CN106543414A - A kind of preparation method of novel flexible epoxy resin - Google Patents
A kind of preparation method of novel flexible epoxy resin Download PDFInfo
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- CN106543414A CN106543414A CN201610887994.2A CN201610887994A CN106543414A CN 106543414 A CN106543414 A CN 106543414A CN 201610887994 A CN201610887994 A CN 201610887994A CN 106543414 A CN106543414 A CN 106543414A
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- epoxy resin
- preparation
- polymerization reaction
- reaction kettle
- amino
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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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
-
- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
- C08G65/2621—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
- C08G65/2624—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing aliphatic amine groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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 invention discloses a kind of preparation method of novel flexible epoxy resin, including the preparation and the preparation of flexible-epoxy of amino-polyether, the preparation of amino-polyether comprises the steps：Polymerization reaction kettle is vacuumized, and it is secondary to be filled with nitrogen displacement；Amino initiator is added in polymerization reaction kettle, agitating device is opened, the reaction temperature and reaction pressure condition of polymerization reaction kettle is controlled；Raw material monomer is uniformly added into into polymerization reaction kettle slowly.The present invention is by the raw material of different molecular weight, water white transparency, the different flexible epoxy resin of different viscosities (25 DEG C of viscosity, 350CPS 50000CPS) are prepared using different preparation conditions and method, with suitable for epoxy coating, the requirement of the different industries to flexible-epoxy such as epoxy adhesive, electronics adhesive, epoxy composite material, the weatherability of reinforced epoxy solidification, it is low temperature resistant, impact strength, the performance such as fatigue resistance.
Description
Technical field
The present invention relates to Epoxy Resin Technology field, more particularly to a kind of preparation method of novel flexible epoxy resin.
Background technology
In all molecular structures, the macromolecular compound containing epoxide group is referred to as epoxy resin at present.Epoxy resin conduct
One of five big base resins, due to having good physics, chemical property after epoxy resin cure, it is to metal and non-metallic material
The surface of material has an excellent adhesive strength, and dielectric properties are good, and hardness is high, the features such as to alkali and most of solvent-stable, because
And it is widely used in national defence, each department of national economy, make the purposes such as insulating materials, adhesive, coating, composite.
But have that solidfied material embrittlement, shrinkage factor are bigger than normal, elongation is low not, resistance to low after the solidification of ordinary epoxy resin product
The shortcomings of temperature, weatherability difference, limit application of the epoxy resin in many industries.
The content of the invention
Based on the technical problem that background technology is present, the present invention proposes a kind of preparation side of novel flexible epoxy resin
Method, enhances the performances such as the weatherability of epoxy resin cure, low temperature resistant, impact strength, fatigue resistance, widens epoxy resin
The application of material, is adapted to requirement of the current all trades and professions to epoxide resin material.
A kind of preparation method of novel flexible epoxy resin proposed by the present invention, including preparation and and the flexibility of amino-polyether
The preparation of epoxy resin, the preparation of amino-polyether comprise the steps：
S1, polymerization reaction kettle is vacuumized, and it is secondary to be filled with nitrogen displacement；
S2, agitating device will be opened during amino initiator adds polymerization reaction kettle, control the reaction temperature of polymerization reaction kettle and anti-
Answer pressure condition；
S3, slowly it is uniformly added into raw material monomer into polymerization reaction kettle, treats that raw material monomer is made in polymerization reaction kettle after the completion of adding
Temperature keeps constant, reaches design time and starts sampling, surveys the index such as mean molecule quantity and viscosity, after reaching prescribed limit, take out
Vacuum refining 30-60 minutes；
S4, unreacted complete monomer is carried out negative pressure rectifying, cooling down is filtered, obtains amino-polyether to 25 DEG C；
The preparation of flexible-epoxy comprises the steps：
S5, the amine terminated polyether of amino-polyether or mean molecule quantity 500-100000 is added into polymerization reaction kettle, vacuumize, open
Agitating device, is slowly added into epoxy resin, is filled with nitrogen pressure（0.01MPa.s-0.2MPa.s）, controlling reaction temperature is m, instead
It is n between seasonable；
S6, sampling viscosimetric and epoxide number, after reaching product requirement, vacuumize 15-30 minutes, after cooling is filtered, obtain flexible ring
Oxygen tree fat finished product.
Preferably, in S2, amino initiator is propane diamine, ethylenediamine, butanediamine, one or two or more kinds in pentanediamine
Mixture.
Preferably, in S2, reaction temperature is 50 DEG C -130 DEG C, and reaction pressure condition is 0.1MPa.s-1MPa.s.
Preferably, in S3, raw material monomer be oxirane, expoxy propane, epoxy butane and tetrahydrofuran in one kind or
More than two kinds of mixture.
Preferably, the amino-polyether molecular structure in S4 is NH2- (R-O-R) n-NH2 or NH2- [R-OCO-R] n-NH2.
Preferably, the epoxy resin in S5 is bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol S type epoxy tree
In fat, cycloaliphatic epoxy resin, glycolylurea epoxide resin, low molecule tetraglycidel ether epoxy resin and ethylene oxidic ester epoxy resin
One of which.
The present invention prepares water white transparency using different preparation conditions and method, no by the raw material of different molecular weight
The different flexible epoxy resin of same viscosity (25 DEG C of viscosity, 350CPS-50000CPS), with suitable for epoxy coating, Wear Characteristics of Epoxy Adhesive
The requirement of the different industries to flexible-epoxy such as agent, electronics adhesive, epoxy composite material, it is resistance to that reinforced epoxy solidifies
The performances such as Hou Xing, low temperature resistant, impact strength, fatigue resistance.
Specific embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
The preparation method of novel flexible epoxy resin proposed by the present invention, including preparation and the flexible-epoxy of amino-polyether
Prepare, the preparation of amino-polyether comprises the steps：
S1, polymerization reaction kettle is vacuumized, and it is secondary to be filled with nitrogen displacement；
S2, by propane diamine add polymerization reaction kettle in, open agitating device, control polymerization reaction kettle reaction temperature maintain 50
DEG C -75 DEG C and reaction pressure condition maintain 0.1MPa.s-1MPa.s；
S3, slowly it is uniformly added into expoxy propane into polymerization reaction kettle, treats that expoxy propane is made in polymerization reaction kettle after the completion of adding
Temperature keeps constant, reaches design time and starts sampling, surveys the index such as mean molecule quantity and viscosity, after reaching prescribed limit, take out
Vacuum refining 30-60 minutes；
S4, unreacted complete monomer is carried out negative pressure rectifying, cooling down is filtered, obtains amino-polyether to 25 DEG C；
The preparation of flexible-epoxy comprises the steps：
S5, amino-polyether is added into polymerization reaction kettle, vacuumized, opened agitating device, be slowly added into bisphenol A-type glycidol ring
Oxygen tree fat, is filled with nitrogen pressure（0.01MPa.s-0.2MPa.s）, controlling reaction temperature is 130 DEG C -150 DEG C, is reacted 8 hours；
S6, sampling viscosimetric and epoxide number, after reaching product requirement, vacuumize 15-30 minutes, after cooling is filtered, obtain colourless
Bright flexible-epoxy finished product.
The novel flexible epoxy resin that embodiment 1 is obtained carries out contrast with prior art products effect and shows：This enforcement
Example performance is better than comparative example really.Its correction data is as follows：
Embodiment 2
The preparation method of novel flexible epoxy resin proposed by the present invention, including preparation and the flexible-epoxy of amino-polyether
Prepare, the preparation of amino-polyether comprises the steps：
S1, polymerization reaction kettle is vacuumized, and it is secondary to be filled with nitrogen displacement；
S2, by ethylenediamine add polymerization reaction kettle in, open agitating device, control polymerization reaction kettle reaction temperature maintain 50
DEG C -65 DEG C and reaction pressure condition maintain 0.1MPa.s-0.6MPa.s；
S3, slowly it is uniformly added into expoxy propane into polymerization reaction kettle, treats that expoxy propane is made in polymerization reaction kettle after the completion of adding
Temperature keeps constant, reaches design time and starts sampling, surveys the index such as mean molecule quantity and viscosity, after reaching prescribed limit, take out
Vacuum refining 30-60 minutes；
S4, unreacted complete monomer is carried out negative pressure rectifying, cooling down is filtered, obtains amino-polyether to 25 DEG C；
The preparation of flexible-epoxy comprises the steps：
S5, amino-polyether is added into polymerization reaction kettle, vacuumized, opened agitating device, be slowly added into bisphenol-f type glycidol ring
Oxygen tree fat, is filled with nitrogen pressure（0.01MPa.s-0.2MPa.s）, controlling reaction temperature is 110 DEG C -130 DEG C, is reacted 12 hours；
S6, sampling viscosimetric and epoxide number, after reaching product requirement, vacuumize 15-30 minutes, after cooling is filtered, obtain colourless
Bright flexible-epoxy.
The novel flexible epoxy resin that embodiment 2 is obtained carries out contrast with prior art products effect and shows：This enforcement
Example performance is better than comparative example really.Its correction data is as follows：
Embodiment 3
The preparation method of novel flexible epoxy resin proposed by the present invention, including preparation and the flexible-epoxy of amino-polyether
Prepare, the preparation of amino-polyether comprises the steps：
S1, polymerization reaction kettle is vacuumized, and it is secondary to be filled with nitrogen displacement；
S2, by butanediamine add polymerization reaction kettle in, open agitating device, control polymerization
The reaction temperature of reactor maintains 50 DEG C -60 DEG C and reaction pressure condition maintains 0.1MPa.s-0.6MPa.s；
S3, slowly it is uniformly added into oxirane into polymerization reaction kettle, treats that oxirane is made in polymerization reaction kettle after the completion of adding
Temperature keeps constant, reaches design time and starts sampling, surveys the index such as mean molecule quantity and viscosity, after reaching prescribed limit, take out
Vacuum refining 30-60 minutes；
S4, unreacted complete monomer is carried out negative pressure rectifying, cooling down is filtered, obtains amino-polyether to 25 DEG C；
The preparation of flexible-epoxy comprises the steps：
S5, amino-polyether is added into polymerization reaction kettle, vacuumized, opened agitating device, be slowly added into bisphenol S type glycidol ring
Oxygen tree fat, is filled with nitrogen pressure（0.01MPa.s-0.2MPa.s）, controlling reaction temperature is 90 DEG C -110 DEG C, and 10-12 is little for reaction
When；
S6, sampling viscosimetric and epoxide number, after reaching product requirement, vacuumize 15-30 minutes, after cooling is filtered, obtain slightly yellow
Transparent flexible epoxy resin.
The novel flexible epoxy resin that embodiment 3 is obtained carries out contrast with prior art products effect and shows：This enforcement
Example performance is better than comparative example really.Its correction data is as follows：
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its invention
Design in addition equivalent or change, should all be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of novel flexible epoxy resin, it is characterised in that:Preparation and flexible epoxy including amino-polyether
The preparation of the preparation of resin, wherein amino-polyether comprises the steps：
S1, polymerization reaction kettle is vacuumized, and it is secondary to be filled with nitrogen displacement；
S2, agitating device will be opened during amino initiator adds polymerization reaction kettle, control the reaction temperature of polymerization reaction kettle and anti-
Answer pressure condition；
S3, slowly it is uniformly added into raw material monomer into polymerization reaction kettle, treats that raw material monomer is made in polymerization reaction kettle after the completion of adding
Temperature keeps constant, reaches design time and starts sampling, surveys the index such as mean molecule quantity and viscosity, after reaching prescribed limit, take out
Vacuum refining 30-60 minutes；
S4, unreacted complete monomer is carried out negative pressure rectifying, cooling down is filtered, obtains amino-polyether to 25 DEG C；
The preparation of the flexible-epoxy comprises the steps：
S5, the amine terminated polyether of amino-polyether or mean molecule quantity 500-100000 is added into polymerization reaction kettle, vacuumize, open
Agitating device, is slowly added into epoxy resin, is filled with nitrogen pressure（0.01MPa.s-0.2MPa.s）, controlling reaction temperature is m, instead
It is n between seasonable；
S6, sampling viscosimetric and epoxide number, after reaching product requirement, vacuumize 15-30 minutes, after cooling is filtered, obtain flexible ring
Oxygen tree fat finished product.
2. the preparation method of novel flexible epoxy resin according to claim 1, it is characterised in that amino initiator in S2
For the mixture of one or two or more kinds in propane diamine, ethylenediamine, butanediamine, pentanediamine.
3. the preparation method of novel flexible epoxy resin according to claim 1, it is characterised in that in S2, reaction temperature
For 50 DEG C -130 DEG C, reaction pressure condition is 0.1MPa.s-1MPa.s.
4. the preparation method of novel flexible epoxy resin according to claim 1, it is characterised in that in S3, raw material monomer
For the mixture of one or two or more kinds in oxirane, expoxy propane, epoxy butane and tetrahydrofuran.
5. the preparation method of novel flexible epoxy resin according to claim 1, it is characterised in that the amino-polyether in S4
Molecular structure is NH2- (R-O-R) n-NH2 or NH2- [R-OCO-R] n-NH2.
6. the preparation method of novel flexible epoxy resin according to claim 1, it is characterised in that the epoxy resin in S5
For bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, cycloaliphatic epoxy resin, hydantoin epoxy tree
One of which in fat, low molecule tetraglycidel ether epoxy resin and ethylene oxidic ester epoxy resin.
7. the preparation method of novel flexible epoxy resin according to claim 1, it is characterised in that the value of m is in S5
60 DEG C -160 DEG C, the value of n is 4-16 hours.
8. the preparation method of novel flexible epoxy resin according to claim 1, it is characterised in that flexible ring oxygen tree in S6
The molecular structure of fat finished product is CH (O) CH-CH2OH-CH-NH- (R-O-R) n-NH-CH-CH2OH-CH (O) CH or CH (O)
CH—CH2OH-CH-NH-(R-O-R)n-NH-CH-CH2OH-CH(O)CH。
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| CN201610887994.2A CN106543414B (en) | 2016-10-12 | 2016-10-12 | A kind of preparation method of flexible-epoxy |
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| CN201610887994.2A CN106543414B (en) | 2016-10-12 | 2016-10-12 | A kind of preparation method of flexible-epoxy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330936A (en) * | 2019-06-10 | 2019-10-15 | 佳化化学科技发展（上海）有限公司 | The application and its adhesive of a kind of alkoxylated bisphenol F in the preparation of UV cured adhesive resin |
| CN115775648A (en) * | 2022-12-22 | 2023-03-10 | 潮州三环（集团）股份有限公司 | Conductive resin composition and preparation method and application thereof |
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| CN105348510A (en) * | 2015-12-01 | 2016-02-24 | 王伟跃 | Method for continuously producing amino-terminated polyether |
| CN105623265A (en) * | 2016-04-01 | 2016-06-01 | 中国科学院长春应用化学研究所 | Toughener and modified epoxy resin |
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| CN1368525A (en) * | 2000-01-31 | 2002-09-11 | 日本油漆株式会社 | Amino-polyether modified epoxy and cationic cataphoresis paint composition containing the epoxy |
| CN101220237A (en) * | 2008-01-22 | 2008-07-16 | 武汉理工大学 | Self-emulsifying aqueous epoxide resin paint and method for producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330936A (en) * | 2019-06-10 | 2019-10-15 | 佳化化学科技发展（上海）有限公司 | The application and its adhesive of a kind of alkoxylated bisphenol F in the preparation of UV cured adhesive resin |
| CN110330936B (en) * | 2019-06-10 | 2021-06-29 | 佳化化学科技发展（上海）有限公司 | Application of alkoxylated bisphenol F in preparation of UV (ultraviolet) curing adhesive resin and adhesive thereof |
| CN115775648A (en) * | 2022-12-22 | 2023-03-10 | 潮州三环（集团）股份有限公司 | Conductive resin composition and preparation method and application thereof |
| CN115775648B (en) * | 2022-12-22 | 2023-08-22 | 潮州三环（集团）股份有限公司 | Conductive resin composition and preparation method and application thereof |
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