CN105037690A - Low-temperature epoxy resin curing agent and preparation method thereof - Google Patents

Low-temperature epoxy resin curing agent and preparation method thereof Download PDF

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Publication number
CN105037690A
CN105037690A CN201510336562.8A CN201510336562A CN105037690A CN 105037690 A CN105037690 A CN 105037690A CN 201510336562 A CN201510336562 A CN 201510336562A CN 105037690 A CN105037690 A CN 105037690A
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parts
epoxy resin
agent
curing agent
low temperature
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牛无畏
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Abstract

The invention discloses a low-temperature epoxy resin curing agent and a preparation method thereof. The low-temperature epoxy resin curing agent comprises the following components in parts by weight: 50-65 parts of modified aromatic amine, 10-20 parts of formaldehyde, 5-15 parts of boron trifluoride, 2-6 parts of a modifying agent, 1-10 parts of a coupling agent and 15-25 parts of a diluent. According to the low-temperature epoxy resin curing agent prepared by adopting the preparation method provided by the invention, modified aromatic amine is selected for use, so that the corrosion resistance and the mechanical property of the agent are good, the adaptability is strong, the curing reaction speed is high, environmental protection and nontoxicity are achieved, no toxic effect is caused to the environment and human bodies, application at a low temperature or under a humid environment can be realized, the compatibility of the agent with epoxy resin is good, and an excellent oil and water resisting property is achieved.

Description

A kind of low Temperature Curing Agent for Epoxy Resin and preparation method thereof
Technical field
The present invention relates to solidifying agent field, particularly relate to a kind of low Temperature Curing Agent for Epoxy Resin and preparation method thereof.
Background technology
Synthetic epoxy resin generally all needs to add solidifying agent, to improve solidification and the use properties of epoxy resin further.Nowadays, the research and development of epoxide resin material are mainly concentrated on improve its feature of environmental protection both at home and abroad, comprise no-solvent type epoxy resin material and aqueous epoxy resins material.But in the improvement of the bonding of epoxide resin material in low temperature and water surrounding and curing performance, the research done is not also very ripe.
At present, low temperature curing agent conventional on market is aliphatics amine curing agent, and representative has: (1) fatty amine curing agent; (2) pnenolic aldehyde amine hardener; (3) alicyclic polyamine solidifying agent.But they all also exist the shortcoming of oneself, as bad with epoxy resin compatibility; Low-temperature curing is incomplete, curing speed is slow, solidifying agent solvent absorbs water and makes epoxy resin surface albefaction etc.
Summary of the invention
The object of the invention is to the deficiency overcoming the existence of above-mentioned prior art, the low Temperature Curing Agent for Epoxy Resin that a kind of curing reaction speed is fast, strong adaptability, mechanical property are good is provided.
Meanwhile, present invention also offers a kind of preparation method of low Temperature Curing Agent for Epoxy Resin.
For achieving the above object, the present invention is achieved by the following technical solutions:
A kind of low Temperature Curing Agent for Epoxy Resin, meter comprises following component by weight: modified aromatic amine 50 ~ 65 parts, 10 ~ 20 parts, formaldehyde, boron trifluoride 5 ~ 15 parts, properties-correcting agent 2 ~ 6 parts, coupling agent 1 ~ 10 part, thinner 15 ~ 25 parts.
Preferably, described properties-correcting agent is any one in THIOGLYCOL, polyamide resin, isocyanic ester.
Preferably, described coupling agent is any one in type siloxane coupling agent, aluminate coupling agent, titanate coupling agent.
Preferably, described thinner is any one in polypropylene glycol diglycidyl ether, phenyl glycidyl ether, toluene, acetone.
Above-mentioned low Temperature Curing Agent for Epoxy Resin, its processing step prepared is as follows:
(1) mark ratio takes raw material by weight;
(2) phenol step (1) taken under room temperature, formaldehyde, boron trifluoride are poured in reactor, stir, be warming up to 60 ~ 80 DEG C in whipping process with the rotating speed of 800 ~ 1000 revs/min; Add step (1) and take properties-correcting agent stirring 1 ~ 3 hour, then be warming up to 70 ~ 90 DEG C;
(3) regulate pH7 ~ 8, add all the other raw materials that step (1) takes, constant temperature back flow reaction was cooled to normal temperature after 2 ~ 4 hours, obtained low Temperature Curing Agent for Epoxy Resin.
Beneficial effect of the present invention:
Low Temperature Curing Agent for Epoxy Resin prepared by the present invention, modified aromatic amine selected by solidifying agent, erosion resistance and mechanical property is good, strong adaptability, curing reaction speed are fast, environment-protecting asepsis, environment and human body are not produced and poison, can apply under low temperature or wet environment, good with epoxy resin compatibility, and there is good oil resistant water tolerance.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
A kind of low Temperature Curing Agent for Epoxy Resin, meter comprises following component by weight: modified aromatic amine 50 ~ 65 parts, 10 ~ 20 parts, formaldehyde, boron trifluoride 5 ~ 15 parts, properties-correcting agent 2 ~ 6 parts, coupling agent 1 ~ 10 part, thinner 15 ~ 25 parts.
The processing step of preparation is as follows:
(1) mark ratio takes raw material by weight;
(2) phenol step (1) taken under room temperature, formaldehyde, boron trifluoride are poured in reactor, stir, be warming up to 60 ~ 80 DEG C in whipping process with the rotating speed of 800 ~ 1000 revs/min; Add step (1) and take properties-correcting agent stirring 1 ~ 3 hour, then be warming up to 70 ~ 90 DEG C;
(3) regulate pH7 ~ 8, add all the other raw materials that step (1) takes, constant temperature back flow reaction was cooled to normal temperature after 2 ~ 4 hours, obtained low Temperature Curing Agent for Epoxy Resin.
Low Temperature Curing Agent for Epoxy Resin prepared by the present invention, has the advantages such as curing reaction speed is fast, strong adaptability, mechanical property are good.
Embodiment 1
Low Temperature Curing Agent for Epoxy Resin of the present invention, meter comprises following component by weight: modified aromatic amine 50 parts, 20 parts, formaldehyde, boron trifluoride 15 parts, properties-correcting agent 2 parts, coupling agent 1 part, thinner 25 parts.
The processing step of preparation is as follows:
(1) mark ratio takes raw material by weight;
(2) phenol step (1) taken under room temperature, formaldehyde, boron trifluoride are poured in reactor, stir, be warming up to 60 DEG C in whipping process with the rotating speed of 800 revs/min; Add step (1) to take properties-correcting agent and stir 1 hour, then be warming up to 70 DEG C;
(3) regulate pH7, add all the other raw materials that step (1) takes, constant temperature back flow reaction was cooled to normal temperature after 2 hours, obtained low Temperature Curing Agent for Epoxy Resin.
Embodiment 2
Low Temperature Curing Agent for Epoxy Resin of the present invention, meter comprises following component by weight: modified aromatic amine 65 parts, 10 parts, formaldehyde, boron trifluoride 5 parts, properties-correcting agent 6 parts, coupling agent 10 parts, thinner 15 parts.
The processing step of preparation is as follows:
(1) mark ratio takes raw material by weight;
(2) phenol step (1) taken under room temperature, formaldehyde, boron trifluoride are poured in reactor, stir, be warming up to 80 DEG C in whipping process with the rotating speed of 1000 revs/min; Add step (1) to take properties-correcting agent and stir 3 hours, then be warming up to 90 DEG C;
(3) regulate pH8, add all the other raw materials that step (1) takes, constant temperature back flow reaction was cooled to normal temperature after 4 hours, obtained low Temperature Curing Agent for Epoxy Resin.
Embodiment 3
Low Temperature Curing Agent for Epoxy Resin of the present invention, meter comprises following component by weight: modified aromatic amine 58 parts, 15 parts, formaldehyde, boron trifluoride 10 parts, properties-correcting agent 4 parts, coupling agent 6 parts, thinner 20 parts.
The processing step of preparation is as follows:
(1) mark ratio takes raw material by weight;
(2) phenol step (1) taken under room temperature, formaldehyde, boron trifluoride are poured in reactor, stir, be warming up to 70 DEG C in whipping process with the rotating speed of 900 revs/min; Add step (1) to take properties-correcting agent and stir 2 hours, then be warming up to 80 DEG C;
(3) regulate pH7, add all the other raw materials that step (1) takes, constant temperature back flow reaction was cooled to normal temperature after 2 ~ 4 hours, obtained low Temperature Curing Agent for Epoxy Resin.
Embodiment 4
Low Temperature Curing Agent for Epoxy Resin of the present invention, meter comprises following component by weight: modified aromatic amine 52 parts, 18 parts, formaldehyde, boron trifluoride 12 parts, properties-correcting agent 5 parts, coupling agent 8 parts, thinner 21 parts.
The processing step of preparation is as follows:
(1) mark ratio takes raw material by weight;
(2) phenol step (1) taken under room temperature, formaldehyde, boron trifluoride are poured in reactor, stir, be warming up to 75 DEG C in whipping process with the rotating speed of 800 revs/min; Add step (1) and take properties-correcting agent stirring 1 ~ 3 hour, then be warming up to 75 DEG C;
(3) regulate pH8, add all the other raw materials that step (1) takes, constant temperature back flow reaction was cooled to normal temperature after 2.5 hours, obtained low Temperature Curing Agent for Epoxy Resin.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.

Claims (5)

1. a low Temperature Curing Agent for Epoxy Resin, is characterized in that, meter comprises following component by weight: modified aromatic amine 50 ~ 65 parts, 10 ~ 20 parts, formaldehyde, boron trifluoride 5 ~ 15 parts, properties-correcting agent 2 ~ 6 parts, coupling agent 1 ~ 10 part, thinner 15 ~ 25 parts.
2. low Temperature Curing Agent for Epoxy Resin according to claim 1, is characterized in that: described properties-correcting agent is any one in THIOGLYCOL, polyamide resin, isocyanic ester.
3. low Temperature Curing Agent for Epoxy Resin according to claim 1, is characterized in that: described coupling agent is any one in type siloxane coupling agent, aluminate coupling agent, titanate coupling agent.
4. low Temperature Curing Agent for Epoxy Resin according to claim 1, is characterized in that: described thinner is any one in polypropylene glycol diglycidyl ether, phenyl glycidyl ether, toluene, acetone.
5. a preparation method for low Temperature Curing Agent for Epoxy Resin as claimed in claim 1, is characterized in that, comprises the following steps:
(1) mark ratio takes raw material by weight;
(2) phenol step (1) taken under room temperature, formaldehyde, boron trifluoride are poured in reactor, stir, be warming up to 60 ~ 80 DEG C in whipping process with the rotating speed of 800 ~ 1000 revs/min; Add step (1) and take properties-correcting agent stirring 1 ~ 3 hour, then be warming up to 70 ~ 90 DEG C;
(3) regulate pH7 ~ 8, add all the other raw materials that step (1) takes, constant temperature back flow reaction was cooled to normal temperature after 2 ~ 4 hours, obtained low Temperature Curing Agent for Epoxy Resin.
CN201510336562.8A 2015-06-17 2015-06-17 Low-temperature epoxy resin curing agent and preparation method thereof Pending CN105037690A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106883691A (en) * 2017-04-18 2017-06-23 德阳森华新材料科技有限公司 Cold aqueous non-corrosive metal (NCM) coating
CN107952481A (en) * 2017-11-09 2018-04-24 同济大学 A kind of porous material catalyst of supported precious metal nano-particle and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1640980A (en) * 2004-11-17 2005-07-20 袁宏伟 Ceramic wine glass anticounterfeit epoxy adhesive and its preparing method
CN1670109A (en) * 2005-05-11 2005-09-21 李洁华 Modified epoxy resin adhesive and its preparation process
CN1690154A (en) * 2004-04-28 2005-11-02 陈惠� Double component adhesive for double-ply board
CN101531872A (en) * 2009-04-28 2009-09-16 黑龙江省科学院石油化学研究院 Room curing fluoro rubber adhesive and preparation method
WO2013179915A1 (en) * 2012-05-29 2013-12-05 三菱瓦斯化学株式会社 Aromatic aldehyde, epoxy resin curing agent comprising aromatic aldehyde, and epoxy resin composition comprising same
CN103627143A (en) * 2013-11-29 2014-03-12 拉法基技术服务(北京)有限公司 Binder and preparation method thereof
CN103849296A (en) * 2014-02-28 2014-06-11 北京东方雨虹防水技术股份有限公司 Elastic epoxy resin waterproof coating and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1690154A (en) * 2004-04-28 2005-11-02 陈惠� Double component adhesive for double-ply board
CN1640980A (en) * 2004-11-17 2005-07-20 袁宏伟 Ceramic wine glass anticounterfeit epoxy adhesive and its preparing method
CN1670109A (en) * 2005-05-11 2005-09-21 李洁华 Modified epoxy resin adhesive and its preparation process
CN101531872A (en) * 2009-04-28 2009-09-16 黑龙江省科学院石油化学研究院 Room curing fluoro rubber adhesive and preparation method
WO2013179915A1 (en) * 2012-05-29 2013-12-05 三菱瓦斯化学株式会社 Aromatic aldehyde, epoxy resin curing agent comprising aromatic aldehyde, and epoxy resin composition comprising same
CN103627143A (en) * 2013-11-29 2014-03-12 拉法基技术服务(北京)有限公司 Binder and preparation method thereof
CN103849296A (en) * 2014-02-28 2014-06-11 北京东方雨虹防水技术股份有限公司 Elastic epoxy resin waterproof coating and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106883691A (en) * 2017-04-18 2017-06-23 德阳森华新材料科技有限公司 Cold aqueous non-corrosive metal (NCM) coating
CN107952481A (en) * 2017-11-09 2018-04-24 同济大学 A kind of porous material catalyst of supported precious metal nano-particle and preparation method thereof
CN107952481B (en) * 2017-11-09 2020-07-28 同济大学 Noble metal nanoparticle-loaded porous material catalyst and preparation method thereof

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Application publication date: 20151111