CN102898884B - Environment-friendly cashew amine epoxy curing agent for low volatile organic compound (VOC) anticorrosive coating and preparation method for curing agent - Google Patents
Environment-friendly cashew amine epoxy curing agent for low volatile organic compound (VOC) anticorrosive coating and preparation method for curing agent Download PDFInfo
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Abstract
The invention discloses an environment-friendly cashew amine epoxy curing agent for a low volatile organic compound (VOC) anticorrosive coating and a preparation method for the curing agent. The curing agent is prepared from the following raw materials in parts by weight: 1.5 to 2.5 parts of cardanol, 1 to 1.5 parts of diethylenetriamine, and 1.5 to 2 parts of 37 percent formaldehyde aqueous solution. The raw material composition and the optimal proportion of the raw materials are selected through a large quantity of experiments, so that the proportion of each component is scientific and reasonable. The curing agent synthesized by adopting excessive amine and a low-temperature reaction method is high in activity, low in viscosity, good in mixing property, light in color, oil-free, convenient in construction, environment-friendly and solvent-free, can meet various requirements of low VOC anticorrosion, and can overcome many defects of the cashew amine epoxy curing agent prepared by the method in the prior art.
Description
Technical field
The present invention relates to a kind of epoxy hardener, be specifically related to the low VOC protective system cashew nut amine epoxy curing agent of a kind of environment-friendly type.
Background technology
Environment friendly anti-corrosive paint cashew nut amine epoxy curing agent, as solvent-free terrace coating, pipeline and reservoir walls coating etc., often need to meet solvent-free and low viscosity requirement, but cashew nut amine epoxy curing agent prepared by prior art is failed the fine low VOC requirement for anticorrosion that meets, and in prior art, prepare cashew nut amine epoxy curing agent, the substrate that does bridge of often selecting has two kinds of the aqueous solution of paraformaldehyde and 37% formaldehyde.Cook cashew nut amine epoxy curing agent prepared by bridge with paraformaldehyde, application performance is better, but because paraformaldehyde is solid, after dissolving, local reaction is too fast, causes product viscosity larger, relative molecular weight wider distribution, because system need be preheating to 60oC left and right, cause product colour darker simultaneously.But cook cashew nut amine epoxy curing agent prepared by bridge with the aqueous solution of 37% formaldehyde, often have easily fuel-displaced and this difficult problem of bubbling.Therefore, how on the basis of prior art, to prepare high performance, low viscous, high solid, that color is more shallow, not fuel-displaced cashew nut amine epoxy curing agent significant.
Summary of the invention
Goal of the invention: technical problem to be solved by this invention is to overcome the deficiencies in the prior art, provide a kind of component proportioning scientific and reasonable, have wide range of applications, there is high-performance, low viscosity, high solid, the low VOC protective system cashew nut amine epoxy curing agent of color environment-friendly type more shallow and not fuel-displaced advantage.Another object of the present invention is to provide the preparation method of the low VOC protective system of a kind of environment-friendly type cashew nut amine epoxy curing agent.
Technical scheme: for solving above technical problem, the present invention takes following technical scheme:
The low VOC protective system cashew nut amine epoxy curing agent of a kind of environment-friendly type, it is made up of the raw material of following parts by weight: 1.5 ~ 2 parts of the aqueous solution of 1.5 ~ 2.5 parts of cardanols, 1 ~ 1.5 part of diethylenetriamine, 37% formaldehyde.
As preferred version, the low VOC protective system cashew nut amine epoxy curing agent of above-described environment-friendly type, it is made up of the raw material of following parts by weight: 1.5 ~ 2 parts of the aqueous solution of 1.5 ~ 2.5 parts of cardanols, 1 part of diethylenetriamine, 37% formaldehyde.
The preparation method of cashew nut amine epoxy curing agent for the low VOC protective system of environment-friendly type of the present invention, it comprises the following steps:
(1) air of first finding time in reactor, then in reactor, pass into nitrogen to pressure-fired, then by ratio of weight and the number of copies successively toward the cardanol and the diethylenetriamine that drop into parts by weight described in claim 1 or 2 in reactor, and open water coolant, the temperature of reaction in maintenance reactor is below 60oC;
(2) after stirring, toward the aqueous solution that drips by weight 37% formaldehyde in reactor, rate of addition homogeneous, and control temperature of reaction system below 70oC, the time for adding of the aqueous solution of 37% formaldehyde is controlled at 2 to 3 hours;
(3) then reactor is carried out to steam heating, make reactor temperature remain on 70oC left and right, and be incubated 2 to 3 hours;
(4) then between 70oC to 80oC, reactor is vacuumized to dehydration 2 to 3 hours, blowing is both after dehydration completely.
As preferred version, the preparation method of cashew nut amine epoxy curing agent for the low VOC protective system of above-described environment-friendly type, the temperature of reaction in step (1) reactor is controlled at 50 to 60oC.
As preferred version, the preparation method of cashew nut amine epoxy curing agent for the low VOC protective system of above-described environment-friendly type, wherein in step (2) reactor, temperature of reaction system is controlled at 60 to 70oC.
Beneficial effect: the low VOC protective system of environment-friendly type provided by the invention with cashew nut amine epoxy curing agent compared to the prior art tool have the following advantages:
1, the low VOC protective system cashew nut amine epoxy curing agent of environment-friendly type provided by the invention, optimizes the best proportioning of raw material composition and each raw material by great many of experiments, each component proportion is scientific and reasonable.The present invention adopts the pre-excessive and low-temp reaction method of amine, and the solidifying agent activity that synthesizes is high, viscosity is low, compatibility good, lighter color and not fuel-displaced, easy construction, and environment-friendly solvent-free, can meet low VOC rot-resistant requirements.Can overcome many deficiencies of the cashew nut amine epoxy curing agent that art methods prepares.
2, the cured article that adopts cashew nut amine epoxy curing agent cured epoxy resin provided by the invention to obtain, have that gloss is high, good toughness, intensity and hardness balance good, and there is excellent sticking power and the wetting capacity to ground, excellent low surface construction performance, can be widely used in low VOC protective system as fields such as solvent-free terrace coating, pipeline and reservoir walls coating.
Brief description of the drawings
Fig. 1 is the reacting flow chart of the low VOC protective system of environment-friendly type provided by the invention cashew nut amine epoxy curing agent.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the amendment of the various equivalent form of values of the present invention.
Embodiment 1
The low VOC protective system cashew nut amine epoxy curing agent of a kind of environment-friendly type, it is made up of the raw material of following parts by weight: 2 parts of the aqueous solution of 2.5 parts of cardanols, 1.5 parts of diethylenetriamines, 37% formaldehyde.
Embodiment 2
The low VOC protective system cashew nut amine epoxy curing agent of a kind of environment-friendly type, it is made up of the raw material of following parts by weight: 1.5 parts of the aqueous solution of 1.5 parts of cardanols, 1 part of diethylenetriamine, 37% formaldehyde.
Embodiment 3
The low VOC protective system cashew nut amine epoxy curing agent of a kind of environment-friendly type, it is made up of the raw material of following parts by weight:
It is made up of the raw material of following parts by weight: 2 parts of the aqueous solution of 2 parts of cardanols, 1 part of diethylenetriamine, 37% formaldehyde.
Embodiment 4
The preparation method of cashew nut amine epoxy curing agent for the low VOC protective system of environment-friendly type:
Reaction process is as shown in Figure 1:
In a 1000mL four-hole bottle, import nitrogen tube; carry out nitrogen purging; then drop into successively 300g cardanol and 155g diethylenetriamine; then proceed nitrogen purging in reaction system bottom; after purging; under mechanical stirring and nitrogen protection; slowly drip the aqueous solution 250g of 37% formaldehyde; time for adding is controlled at 2 hours, controls temperature of reaction system below 70oC, and 70oC left and right insulation 2 hours; vacuumize dehydration; vacuumize top temperature and be no more than 80oC, blowing after dehydration completely, obtains target product cashew nut amine epoxy curing agent.
Performance test results: cashew nut amine epoxy curing agent is bright, color and luster: No. 12 looks (iron cobalt method), amine value: 315 mg KOH/g, viscosity: 2700 cPs(25oC), admittedly contain: >99%; Slide carriage surface drying: 2.5 hours, do solid work: 8 o'clock, surfacing light, anti-impact force is crossed 50 cm, 1 grade of snappiness, adhesion 1 grade, hardness 3H, varnish gloss: 150.
Embodiment 5
The preparation method of cashew nut amine epoxy curing agent for the low VOC protective system of environment-friendly type:
Reaction process is as shown in Figure 1:
0.5 M finds time
3stainless steel cauldron, and mend nitrogen to pressure-fired, then drop into successively 150 Kg cardanols and 75 Kg diethylenetriamines, open water coolant, after mechanical stirring half an hour, slowly drip the aqueous solution 121 Kg of 37% formaldehyde, time for adding is controlled at 3 hours, temperature of reaction system is controlled at below 70oC, and 70oC left and right insulation 3 hours, vacuumize dehydration, vacuumize top temperature and be no more than 80oC, blowing after dehydration completely, obtains target product cashew nut amine epoxy curing agent.
Performance test results: cashew nut amine epoxy curing agent is bright, color and luster: No. 12 looks (iron cobalt method), amine value: 326 mg KOH/g, viscosity: 3170 cPs(25oC), admittedly contain: >99%; Slide carriage surface drying: 2.5 hours, do solid work: 7 o'clock, surfacing light, anti-impact force is crossed 55 cm, 1 grade of snappiness, adhesion 1 grade, hardness 3H, varnish gloss: 160.
Darker in order to solve in prior art cashew nut amine epoxy curing agent color; viscosity is large, poor adhesive force; easily go out wet goods problem, the present invention adopts the aqueous solution of 37% formaldehyde to do bridge, adopts low-temp reaction method and nitrogen protection to protect product colour, and adopts the pre-overflow method of amine to reduce product viscosity.The cashew nut amine hardener prepared by this technique is of light color, activity is high, viscosity is low, not fuel-displaced, have wide range of applications.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (1)
1. the preparation method of cashew nut amine epoxy curing agent for the low VOC protective system of environment-friendly type, is characterized in that, it is made up of the raw material of following parts by weight: 1.5～2 parts of the aqueous solution of 1.5～2.5 parts of cardanols, 1 part of diethylenetriamine, 37% formaldehyde,
It comprises the following steps:
(1) air of first finding time in reactor then passes into nitrogen to pressure-fired in reactor, then in reactor, drops into 1.5～2.5 parts of cardanols, 1 part of diethylenetriamine successively, and opens water coolant, and the temperature of reaction in maintenance reactor is below 60 DEG C;
(2) after stirring, 1.5～2 parts of the aqueous solution of the interior dropping of past reactor 37% formaldehyde, rate of addition homogeneous, and control temperature of reaction system below 70 DEG C, the time for adding of the aqueous solution of 37% formaldehyde is controlled at 2 to 3 hours;
(3) then reactor is carried out to steam heating, make reactor temperature remain on 70 DEG C, and be incubated 2 to 3 hours;
(4), then between 70 DEG C to 80 DEG C, reactor is vacuumized to dehydration 2 to 3 hours, blowing and get final product after dehydration completely.
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| CN201210362330.6A CN102898884B (en) | 2012-09-26 | 2012-09-26 | Environment-friendly cashew amine epoxy curing agent for low volatile organic compound (VOC) anticorrosive coating and preparation method for curing agent |
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| CN201210362330.6A CN102898884B (en) | 2012-09-26 | 2012-09-26 | Environment-friendly cashew amine epoxy curing agent for low volatile organic compound (VOC) anticorrosive coating and preparation method for curing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105601887A (en) * | 2015-12-31 | 2016-05-25 | 上海美东生物材料股份有限公司 | Alicyclic amine curing agent and preparing method thereof |
| CN112898870B (en) * | 2021-01-25 | 2022-05-17 | 江南大学 | Cardanol aldehyde amine low-temperature curing montmorillonite/epoxy anticorrosive paint and preparation method and application thereof |
| CN113651704A (en) * | 2021-08-18 | 2021-11-16 | 四川轻化工大学 | Preparation method and application of novel modified amine epoxy curing agent |
| CN114163615A (en) * | 2021-11-25 | 2022-03-11 | 江苏三木化工股份有限公司 | Flexible epoxy curing agent for encapsulating material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374292A (en) * | 2002-04-05 | 2002-10-16 | 中国科学院长春应用化学研究所 | Synthesis of anacardian amine as epoxy resin curing agent |
| CN101333286A (en) * | 2007-06-26 | 2008-12-31 | 上海经天新材料科技有限公司 | Amine epoxy curing agent modified by cardanol |
| CN101508856A (en) * | 2008-02-13 | 2009-08-19 | 上海涂料有限公司上海长风化工厂 | Cashew pnenolic aldehyde amine epoxide resin paint solidifying agent and method for producing the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374292A (en) * | 2002-04-05 | 2002-10-16 | 中国科学院长春应用化学研究所 | Synthesis of anacardian amine as epoxy resin curing agent |
| CN101333286A (en) * | 2007-06-26 | 2008-12-31 | 上海经天新材料科技有限公司 | Amine epoxy curing agent modified by cardanol |
| CN101508856A (en) * | 2008-02-13 | 2009-08-19 | 上海涂料有限公司上海长风化工厂 | Cashew pnenolic aldehyde amine epoxide resin paint solidifying agent and method for producing the same |
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Denomination of invention: Environment-friendly cashew amine epoxy curing agent for low volatile organic compound (VOC) anticorrosive coating and preparation method for curing agent Effective date of registration: 20160719 Granted publication date: 20140709 Pledgee: Fenghui Leasing Co. Ltd. Pledgor: Jiangsu Sanmu Group Co., Ltd. Registration number: 2016990000611 |
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Date of cancellation: 20190923 Granted publication date: 20140709 Pledgee: Fenghui Leasing Co. Ltd. Pledgor: Jiangsu Sanmu Group Co., Ltd. Registration number: 2016990000611 |