CN102898624B - Epoxy resin curing agent and preparation method thereof - Google Patents
Epoxy resin curing agent and preparation method thereof Download PDFInfo
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- CN102898624B CN102898624B CN201210422258.1A CN201210422258A CN102898624B CN 102898624 B CN102898624 B CN 102898624B CN 201210422258 A CN201210422258 A CN 201210422258A CN 102898624 B CN102898624 B CN 102898624B
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- curing agent
- epoxy resin
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- phenylcarbinol
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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 epoxy curing agent field, specifically, relate to epoxy curing agent that a kind of hardness high-weatherability is good and preparation method thereof.
Background technology:
Epoxy resin 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 epoxy resin producing country in the whole world at present, and output is the world 37.1%.But epoxy resin is a kind of amorphous thick liquid, heating is plasticity, there is no obvious fusing point, the deliquescing of being heated is melted and stickness gradually, water insoluble, itself can not harden, and therefore it does not almost have independent use value, only has with the cancellated not cladding polymer of solidifying agent reaction generating three-dimensional and just has using value.Just solidify to form gradually the different chemical substance of performance when adding after a certain amount of solidifying agent, therefore, must add solidifying agent, compositing formula resin, and be cured reaction under certain condition, the macromolecular material that generates tridimensional network, just can show various good performances, becomes the epoxy material with real use value.
Conventional epoxy curing agent is divided into alkaline species solidifying agent and acid class solidifying agent, and alkaline species solidifying agent mainly comprises aliphatie diamine and polyamines, aliphatic cyclic amine, aromatic polyamine compound and modified polyether amine, aromatics is better as solidifying agent hardness of film, but the weathering resistance of film is not good enough, aliphatic polyamine weathering resistance is better, but the easy moisture absorption and make 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 using now easily volatilizees as diethylenetriamine, triethylene tetramine compound, and smell is larger, and environment is caused to larger harm; The aromatic amine solidifying agent such as mphenylenediamine and epoxy host film-forming weathering resistance are poor, and xanthochromia easily occurs, and 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 more soft, and epoxy resin film is not wear-resisting yet, and therefore duration of service can be not longer, and duration of service, longer appearance effect was 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 are provided the object of the invention, after this epoxy curing agent mixes with epoxy resin host, Self-leveling is respond well, filmogen good weatherability, and hardness is high, 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 is 12 hours.
For achieving the above object, technical scheme disclosed by the invention is: a kind of epoxy curing agent, and the each component of described epoxy curing agent by mass percent is: phenylcarbinol-40%-50%, isophorone diamine 30%-45%, epoxy resin 10%-20%, scratch resistance wax 0.1%-1%, promotor 1%-5%.
What preferably, described promotor adopted is Schiff's base.In concrete 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-tri-(dimethylamino methyl) phenol.In concrete production, can also add according to the condition of production Schiff's base of other types.
Preferably, described epoxy resin adopts E-51 epoxy resin or E-44 epoxy resin.In concrete production, can also be according to the epoxy resin of other kinds of practical situation choice for use, as: E-54 epoxy resin, E-20 epoxy resin.
A kind of preparation method of epoxy curing agent, operate as follows: in reactor, add appropriate phenylcarbinol, isophorone diamine, after both are stirred, in reactor, add epoxy resin, be steam heated to while stirring after reacting liquid temperature reaches 60-75 DEG C and continue stirring reaction 2 hours, then in reactor, add scratch resistance wax and promotor, be uniformly dispersed, cooling rear packing.For ensureing quality product, the reacting liquid temperature of steam heating control is while stirring at 60-75 DEG C.
Further, because epoxy curing agent of the present invention is in the time mixing use with epoxy resin, can affect because of the difference of construction environment temperature both speed of response, therefore for better making solidifying agent of the present invention and epoxy resin be used in conjunction with, in preparation process, in the time that the construction environment temperature of solidifying agent is spent higher than 20, the mass percent of the component promotor of adding in preparation manipulation is 1%-3%; In the time that the construction environment temperature of solidifying agent is spent lower than 20, the mass percent of the component promotor of adding in preparation manipulation is 3%-5%.
The effect of the promotor of adding in the present invention is: the speed of accelerating resin film forming; The effect of scratch resistance wax is: the adhesion strength that strengthens paint film.
In the present invention, utilize isophorone diamine and epoxy resin to heat in phenylcarbinol, make isophorone diamine modification obtain epoxide modified isophorone diamine by reaction between the two, strengthen the consistency of solidifying agent and epoxy resin, and realize solvent free in operation, product Self-leveling is effective.
The invention has the beneficial effects as follows: the epoxy curing agent in the present invention mixes use with epoxy coating host, weathering resistance that can reinforced epoxy coating, the anti-accelerated deterioration performance of coating is improved more than 10%, scratch resistance wax in epoxy curing agent also can reinforced epoxy paint coatings hardness, the shore hardness of epoxy coating coating is reached more than 85.Epoxy curing agent of the present invention makes the paint solidification time suitable after coordinating epoxy coating host to use, and meets 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 to more explicit defining.
Embodiment mono-: a kind of epoxy curing agent, its component by mass percent is: phenylcarbinol 40%, isophorone diamine 45%, epoxy resin 13%, scratch resistance wax 1%, promotor 1%.
The preparation method of this epoxy curing agent is as follows: in reactor, add phenylcarbinol, isophorone diamine, after both are stirred, in reactor, add epoxy resin, steam heating while stirring, when reacting liquid temperature reaches after 60 DEG C, continues stirring reaction 2 hours, then in reactor, add scratch resistance wax and promotor, after being uniformly dispersed, naturally cooling, obtains product epoxy curing agent.What in the present embodiment, epoxy resin adopted is E-51 epoxy resin, and what promotor adopted is Schiff's base promotor.
This epoxy curing agent and epoxy self-leveling coating host are that after mixing under the temperature condition of 25 degree and using, the shore hardness of epoxy coating paint film is 83 in construction environment, and surface drying time is 2 hours, and the time of doing solid work is 12 hours.
Embodiment bis-: 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, to the E-20 epoxy resin that adds 15 Kg in reactor, steam heating while stirring, when reacting liquid temperature reaches after 65 DEG C, continue stirring reaction 2 hours, then in reactor, add 0.3Kg scratch resistance wax and 4.7Kg promotor Schiff's base and be uniformly dispersed.After naturally cooling, obtain product epoxy curing agent 100Kg.This epoxy curing agent mixes with epoxy self-leveling coating host after use, and 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 tri-: a kind of epoxy curing agent, its component by mass percent is: phenylcarbinol 45%, isophorone diamine 30%, E-51 epoxy resin 20 %, 0.4% scratch resistance wax, promotor Schiff's base 4.6%.
The preparation method of this epoxy curing agent is as follows: in reactor, add 45Kg phenylcarbinol, 30Kg isophorone diamine, after both are stirred, to the E-51 epoxy resin that adds 20 Kg in reactor, steam heating while stirring, in reaction process, isophorone diamine reacts and makes isophorone diamine modification with E-51 epoxy resin.When reacting liquid temperature reaches after 70 DEG C, continue stirring reaction 2 hours, then in reactor, add 0.4Kg scratch resistance wax and 4.6Kg promotor Schiff's base, be uniformly dispersed, after naturally cooling, obtain product epoxy curing agent 100Kg.
This epoxy curing agent mixes with epoxy self-leveling coating host after use, and 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 tetra-: a kind of epoxy curing agent, its each component by mass percent is: phenylcarbinol 40%, isophorone diamine 45%, epoxy resin 10%, scratch resistance wax 0.8%, promotor 4.2%.Its preparation method is with the preparation method in embodiment mono-.
The epoxy resin adopting in embodiment is E-54 epoxy resin, and what promotor adopted is 2,4,6-tri-(dimethylamino methyl) phenol.This epoxy curing agent mixes with epoxy self-leveling coating host and uses after construction environment is to mix under the temperature condition of 16 DEG C and use, and 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 five: utilize preparation method of the present invention to prepare epoxy curing agent, in reactor, add phenylcarbinol 40%, isophorone diamine 40% by mass percent, after both are stirred, in reactor, add E-54 epoxy resin 14%, steam heating while stirring, when reacting liquid temperature reaches after 60 DEG C, continue stirring reaction 2 hours, then in reactor, add scratch resistance wax 1% and promotor Schiff's base 5%, be uniformly dispersed, after naturally cooling, obtain product epoxy curing agent.
This epoxy curing agent and epoxy self-leveling coating host are that after mixing under the temperature condition of 10 DEG C and using, the shore hardness of epoxy coating paint film is 87 in construction environment, and surface drying time is 3 hours, and 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, in reactor, add 17KgE-44 epoxy resin, steam heating while stirring, when reacting liquid temperature reaches after 75 DEG C, continue stirring reaction 2 hours, then in reactor, add 0.5Kg scratch resistance wax and 2.5Kg promotor Schiff's base and be uniformly dispersed, after naturally cooling, obtaining product epoxy curing agent 100Kg.In reaction process, isophorone diamine reacts and makes isophorone diamine modification with E-44 epoxy resin.
This epoxy curing agent mixes with epoxy self-leveling coating host after use, and 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 epoxy resin 10%, scratch resistance wax 1%, promotor 3%.Its preparation method is with the preparation method in embodiment mono-.
This epoxy curing agent mixes with epoxy self-leveling coating host and uses after construction environment is to mix under the temperature condition of 16 DEG C and use, and the shore hardness of epoxy coating paint film is 87, and surface drying time is 3 hours, and 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 epoxy resin 10%, scratch resistance wax 1%, promotor 2%.Its preparation method is with the preparation method in embodiment mono-, and what wherein promotor adopted is 2,4,6-tri-(dimethylamino methyl) phenol.
This epoxy curing agent mixes with epoxy self-leveling coating host and uses after construction environment is to mix under the temperature condition of 22 DEG C and use, and the shore hardness of epoxy coating paint film is 88, and surface drying time is 2 hours, and the time of doing solid work is 11 hours.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; 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 (8)
1. an epoxy curing agent, is characterized in that, the each component of described epoxy curing agent by mass percent is: phenylcarbinol 40%--50%, isophorone diamine 30%--45%, epoxy resin 10%--20%, scratch resistance wax 0.1%--1%, promotor 1%--5%; What described promotor adopted is Schiff's base.
2. according to a kind of epoxy curing agent described in claim 1, it is characterized in that, what described Schiff's base adopted is 2,4,6-tri-(dimethylamino methyl) phenol.
3. according to a kind of epoxy curing agent described in claim 1, it is characterized in that, described epoxy resin adopts E-51 epoxy resin or E-44 epoxy resin.
4. according to a kind of epoxy curing agent described in claim 1 or 2 or 3, it is characterized in that, the each component of described epoxy curing agent by mass percent is: phenylcarbinol 40%, isophorone diamine 45%, epoxy resin 13%, scratch resistance wax 1%, promotor 1%.
5. according to a kind of epoxy curing agent described in claim 1 or 2 or 3, it is characterized in that, the each component of described epoxy curing agent by mass percent is: phenylcarbinol 40%, isophorone diamine 45%, epoxy resin 10%, scratch resistance wax 0.8%, promotor 4.2%.
6. a kind of epoxy curing agent according to claim 3, is characterized in that, the each component of described epoxy curing agent by mass percent is: phenylcarbinol 41%, isophorone diamine 45%, E-51 epoxy resin 10%, scratch resistance wax 1%, promotor 3%.
7. a kind of epoxy curing agent according to claim 3, is characterized in that, the each component of described epoxy curing agent by mass percent is: phenylcarbinol 42%, isophorone diamine 45%, E-44 epoxy resin 10%, scratch resistance wax 1%, promotor 2%.
8. the preparation method of an epoxy curing agent, operate as follows: in reactor, add appropriate phenylcarbinol, isophorone diamine, after both are stirred, in reactor, add epoxy resin, be steam heated to while stirring after reacting liquid temperature reaches 60-75 DEG C and continue stirring reaction 2 hours, then in reactor, add scratch resistance wax and promotor, be uniformly dispersed, cooling rear packing.
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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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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN110358404B (en) * | 2019-06-21 | 2022-01-28 | 江苏兰陵高分子材料有限公司 | Solvent-free epoxy weather-resistant paint for outdoor weighing apparatus and preparation process thereof |
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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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Effective date of registration: 20170818 Address after: 226200 Binjiang fine chemical industry park, Nantong, Jiangsu, Qidong Patentee after: Qidong dimension Chemical Technology Co., Ltd. Address before: 200100, B, building 7, room 1, building 977, 7020 Feng Feng Road, Shanghai, Pudong New Area Patentee before: Shanghai dimension Chemical Industry Science Co., Ltd |
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Effective date of registration: 20210604 Address after: Room 301, 3 / F, building 1, 151 Daxiu Road, Pudong New Area, Shanghai, 200120 Patentee after: SHANGHAI WEDO CHEMICAL Co.,Ltd. Address before: 226200 Qidong Binjiang fine chemical industry park, Nantong City, Jiangsu Province Patentee before: QIDONG WEIDU CHEMICAL TECHNOLOGY Co.,Ltd. |
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