CN102898624A - Epoxy resin curing agent and preparation method thereof - Google Patents
Epoxy resin curing agent and preparation method thereof Download PDFInfo
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- CN102898624A CN102898624A CN2012104222581A CN201210422258A CN102898624A CN 102898624 A CN102898624 A CN 102898624A CN 2012104222581 A CN2012104222581 A CN 2012104222581A CN 201210422258 A CN201210422258 A CN 201210422258A CN 102898624 A CN102898624 A CN 102898624A
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Abstract
The invention discloses epoxy resin curing agent and a preparation method thereof. The epoxy resin curing agent comprises the following components in percentage by mass: 40 to 50 percent of phenylcarbinol, 30 to 45 percent of isophorone diamine, 10 to 20 percent of epoxy resin, 0.1 to 1 percent of anti-scratch wax, and 1 to 5 percent of an accelerating agent. The method for preparing the epoxy resin curing agent comprises the following steps of: adding proper phenylcarbinol and isophorone diamine into a reaction kettle; uniformly stirring the phenylcarbinol and isophorone diamine, and adding the epoxy resin into the reaction kettle; stirring and heating with steam until the temperature of the reaction liquid is 60 to 75 DEG C; keeping on reaction for 2 hours, and adding the anti-scratch wax and the accelerating agent Schiff base into the reaction kettle; and uniformly dispersing, cooling and subpackaging. By the mode, the invention can provide the epoxy resin curing agent with high hardness and good weather resistance, which is excellent in self-leveling effect when being mixed with an epoxy self-leveling host, good in coating weather resistance after being cured, and high in hardness.
Description
Technical field:
The present invention relates to the epoxy curing agent field, specifically, relate to good epoxy curing agent of a kind of hardness high-weatherability and preparation method thereof.
Background technology:
Resins, epoxy is widely used in the fields such as civil construction, electronic apparatus, space flight and aviation, automobile mechanical, is the important component part of national product, and China is the maximum Resins, epoxy producing country in the whole world at present, and output is 37.1% of the world.Yet Resins, epoxy is a kind of amorphous thick liquid, heating is plasticity, there is not obvious fusing point, the deliquescing of being heated is melted and stickness gradually, water insoluble, itself can not harden, so it does not almost have independent use value, only has with the cancellated not cladding polymer of solidifying agent reaction generating three-dimensional using value is just arranged.After adding a certain amount of solidifying agent, just solidify to form gradually the different chemical substance of performance, therefore, must add solidifying agent, the compositing formula resin, and be cured reaction under certain condition, generate the macromolecular material of tridimensional network, just can show various good performances, become the epoxy material with real use value.
Epoxy curing agent commonly used is divided into alkaline species solidifying agent and acid class solidifying agent, and the alkaline species solidifying agent mainly comprises aliphatie diamine and polyamines, aliphatic cyclic amine, aromatic polyamine compound and modified polyether amine, aromatics is better as the solidifying agent hardness of film, but the weathering resistance of filming is not good enough, the aliphatic polyamine weathering resistance is better, but the easy moisture absorption and make and film whiting or produce greasy dirt; Polyetheramine and epoxy host film-forming coating are more pliable and tougher, and hardness is not high.
The polyamine curing agent that uses now such as diethylenetriamine, triethylene tetramine compound volatilize easily, and smell is larger, and environment is caused larger harm; The aromatic amine solidifying agent such as mphenylenediamine and epoxy host film-forming weathering resistance are relatively poor, and xanthochromia occurs easily, can not be used for place outdoor or that solar radiation is stronger; The coating of polyetheramine solidifying agent and epoxy host film-forming is soft, and Resins, epoxy films also not wear-resistingly, so duration of service can be not longer, and duration of service, longer appearance effect was relatively poor.
Summary of the invention:
For above-mentioned deficiency of the prior art, the epoxy curing agent and the manufacture craft thereof that provide a kind of hardness high-weatherability good is provided the object of the invention, Self-leveling was respond well after this epoxy curing agent mixed with Resins, epoxy host, the filmogen good weatherability, and hardness is high, and shore hardness (D) can reach more than 85, and set time is suitable, surface drying time 2-3 hour, the time of doing solid work was 12 hours.
For achieving the above object, technical scheme disclosed by the invention is: a kind of epoxy curing agent, and each component of described epoxy curing agent by mass percent is: phenylcarbinol-40%-50%, isophorone diamine 30%-45%, Resins, epoxy 10%-20%, scratch resistance wax 0.1%-1%, promotor 1%-5%.
What preferably, described promotor was adopted is Schiff's base.In concrete the production, can also add according to the condition of production promotor of other types.
What further, described Schiff's base adopted is 2,4,6-three (dimethylamino methyl) phenol.In concrete the production, can also add according to the condition of production Schiff's base of other types.
Preferably, described Resins, epoxy adopts E-51 Resins, epoxy or E-44 Resins, epoxy.In concrete the production, can also be according to the Resins, epoxy of other kinds of practical situation choice for use, as: E-54 Resins, epoxy, E-20 Resins, epoxy.
A kind of preparation method of epoxy curing agent, operate as follows: in reactor, add an amount of phenylcarbinol, isophorone diamine, after both are stirred, in reactor, add Resins, epoxy, continued stirring reaction 2 hours after being steam heated to while stirring reacting liquid temperature and reaching 60-75 ℃, then in reactor, add scratch resistance wax and promotor, be uniformly dispersed, packing after the cooling.For guaranteeing quality product, while stirring steam heating control reacting liquid temperature is at 60-75 ℃.
Further, because epoxy curing agent of the present invention is mixing with Resins, epoxy when using, can affect because of the difference of construction environment temperature both speed of response, so for solidifying agent of the present invention and Resins, epoxy are used, in preparation process, when the construction environment temperature of solidifying agent is higher than 20 when spending, the mass percent of the component promotor of adding in the preparation manipulation is 1%-3%; When the construction environment temperature of solidifying agent is lower than 20 when spending, the mass percent of the component promotor of adding in the preparation manipulation is 3%-5%.
The effect of the promotor of adding among the present invention is: the speed of accelerating the resin film forming; The effect of scratch resistance wax is: the adhesion strength that strengthens paint film.
Utilize isophorone diamine and Resins, epoxy in phenylcarbinol, to heat among the present invention, reaction by between the two makes the isophorone diamine modification obtain epoxide modified isophorone diamine, strengthen the consistency of solidifying agent and Resins, epoxy, and realize solvent free in the operation, the product Self-leveling is effective.
The invention has the beneficial effects as follows: the epoxy curing agent among the present invention mixes use with epoxy coating host, weathering resistance that can reinforced epoxy coating, make the anti-accelerated deterioration performance of coating improve more than 10%, scratch resistance wax in the epoxy curing agent also can the reinforced epoxy paint coatings hardness, the shore hardness of epoxy coating coating is reached more than 85.After epoxy curing agent of the present invention cooperates epoxy coating host to use, make the paint solidification time suitable, satisfy the construction demand.
Embodiment:
Below in conjunction with preferred embodiment of the present invention technical scheme of the present invention is described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that protection scope of the present invention is made more explicit defining.
Embodiment one: a kind of epoxy curing agent, its component by mass percent is: phenylcarbinol 40%, isophorone diamine 45%, Resins, epoxy 13%, scratch resistance wax 1%, promotor 1%.
The preparation method of this epoxy curing agent is as follows: add phenylcarbinol, isophorone diamine in reactor, after both are stirred, in reactor, add Resins, epoxy, steam heating after reacting liquid temperature reaches 60 ℃, continued stirring reaction 2 hours while stirring, then in reactor, add scratch resistance wax and promotor, after being uniformly dispersed, naturally cooling obtains the product epoxy curing agent.What Resins, epoxy adopted in the present embodiment is E-51 Resins, epoxy, and what promotor was adopted is Schiff's base promotor.
This epoxy curing agent and epoxy self-leveling coating host are that the shore hardness of epoxy coating paint film is 83 after mixing use under the temperature condition of 25 degree in construction environment, and surface drying time is 2 hours, and the time of doing solid work is 12 hours.
Embodiment two: utilize preparation method of the present invention to prepare epoxy curing agent, in reactor, add 50 Kg phenylcarbinols, 30 Kg isophorone diamines, after both are stirred, add the E-20 Resins, epoxy of 15 Kg in the reactor, steam heating while stirring, after reacting liquid temperature reaches 65 ℃, continued stirring reaction 2 hours, then add 0.3Kg scratch resistance wax and 4.7Kg promotor Schiff's base in the reactor and be uniformly dispersed.Behind the naturally cooling, obtain product epoxy curing agent 100Kg.This epoxy curing agent mixes use with epoxy self-leveling coating host after, the shore hardness of epoxy coating paint film is 80, and surface drying time is 3 hours, and the time of doing solid work is 12 hours.
Embodiment three: a kind of epoxy curing agent, its component by mass percent is: phenylcarbinol 45%, isophorone diamine 30%, E-51 Resins, epoxy 20 %, 0.4% scratch resistance wax, promotor Schiff's base 4.6%.
The preparation method of this epoxy curing agent is as follows: add 45Kg phenylcarbinol, 30Kg isophorone diamine in reactor, after both are stirred, add the E-51 Resins, epoxy of 20 Kg in the reactor, steam heating while stirring, in the reaction process, isophorone diamine and the reaction of E-51 Resins, epoxy make the isophorone diamine modification.After reacting liquid temperature reaches 70 ℃, continued stirring reaction 2 hours, then in reactor, add 0.4Kg scratch resistance wax and 4.6Kg promotor Schiff's base, be uniformly dispersed, behind the naturally cooling, obtain product epoxy curing agent 100Kg.
This epoxy curing agent mixes use with epoxy self-leveling coating host after, the shore hardness of epoxy coating paint film is 86, and surface drying time is 2.5 hours, and the time of doing solid work is 12 hours.
Embodiment four: a kind of epoxy curing agent, its each component by mass percent is: phenylcarbinol 40%, isophorone diamine 45%, Resins, epoxy 10%, scratch resistance wax 0.8%, promotor 4.2%.Its preparation method is with the preparation method among the embodiment one.
The Resins, epoxy that adopts among the embodiment is E-54 Resins, epoxy, and what promotor was adopted is 2,4,6-three (dimethylamino methyl) phenol.This epoxy curing agent mix with epoxy self-leveling coating host use under construction environment is 16 ℃ temperature condition, mix use after, the shore hardness of epoxy coating paint film is 86, surface drying time is 2.5 hours, the time of doing solid work is 12 hours.
Embodiment five: utilize preparation method of the present invention to prepare epoxy curing agent, press mass percent and in reactor, add phenylcarbinol 40%, isophorone diamine 40%, after both are stirred, in reactor, add E-54 Resins, epoxy 14%, while stirring steam heating, after reacting liquid temperature reaches 60 ℃, continued stirring reaction 2 hours, and then in reactor, added scratch resistance wax 1% and promotor Schiff's base 5%, be uniformly dispersed, behind the naturally cooling, obtain the product epoxy curing agent.
This epoxy curing agent and epoxy self-leveling coating host in construction environment be mix under 10 ℃ the temperature condition use after, the shore hardness of epoxy coating paint film is 87, surface drying time is 3 hours, the time of doing solid work is 14 hours.
Embodiment six: utilize preparation method of the present invention to prepare epoxy curing agent, in reactor, add 40Kg phenylcarbinol, 40Kg isophorone diamine, after both are stirred, add 17KgE-44 Resins, epoxy in the reactor, steam heating while stirring is after reacting liquid temperature reaches 75 ℃, continued stirring reaction 2 hours, then add 0.5Kg scratch resistance wax and 2.5Kg promotor Schiff's base in the reactor and be uniformly dispersed, behind the naturally cooling, obtain product epoxy curing agent 100Kg.In the reaction process, isophorone diamine and the reaction of E-44 Resins, epoxy make the isophorone diamine modification.
This epoxy curing agent mixes use with epoxy self-leveling coating host after, the shore hardness of epoxy coating paint film is 87, and surface drying time is 2 hours, and the time of doing solid work is 12 hours.
Embodiment seven: a kind of epoxy curing agent, its each component by mass percent is: phenylcarbinol 41%, isophorone diamine 45%, E-51 Resins, epoxy 10%, scratch resistance wax 1%, promotor 3%.Its preparation method is with the preparation method among the embodiment one.
This epoxy curing agent mix with epoxy self-leveling coating host use under construction environment is 16 ℃ temperature condition, mix use after, the shore hardness of epoxy coating paint film is 87, surface drying time is 3 hours, the time of doing solid work is 12 hours.
Embodiment eight: a kind of epoxy curing agent, its each component by mass percent is: phenylcarbinol 42%, isophorone diamine 45%, E-44 Resins, epoxy 10%, scratch resistance wax 1%, promotor 2%.Its preparation method is with the preparation method among the embodiment one, and what wherein promotor was adopted is 2,4,6-three (dimethylamino methyl) phenol.
This epoxy curing agent mix with epoxy self-leveling coating host use under construction environment is 22 ℃ temperature condition, mix use after, the shore hardness of epoxy coating paint film is 88, surface drying time is 2 hours, the time of doing solid work is 11 hours.
The above only is embodiments of the invention; be not so limit claim of the present invention; every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (9)
1. an epoxy curing agent is characterized in that, each component of described epoxy curing agent by mass percent is: phenylcarbinol 40%--50%, isophorone diamine 30%--45%, Resins, epoxy 10%--20%, scratch resistance wax 0.1%--1%, promotor 1%--5%.
2. a kind of epoxy curing agent described in according to claim 1 is characterized in that, what described promotor was adopted is Schiff's base.
3. a kind of epoxy curing agent described in according to claim 2 is characterized in that, what described Schiff's base adopted is 2,4,6-three (dimethylamino methyl) phenol.
4. a kind of epoxy curing agent described in according to claim 1 is characterized in that, described Resins, epoxy adopts E-51 Resins, epoxy or E-44 Resins, epoxy.
5. according to claim 1 and 2 or 3 or 4 described a kind of epoxy curing agents, it is characterized in that each component of described epoxy curing agent by mass percent is: phenylcarbinol 40%, isophorone diamine 45%, Resins, epoxy 13%, scratch resistance wax 1%, promotor 1%.
6. according to claim 1 and 2 or 3 or 4 described a kind of epoxy curing agents, it is characterized in that each component of described epoxy curing agent by mass percent is: phenylcarbinol 40%, isophorone diamine 45%, Resins, epoxy 10%, scratch resistance wax 0.8%, promotor 4.2%.
7. a kind of epoxy curing agent according to claim 4 is characterized in that, each component of described epoxy curing agent by mass percent is: phenylcarbinol 41%, isophorone diamine 45%, E-51 Resins, epoxy 10%, scratch resistance wax 1%, promotor 3%.
8. a kind of epoxy curing agent according to claim 4 is characterized in that, each component of described epoxy curing agent by mass percent is: phenylcarbinol 42%, isophorone diamine 45%, E-44 Resins, epoxy 10%, scratch resistance wax 1%, promotor 2%.
9. the preparation method of an epoxy curing agent, operate as follows: in reactor, add an amount of phenylcarbinol, isophorone diamine, after both are stirred, in reactor, add Resins, epoxy, continued stirring reaction 2 hours after being steam heated to while stirring reacting liquid temperature and reaching 60-75 ℃, then in reactor, add scratch resistance wax and promotor, be uniformly dispersed, packing after the cooling.
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| CN201210422258.1A CN102898624B (en) | 2012-10-29 | 2012-10-29 | Epoxy resin curing agent and preparation method thereof |
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| CN201210422258.1A CN102898624B (en) | 2012-10-29 | 2012-10-29 | Epoxy resin curing agent and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224612A (en) * | 2013-05-15 | 2013-07-31 | 程梦喜 | Solvent-free self-leveling epoxy resin curing agent 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 |
| CN104893255A (en) * | 2015-06-05 | 2015-09-09 | 安徽凯盛众普新光源有限公司 | Curing agent and preparation method thereof |
| CN104892908A (en) * | 2015-06-05 | 2015-09-09 | 安徽凯盛众普新光源有限公司 | Epoxy resin curing agent and preparation method thereof |
| CN108962585A (en) * | 2018-07-19 | 2018-12-07 | 德阳新源电器有限责任公司 | A kind of continuous disk-type winding pouring technology |
| CN109824869A (en) * | 2019-01-31 | 2019-05-31 | 厦门源创力科技服务有限公司 | A kind of epoxy curing agent and preparation method thereof |
| CN110358404A (en) * | 2019-06-21 | 2019-10-22 | 江苏兰陵高分子材料有限公司 | A kind of weather-proof coating of non-solvent epoxy for outdoor weighing apparatus and preparation process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255325A (en) * | 2007-02-28 | 2008-09-03 | 上海华夏化工材料有限公司 | Synthesis technique of dual-component wet and heat ageing resistant epoxy building structure strengthening adhesive |
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2012
- 2012-10-29 CN CN201210422258.1A patent/CN102898624B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255325A (en) * | 2007-02-28 | 2008-09-03 | 上海华夏化工材料有限公司 | Synthesis technique of dual-component wet and heat ageing resistant epoxy building structure strengthening adhesive |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224612A (en) * | 2013-05-15 | 2013-07-31 | 程梦喜 | Solvent-free self-leveling epoxy resin curing agent and preparation method thereof |
| CN103224612B (en) * | 2013-05-15 | 2016-02-24 | 程梦喜 | A kind of solvent-free self leveling epoxy resin curing agent 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 |
| CN104893255A (en) * | 2015-06-05 | 2015-09-09 | 安徽凯盛众普新光源有限公司 | Curing agent and preparation method thereof |
| CN104892908A (en) * | 2015-06-05 | 2015-09-09 | 安徽凯盛众普新光源有限公司 | Epoxy resin curing agent and preparation method thereof |
| CN108962585A (en) * | 2018-07-19 | 2018-12-07 | 德阳新源电器有限责任公司 | A kind of continuous disk-type winding pouring technology |
| CN109824869A (en) * | 2019-01-31 | 2019-05-31 | 厦门源创力科技服务有限公司 | A kind of epoxy curing agent and preparation method thereof |
| CN110358404A (en) * | 2019-06-21 | 2019-10-22 | 江苏兰陵高分子材料有限公司 | A kind of weather-proof coating of non-solvent epoxy for outdoor weighing apparatus and preparation process |
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| Publication number | Publication date |
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| CN102898624B (en) | 2014-11-05 |
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