CN105348489A - Self-emulsified epoxy resin curing agent - Google Patents
Self-emulsified epoxy resin curing agent Download PDFInfo
- Publication number
- CN105348489A CN105348489A CN201510941680.1A CN201510941680A CN105348489A CN 105348489 A CN105348489 A CN 105348489A CN 201510941680 A CN201510941680 A CN 201510941680A CN 105348489 A CN105348489 A CN 105348489A
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- CN
- China
- Prior art keywords
- self
- reaction
- emulsified epoxy
- ethylene glycol
- solidifying agent
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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
- C08G59/5006—Amines aliphatic
- C08G59/5013—Amines aliphatic containing more than seven carbon atoms, e.g. fatty amines
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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 self-emulsified epoxy resin curing agent comprising the following raw materials: octadecylamine, ethylene glycol and triethylenetetramine, wherein the ratio (mol ratio) of the raw materials, namely octadecylamine to ethylene glycol to triethylenetetramine, is equal to 1:(3-4):(2-3). A preparation method of the self-emulsified epoxy resin curing agent comprises the following steps of a, addition, namely slowly dropping an octadecylamine solution into ethylene glycol, and reacting at the temperature of 50-60 DEG C for 3-4h after ending dropwise adding operation; and b, blocking, namely slowly dropping an addition product into a triethylenetetramine solution when the temperature is up to 65 DEG C, and reacting at the temperature of 55-65 DEG C for 1-2h to obtain the self-emulsified epoxy resin curing agent after ending the reaction. In such a way, the self-emulsified epoxy resin curing agent is simple in preparation process, can be prepared without high-temperature reaction and organic neutralization salt formation reaction and is stable in performance as well as good in hydrophilcity and viscosity.
Description
Technical field
The present invention relates to epoxy resin field, particularly relate to a kind of Self-Emulsified Epoxy solidifying agent.
Background technology
Epoxypaint has that hardness is high, wear resistance good, sticking power is high and the feature such as chemical resistance is excellent, is widely used in field of coating.Along with improving constantly of people's environmental consciousness, many countries have promulgated the environmental regulation of restriction volatile organic solvent (VOC) in succession, the Water-borne modification of coating becomes the trend of paint development, and the self-emulsifying water borne epoxy resin curing agent that preparation matches seems particularly important.
In epoxy curing agent, amine curing agent kind is many, consumption is large, purposes is wide, but general amine curing agent at normal temperatures large, the toxicity of volatility large, solidify fast, proportioning too sternly, even absorbing carbon dioxide reduce effect.And self-emulsifying aqueous epoxy hardener is through traditional amine curing agent modification and obtains, which overcome the shortcoming of unmodified amine curing agent.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of Self-Emulsified Epoxy solidifying agent, and its preparation technology is simple, and without the need to pyroreaction, be neutralized into reactant salt without the need to organic acid and can obtain, its stable performance, good hydrophilic property, viscosity are good.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide a kind of Self-Emulsified Epoxy solidifying agent, its raw material comprises: stearylamine, ethylene glycol ethyl ether, triethylene tetramine, described each proportioning raw materials (mol than) is: stearylamine: ethylene glycol ethyl ether: triethylene tetramine=1:3-4:2-3, and it is as follows that the preparation method of described Self-Emulsified Epoxy solidifying agent comprises step:
A, addition: slowly instill in described ethylene glycol ethyl ether by described stearylamine solution, drip after terminating, reaction 3-4h, and temperature of reaction is 50-60 DEG C, is then taken out by adduct, is placed in constant pressure funnel;
B, end-blocking: 65 DEG C time, instill lentamente by adduct in triethylene tetramine solution, reaction 1-2h, and temperature of reaction is 55-65 DEG C, obtains Self-Emulsified Epoxy solidifying agent after reaction terminates.
In a preferred embodiment of the present invention, in described step a, described stearylamine is 1:3.5 with the mol ratio of described ethylene glycol ethyl ether.
In a preferred embodiment of the present invention, in described step b, in described affixture and triethylene tetramine reaction process, add the propylene glycol monomethyl ether of 10%.
The invention has the beneficial effects as follows: the present invention obtains affixture by the addition reaction of stearylamine and ethylene glycol ethyl ether, by triethylene tetramine, end-blocking is carried out to this affixture again, obtained Self-Emulsified Epoxy solidifying agent, this solidifying agent stable performance, productive rate are high, and the film effect finally prepared is good, preparation technology is simple simultaneously.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
A kind of Self-Emulsified Epoxy solidifying agent, its raw material comprises: stearylamine, ethylene glycol ethyl ether, triethylene tetramine, described each proportioning raw materials (mol than) is: stearylamine: ethylene glycol ethyl ether: triethylene tetramine=1:3-4:2-3, and it is as follows that the preparation method of described Self-Emulsified Epoxy solidifying agent comprises step:
A, addition: slowly instill in described ethylene glycol ethyl ether by described stearylamine solution, drip after terminating, reaction 3-4h, and temperature of reaction is 50-60 DEG C, is then taken out by adduct, is placed in constant pressure funnel;
B, end-blocking: 65 DEG C time, instill lentamente by adduct in triethylene tetramine solution, reaction 1-2h, and temperature of reaction is 55-65 DEG C, obtains Self-Emulsified Epoxy solidifying agent after reaction terminates.
Wherein, in described step a, described stearylamine is 1:3.5 with the mol ratio of described ethylene glycol ethyl ether.
In described step b, in described affixture and triethylene tetramine reaction process, add the propylene glycol monomethyl ether of 10%.The solidifying agent stable performance making to prepare, productive rate are high, can save salifying process simultaneously.
Embodiment one:
A kind of Self-Emulsified Epoxy solidifying agent, its raw material comprises: stearylamine, ethylene glycol ethyl ether, triethylene tetramine, and it is as follows that the preparation method of described Self-Emulsified Epoxy solidifying agent comprises step:
A, addition: slowly by stearylamine solution instillation ethylene glycol ethyl ether, wherein said stearylamine is 1:3.5 with the mol ratio of described ethylene glycol ethyl ether, drips after terminating, reaction 3h, and temperature of reaction is 60 DEG C, is then taken out by adduct, is placed in constant pressure funnel;
B, end-blocking: in triethylene tetramine, add the propylene glycol monomethyl ether solubility promoter of 10%, then 65 DEG C time, adduct is instilled lentamente in the mixing solutions of described triethylene tetramine and propylene glycol monomethyl ether, wherein said affixture is 2.8:1 with the mol ratio of described triethylene tetramine, reaction 1h, temperature of reaction is 65 DEG C, obtains Self-Emulsified Epoxy solidifying agent after reaction terminates.
Embodiment two:
A kind of Self-Emulsified Epoxy solidifying agent, its raw material comprises: stearylamine, ethylene glycol ethyl ether, triethylene tetramine, and it is as follows that the preparation method of described Self-Emulsified Epoxy solidifying agent comprises step:
A, addition: slowly by stearylamine solution instillation ethylene glycol ethyl ether, wherein said stearylamine is 1:3.5 with the mol ratio of described ethylene glycol ethyl ether, drips after terminating, reaction 4h, and temperature of reaction is 50 DEG C, is then taken out by adduct, is placed in constant pressure funnel;
B, end-blocking: end-blocking: in triethylene tetramine, add the propylene glycol monomethyl ether solubility promoter of 10%, then 65 DEG C time, adduct is instilled lentamente in the mixing solutions of described triethylene tetramine and propylene glycol monomethyl ether, wherein said affixture is 3:1 with the mol ratio of described triethylene tetramine, reaction 2h, temperature of reaction is 55 DEG C, obtains Self-Emulsified Epoxy solidifying agent after reaction terminates.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (3)
1. a Self-Emulsified Epoxy solidifying agent, it is characterized in that, its raw material comprises: stearylamine, ethylene glycol ethyl ether, triethylene tetramine, described each proportioning raw materials (mol than) is: stearylamine: ethylene glycol ethyl ether: triethylene tetramine=1:3-4:2-3, and it is as follows that the preparation method of described Self-Emulsified Epoxy solidifying agent comprises step:
A, addition: slowly instill in described ethylene glycol ethyl ether by described stearylamine solution, drip after terminating, reaction 3-4h, and temperature of reaction is 50-60 DEG C, is then taken out by adduct, is placed in constant pressure funnel;
B, end-blocking: 65 DEG C time, instill lentamente by adduct in triethylene tetramine solution, reaction 1-2h, and temperature of reaction is 55-65 DEG C, obtains Self-Emulsified Epoxy solidifying agent after reaction terminates.
2. Self-Emulsified Epoxy solidifying agent according to claim 1, is characterized in that, in described step a, described stearylamine is 1:3.5 with the mol ratio of described ethylene glycol ethyl ether.
3. Self-Emulsified Epoxy solidifying agent according to claim 1, is characterized in that, in described step b, in described affixture and triethylene tetramine reaction process, adds the propylene glycol monomethyl ether of 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510941680.1A CN105348489A (en) | 2015-12-16 | 2015-12-16 | Self-emulsified epoxy resin curing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510941680.1A CN105348489A (en) | 2015-12-16 | 2015-12-16 | Self-emulsified epoxy resin curing agent |
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| Publication Number | Publication Date |
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| CN105348489A true CN105348489A (en) | 2016-02-24 |
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| CN201510941680.1A Pending CN105348489A (en) | 2015-12-16 | 2015-12-16 | Self-emulsified epoxy resin curing agent |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624385A (en) * | 2009-06-23 | 2010-01-13 | 中国科学院广州化学研究所 | Non-ionic self-emulsifying aqueous epoxy hardener and preparation method and application thereof |
| CN101891936A (en) * | 2010-08-06 | 2010-11-24 | 上海交通大学 | Preparation method of composite material based on epoxy resin and phosphazene nanotubes |
| CN103172832A (en) * | 2013-04-10 | 2013-06-26 | 湖北奥生新材料科技有限公司 | Epoxy resin early-strength curing agent for binding and preparation method thereof |
| CN104072726A (en) * | 2014-06-06 | 2014-10-01 | 苏州之诺新材料科技有限公司 | Epoxy resin curing agent and modification method thereof |
| CN104559066A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Mid-temperature curing epoxy resin composition for melting prepared prepreg and preparation method of composition |
| CN104788647A (en) * | 2015-04-02 | 2015-07-22 | 沈阳化工大学 | Phosphorous-containing epoxy resin amine curing agent and preparation method thereof |
-
2015
- 2015-12-16 CN CN201510941680.1A patent/CN105348489A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624385A (en) * | 2009-06-23 | 2010-01-13 | 中国科学院广州化学研究所 | Non-ionic self-emulsifying aqueous epoxy hardener and preparation method and application thereof |
| CN101891936A (en) * | 2010-08-06 | 2010-11-24 | 上海交通大学 | Preparation method of composite material based on epoxy resin and phosphazene nanotubes |
| CN103172832A (en) * | 2013-04-10 | 2013-06-26 | 湖北奥生新材料科技有限公司 | Epoxy resin early-strength curing agent for binding and preparation method thereof |
| CN104559066A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Mid-temperature curing epoxy resin composition for melting prepared prepreg and preparation method of composition |
| CN104072726A (en) * | 2014-06-06 | 2014-10-01 | 苏州之诺新材料科技有限公司 | Epoxy resin curing agent and modification method thereof |
| CN104788647A (en) * | 2015-04-02 | 2015-07-22 | 沈阳化工大学 | Phosphorous-containing epoxy resin amine curing agent and preparation method thereof |
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Application publication date: 20160224 |