modified epoxy.
Embodiment 5
A kind of preparation method of isocyanate-terminated polyethers 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；
D, in another four round flask with electric stirring, condenser pipe, charge door and nitrogen mouth, recipe requirements amount is added Epoxy resin E-51, while add reaction dissolvent dimethylbenzene and MEK；
E, stirring is started to be sufficiently mixed the epoxy resin E-51 and solvent of above-mentioned addition uniformly；Terminal isocyanate group is added to gather Ether, reaction temperature is risen to 80 DEG C under nitrogen protection, react 3h, obtain isocyanate-terminated polyethers modified epoxy.
Embodiment 6
A kind of preparation method of isocyanate-terminated polyethers 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；
D, in another four round flask with electric stirring, condenser pipe, charge door and nitrogen mouth, recipe requirements amount is added Epoxy resin E-51, while add reaction dissolvent dimethylbenzene and MEK；
E, stirring is started to be sufficiently mixed the epoxy resin E-51 and solvent of above-mentioned addition uniformly；Terminal isocyanate group is added to gather Ether, reaction temperature is risen to 75 DEG C under nitrogen protection, react 2.5h, obtain isocyanate-terminated polyethers modified epoxy.

Claims (2)

  1. A kind of 1. isocyanate-terminated polyethers modified epoxy, it is characterised in that：Including following original in parts by weight Material：
    Isocyanate-terminated polyethers 20-30 parts
    Epoxy resin E-51 30-40 parts
    Dimethylbenzene 50-80 parts
    MEK 20-30 parts；
    Wherein isocyanate-terminated polyethers include following raw materials by weight：
    Diethylene glycol monobutyl ether 20-30 parts
    Toluene-2,4-diisocyanate, 4- diisocyanate 40-50 parts
    Hexamethylene 50-100 parts.
  2. 2. a kind of preparation method of isocyanate-terminated polyethers modified epoxy according to claim 1, its feature exist In：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；
    D, in another four round flask with electric stirring, condenser pipe, charge door and nitrogen mouth, recipe requirements amount is added Epoxy resin E-51, while add reaction dissolvent dimethylbenzene and MEK；
    E, stirring is started to be sufficiently mixed the epoxy resin E-51 and solvent of above-mentioned addition uniformly；Terminal isocyanate group is added to gather Ether, reaction temperature is risen to 70-80 DEG C under nitrogen protection, react 2-3h, obtain isocyanate-terminated polyethers modified epoxy.
CN201711124494.4A 2017-11-14 2017-11-14 A kind of isocyanate-terminated polyethers modified epoxy and preparation method thereof Pending CN107722234A (en)

Priority Applications (1)

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CN201711124494.4A CN107722234A (en) 2017-11-14 2017-11-14 A kind of isocyanate-terminated polyethers modified epoxy and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711124494.4A CN107722234A (en) 2017-11-14 2017-11-14 A kind of isocyanate-terminated polyethers modified epoxy and preparation method thereof

Publications (1)

Publication Number Publication Date
CN107722234A true CN107722234A (en) 2018-02-23

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109293880A (en) * 2018-09-06 2019-02-01 苏州兴业材料科技股份有限公司 A kind of preparation method of modified o-cresol formaldehyde epoxy resin

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109293880A (en) * 2018-09-06 2019-02-01 苏州兴业材料科技股份有限公司 A kind of preparation method of modified o-cresol formaldehyde epoxy resin

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Application publication date: 20180223