CN102633987A - Liquid dicyandiamide latent type epoxy resin curing agent and preparation method thereof - Google Patents
Liquid dicyandiamide latent type epoxy resin curing agent and preparation method thereof Download PDFInfo
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- CN102633987A CN102633987A CN2012101262498A CN201210126249A CN102633987A CN 102633987 A CN102633987 A CN 102633987A CN 2012101262498 A CN2012101262498 A CN 2012101262498A CN 201210126249 A CN201210126249 A CN 201210126249A CN 102633987 A CN102633987 A CN 102633987A
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Abstract
The invention provides a liquid dicyandiamide latent type epoxy resin curing agent and a preparation method thereof and relates to the epoxy resin curing agent. The invention provides the liquid dicyandiamide latent type epoxy resin curing agent which can improve the solubility of dicyandiamide and epoxy resin which are liquefied, and the preparation method thereof. The liquid dicyandiamide latent type epoxy resin curing agent is composed of the following components by mass percentage: 100 of dicyandiamide, 120-300 of epoxy resin diluting agent, 0.5-1.0 of accelerating agent and 100-200 of solvent. The preparation method comprises the following steps of: adding the dicyandiamide into a container and then adding the solvent; adding an agitator and a condensing pipe; placing the container into an electric jacket to be heated; and after the dicyandiamide is dissolved, adding the epoxy resin diluting agent and the accelerating agent to react to obtain the liquid dicyandiamide latent type epoxy resin curing agent.
Description
Technical field
The present invention relates to a kind of epoxy curing agent, especially relate to a kind of liquid Dyhard RU 100 incubated epoxide curing agent and preparation method thereof.
Background technology
Epoxy resin is widely used in various fields as one of important matrix resin of coating, electrical apparatus insulation material, industrial adhesive and matrix material.When epoxy resin uses, must add solidifying agent, and be cured reaction under certain condition, generate the product of tridimensional network, just can show various good performances, become epoxy material with real practical value.Therefore, solidifying agent has conclusive effect in the application of epoxy resin.
Epoxy curing agent is divided into and shows at type solidifying agent and latent curing agent.Show at type solidifying agent and epoxy resin and form bicomponent system, promptly solidifying agent and epoxy resin are packed respectively, during construction two kinds of component proportional mixing are used; Latent curing agent and epoxy resin are formed single-component system, at room temperature have certain stability in storage, and under conditions such as heating, illumination, moisture, pressurization, can be cured reaction rapidly.Compare with the bi-component epoxide-resin system, the one-component epoxy resin system that is formed by latent curing agent and epoxy resin mixed preparing has the production operation of simplification technology, prevent the pollution of the environment, improve the quality of products, adapt to advantage such as modern large-scale industrial production.Therefore, latent curing agent is the emphasis of epoxy curing agent research and development both at home and abroad in recent years.
Dyhard RU 100 is a kind of incubated epoxide curing agent commonly used, and the shelf lives that reaches more than 6 months is at room temperature arranged, but it in use exist the solidification value height, shortcoming such as solubleness is little in epoxy resin, thereby limited its application.Under the prerequisite that satisfies Dyhard RU 100/epoxy-resin systems good shelf-stability, the temperature of reaction of Dyhard RU 100 cured epoxy resin is reduced to mesophilic range, and don't influences its use properties; And make solid-state Dyhard RU 100 liquid phaseization, avoid the not homogeneous phase of single-component epoxy glue; It is the focus of present incubated epoxide curing agent research.The method of reduction Dyhard RU 100 solidification value commonly used has two kinds: 1, add promotor to reduce its solidification value; 2, through molecular designing Dyhard RU 100 is carried out chemical modification, to improve the activity of its curing reaction.People such as Jiao Jian (Jiao J.; Lan L. W.; Polymer Materials Science and Engineering; 2000,16 (6): 115-117) reduce the temperature of reaction of Dyhard RU 100 cured epoxy resin as promotor, but also influenced the shelf lives of Dyhard RU 100/epoxy resin solidifying system with methylacrylic acid passivation 2-ethyl-4 Methylimidazole; Adopt aromatic diamine and Dyhard RU 100 reaction to make its verivate among the Japanese Patent JP49093498A, but products therefrom is a pressed powder, is difficult for homodisperse in epoxy resin.Adopt the ester modified Dyhard RU 100 of neodecanoic acid Racemic glycidol among the Chinese patent CN1194025C, but the reaction times is longer, cost is also than higher.
Though it is more that the research Dyhard RU 100 is done the report of epoxy curing agent, do not see that systematic study epoxy resin diluent modification Dyhard RU 100 prepares the report of liquid incubated epoxide curing agent.
Summary of the invention
The present invention aims to provide liquid Dyhard RU 100 incubated epoxide curing agent of a kind of intermiscibility that improves Dyhard RU 100 and epoxy resin after the liquefaction and preparation method thereof.
Said liquid Dyhard RU 100 incubated epoxide curing agent consisting of by mass ratio:
Dyhard RU 100 100, epoxy resin diluent 120～300, promotor 0.5～1.0, solvent 100～200.
Said liquid Dyhard RU 100 incubated epoxide curing agent is preferably by the composition of mass ratio:
Dyhard RU 100 100, epoxy resin diluent 130～180, promotor 0.6～0.8, solvent 130～150.
The preparation method of said liquid Dyhard RU 100 incubated epoxide curing agent is following:
In container, add Dyhard RU 100, add solvent again, load onto whisking appliance and prolong, place electric mantle to heat in container again, treat Dyhard RU 100 dissolving after, add epoxy resin diluent and booster response after, promptly get liquid Dyhard RU 100 incubated epoxide curing agent.
Said container is preferably the three-necked bottle that has electronic stirring, TM and reflux condensing tube; Said epoxy resin diluent can be selected from a kind of in n-butyl glycidyl ether, phenyl glycidyl ether, the tertiary carbonic acid glycidyl ester etc.; Said promotor can be selected from a kind of in 2-ethyl-4-methylimidazole, the glyoxal ethyline etc.; Said solvent can be selected from a kind of in ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, the propylene glycol monomethyl ether etc.; The temperature of said reaction can be 120～160 ℃, and the time of reaction can be 4～6h.
The liquid Dyhard RU 100 incubated epoxide curing agent that makes and epoxy resin are packed in the glass mortar; After grinding evenly; Dip in glass stick and to get a little solidifying agent/epoxy resin composition and be applied on the slide glass; Again slide glass is put into vacuum drying oven and be heating and curing, the performance of test cured article behind the completion of cure.
It is the epoxy resin of E-51 that said epoxy resin can adopt the trade mark; The mass ratio of said liquid Dyhard RU 100 incubated epoxide curing agent and epoxy resin can be (15～30): 100; Said solidification value can be 140～160 ℃; The said curing reaction time can be 0.5～1h.
The present invention adopts epoxy resin diluent and Dyhard RU 100 reaction, makes liquid Dyhard RU 100 incubated epoxide curing agent, and its cured epoxy resin has good mechanical property, and has following outstanding feature:
1. liquid Dyhard RU 100 incubated epoxide curing agent is the liquid of toughness, and is good with the intermiscibility of epoxy resin, helps mixing with epoxy resin, and can not produce deposition;
2. the product reactive behavior is high, under middle temperature can with epoxy resin generation curing reaction, smell is little, nontoxicity, stability in storage is good;
3. synthesis technique is simple, and is easy to operate, is easy to realize large-scale industrial production.
Embodiment
Embodiment 1
1) takes by weighing the 8.41g Dyhard RU 100 in three-necked bottle, add the 10ml ethylene glycol monomethyl ether then, load onto whisking appliance and prolong; Place electric mantle to heat three-necked bottle again; Temperature is 140 ℃, treats to add the 16.94g n-butyl glycidyl ether after the Dyhard RU 100 dissolving fully; Stopped reaction after the reaction 4h obtains brown toughness transparent liquid.
2) taking by weighing liquid Dyhard RU 100 incubated epoxide curing agent of 0.48g and 3.0g epoxy resin E-51 respectively packs in the glass mortar; After grinding evenly; Dip in glass stick and to get a little solidifying agent/epoxy resin composition and be applied on the slide glass; Again slide glass is put into 150 ℃ of 0.5h that are heating and curing of vacuum drying oven, the performance of test cured article behind the completion of cure.
The performance of liquid Dyhard RU 100 incubated epoxide curing agent is referring to table 1, and the performance of liquid Dyhard RU 100 incubated epoxide curing agent and epoxy resin cured product is referring to table 2.
Table 1
Table 2
| Embodiment | Shearing resistance/MPa | Tensile strength/MPa | Tensile modulus/GPa |
| 1 | 18.6 | 119.8 | 2.28 |
| 2 | 24.5 | 114.2 | 2.68 |
| 3 | 27.8 | 110.5 | 2.79 |
| 4 | 22.3 | 116.4 | 2.59 |
| 5 | 20.2 | 118.2 | 2.41 |
Embodiment 2
1) takes by weighing the 8.41g Dyhard RU 100 in three-necked bottle, add the 10ml ethylene glycol monomethyl ether then, load onto whisking appliance and prolong; Place electric mantle to heat three-necked bottle again; Temperature is 130 ℃, treats to add the 19.54g n-butyl glycidyl ether after the Dyhard RU 100 dissolving fully; Stopped reaction after the reaction 4h obtains brown toughness transparent liquid.
2) taking by weighing liquid Dyhard RU 100 incubated epoxide curing agent of 0.35g and 2.28g epoxy resin E-51 respectively packs in the glass mortar; After grinding evenly; Dip in glass stick and to get a little solidifying agent/epoxy resin composition and be applied on the slide glass; Again slide glass is put into 150 ℃ of 0.5h that are heating and curing of vacuum drying oven, the performance of test cured article behind the completion of cure.
The performance of liquid Dyhard RU 100 incubated epoxide curing agent is referring to table 1, and the performance of liquid Dyhard RU 100 incubated epoxide curing agent and epoxy resin cured product is referring to table 2.
Embodiment 3
1) takes by weighing the 8.41g Dyhard RU 100 in three-necked bottle, add the 15ml ethylene glycol monomethyl ether then, load onto whisking appliance and prolong; Place electric mantle to heat three-necked bottle again; Temperature is 140 ℃, treats to add the 15.02g phenyl glycidyl ether after the Dyhard RU 100 dissolving fully; Stopped reaction after the reaction 4h obtains brown toughness transparent liquid.
2) taking by weighing liquid Dyhard RU 100 incubated epoxide curing agent of 0.58g and 1.94g epoxy resin E-51 respectively packs in the glass mortar; After grinding evenly; Dip in glass stick and to get a little solidifying agent/epoxy resin composition and be applied on the slide glass; Again slide glass is put into 150 ℃ of 0.5h that are heating and curing of vacuum drying oven, the performance of test cured article behind the completion of cure.
The performance of liquid Dyhard RU 100 incubated epoxide curing agent is referring to table 1, and the performance of liquid Dyhard RU 100 incubated epoxide curing agent and epoxy resin cured product is referring to table 2.
Embodiment 4
1) takes by weighing the 10.93g Dyhard RU 100 in three-necked bottle, add the 15ml ethylene glycol monomethyl ether then, load onto whisking appliance and prolong; Place electric mantle to heat three-necked bottle again; Temperature is 140 ℃, treats to add 15.02g phenyl glycidyl ether and 0.059g2-ethyl-4-methylimidazole after the Dyhard RU 100 dissolving fully; Stopped reaction after the reaction 6h obtains brown toughness transparent liquid.
2) taking by weighing liquid Dyhard RU 100 incubated epoxide curing agent of 0.64g and 2.15g epoxy resin E-51 respectively packs in the glass mortar; After grinding evenly; Dip in glass stick and to get a little solidifying agent/epoxy resin composition and be applied on the slide glass; Again slide glass is put into 150 ℃ of 0.5h that are heating and curing of vacuum drying oven, the performance of test cured article behind the completion of cure.
The performance of liquid Dyhard RU 100 incubated epoxide curing agent is referring to table 1, and the performance of liquid Dyhard RU 100 incubated epoxide curing agent and epoxy resin cured product is referring to table 2.
Embodiment 5
1) takes by weighing the 11.78g Dyhard RU 100 in three-necked bottle, add the 15ml ethylene glycol monomethyl ether then, load onto whisking appliance and prolong; Place electric mantle to heat three-necked bottle again; Temperature is 140 ℃, treats to add 15.02g phenyl glycidyl ether and 0.11g2-ethyl-4-methylimidazole after the Dyhard RU 100 dissolving fully; Stopped reaction after the reaction 6h obtains brown toughness transparent liquid.
2) taking by weighing liquid Dyhard RU 100 incubated epoxide curing agent of 0.53g and 2.15g epoxy resin E-51 respectively packs in the glass mortar; After grinding evenly; Dip in glass stick and to get a little solidifying agent/epoxy resin composition and be applied on the slide glass; Again slide glass is put into 150 ℃ of 0.5h that are heating and curing of vacuum drying oven, the performance of test cured article behind the completion of cure.
The performance of liquid Dyhard RU 100 incubated epoxide curing agent is referring to table 1, and the performance of liquid Dyhard RU 100 incubated epoxide curing agent and epoxy resin cured product is referring to table 2.
Claims (8)
1. liquid Dyhard RU 100 incubated epoxide curing agent is characterized in that consisting of by mass ratio:
Dyhard RU 100 100, epoxy resin diluent 120～300, promotor 0.5～1.0, solvent 100～200.
2. a kind of liquid Dyhard RU 100 incubated epoxide curing agent as claimed in claim 1 is characterized in that consisting of by mass ratio:
Dyhard RU 100 100, epoxy resin diluent 130～180, promotor 0.6～0.8, solvent 130～150.
3. the preparation method of a kind of liquid Dyhard RU 100 incubated epoxide curing agent as claimed in claim 1 is characterized in that its concrete steps are following:
In container, add Dyhard RU 100, add solvent again, load onto whisking appliance and prolong, place electric mantle to heat in container again, treat Dyhard RU 100 dissolving after, add epoxy resin diluent and booster response after, promptly get liquid Dyhard RU 100 incubated epoxide curing agent.
4. the preparation method of a kind of liquid Dyhard RU 100 incubated epoxide curing agent as claimed in claim 3 is characterized in that said container is the three-necked bottle that has electronic stirring, TM and reflux condensing tube.
5. the preparation method of a kind of liquid Dyhard RU 100 incubated epoxide curing agent as claimed in claim 3 is characterized in that said epoxy resin diluent is selected from a kind of in n-butyl glycidyl ether, phenyl glycidyl ether, the tertiary carbonic acid glycidyl ester.
6. the preparation method of a kind of liquid Dyhard RU 100 incubated epoxide curing agent as claimed in claim 3 is characterized in that said promotor is selected from a kind of in 2-ethyl-4-methylimidazole, the glyoxal ethyline.
7. the preparation method of a kind of liquid Dyhard RU 100 incubated epoxide curing agent as claimed in claim 3 is characterized in that said solvent is selected from a kind of in ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, the propylene glycol monomethyl ether.
8. the preparation method of a kind of liquid Dyhard RU 100 incubated epoxide curing agent as claimed in claim 3, the temperature that it is characterized in that said reaction is 120～160 ℃, the time of reaction is 4～6h.
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| CN2012101262498A CN102633987A (en) | 2012-04-26 | 2012-04-26 | Liquid dicyandiamide latent type epoxy resin curing agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116120849A (en) * | 2022-12-29 | 2023-05-16 | 江苏新扬新材料股份有限公司 | Low-cost light lightning protection surface film for composite material structure and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1485356A (en) * | 2002-09-28 | 2004-03-31 | 北京科化新材料科技有限公司 | Liquefied dicyandiamide and its preparing process |
| CN101784579A (en) * | 2008-03-07 | 2010-07-21 | 欧姆龙株式会社 | One-pack type epoxy resin composition and use thereof |
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- 2012-04-26 CN CN2012101262498A patent/CN102633987A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1485356A (en) * | 2002-09-28 | 2004-03-31 | 北京科化新材料科技有限公司 | Liquefied dicyandiamide and its preparing process |
| CN101784579A (en) * | 2008-03-07 | 2010-07-21 | 欧姆龙株式会社 | One-pack type epoxy resin composition and use thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116120849A (en) * | 2022-12-29 | 2023-05-16 | 江苏新扬新材料股份有限公司 | Low-cost light lightning protection surface film for composite material structure and application thereof |
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Application publication date: 20120815 |