CN104356362A - Preparation method of modified alicyclic amine curing agent - Google Patents
Preparation method of modified alicyclic amine curing agent Download PDFInfo
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- CN104356362A CN104356362A CN201410673233.8A CN201410673233A CN104356362A CN 104356362 A CN104356362 A CN 104356362A CN 201410673233 A CN201410673233 A CN 201410673233A CN 104356362 A CN104356362 A CN 104356362A
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- thinner
- solidifying agent
- epoxy resin
- curing agent
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Abstract
The invention discloses a preparation method of a modified alicyclic amine curing agent. The preparation method comprises the following steps: pouring epoxy resin into a reaction kettle I, stirring at the rotating speed of 300-800 turns/minute, adding a diluent 1 during stirring and stirring for 20-30 minutes, and heating materials to 80DEG C for later use; adding a curing agent and a diluent 2 into a reaction kettle II, stirring at the rotating speed of 300-800 turns/minute, and heating materials to 80DEG C, then dropwise adding the obtained materials into the reaction kettle II within 1-2 hours, controlling the reaction temperature to 75-85DEG C and further reacting for 1-2 hours after the dropwise addition is completed, finally cooling to room temperature and discharging, thus obtaining the modified alicyclic amine curing agent. The method is simple to operate and easy to popularize on large scale, and the prepared modified alicyclic amine curing agent is low in odor, irritation-free, low in viscosity and convenient to use.
Description
Technical field
The invention belongs to epoxy curing agent preparing technical field, particularly a kind of preparation method of modification aliphatic cyclic amine solidifying agent.
Background technology
Epoxy resin is the important kind of in synthetic resins, owing to having a series of excellent performance, as cohesiveness is strong, shrinking percentage is little, mechanical property, dielectric properties and fine heat-resisting performance, and good chemical stability, the numerous areas such as widespread use and electronics, electrical equipment, machinery, chemical industry, building.
Make epoxy resin have excellent performance, epoxy resin and solidifying agent must be carried out crosslinking reaction and form cancellated macromole.The solidifying agent of epoxy resin is of a great variety, conventional is amine curing agent, aliphatics or alicyclic amine curing agent have very high reactive behavior, can at normal temperature and cured at room temperature epoxy resin, and it is low to have viscosity, the advantages such as chemical resistance is good, but also have a lot of weak point: during (1) solidification, thermal discharge is large, and during construction, the operating time is short.(2) volatile, irritant, the health of people is harmful to.(3) there is moisture absorption, affect ply adhesion.(4) high-polarity, poor with epoxy resin compatibility, easily cause paint film tangerine peel, shrinkage cavity etc.
Summary of the invention
The object of this invention is to provide a kind of preparation method of modification aliphatic cyclic amine solidifying agent, overcome the shortcoming of traditional aliphatic cyclic amine solidifying agent.
Concrete steps are:
(1) raw material is taken by following mass ratio, solidifying agent: epoxy resin: thinner 1: thinner 2=30 ~ 50:10 ~ 20:25 ~ 35:15 ~ 25.
(2) epoxy resin that step (1) takes is poured in reactor I, stir with the rotating speed of 300 ~ 800 revs/min, add the thinner 1 that step (1) takes in whipping process and stir 20 ~ 30 minutes, and heated material to 80 DEG C, stand-by.
(3) thinner 2 that solidifying agent step (1) taken and step (1) take joins in reactor II, stir 30 ~ 50 minutes with the rotating speed of 300 ~ 800 revs/min, and heated material to 80 DEG C, then the material that step (2) is obtained was added dropwise to reactor II in 1 ~ 2 hour, after dropwising, control temperature of reaction and continue reaction 1 ~ 2 hour at 75 ~ 85 DEG C, be finally down to room temperature discharging, be i.e. obtained modification aliphatic cyclic amine solidifying agent.
Described solidifying agent is the one in alicyclic ring amine curing agent.
Described epoxy resin is one or more of bisphenol A type epoxy resin.
Described thinner 1 and thinner 2 are one or more in aromatic alcohol.
Advantage of the present invention:
(1) the inventive method is simple to operate, is easy to large-scale promotion.
(2) the modification aliphatic cyclic amine solidifying agent stink that the inventive method is obtained is little, nonirritant, and viscosity is low, easy to use.
Embodiment
embodiment 1:
(1) take 18 kilograms the Meng alkane diamines, 6 kilograms of E-51 epoxy resin, 14 kilograms of phenylcarbinols and 8 kilograms of terephthalyl alcohols.
(2) the E-51 epoxy resin that step (1) takes is poured in reactor I, stir with the rotating speed of 600 revs/min, add the phenylcarbinol that step (1) takes in whipping process and stir 30 minutes, and heated material to 80 DEG C, stand-by.
(3) step (1) is taken the Meng alkane diamines and terephthalyl alcohol join in reactor II, 45 minutes are stirred with the rotating speed of 500 revs/min, and heated material to 80 DEG C, then the material that step (2) is obtained was added dropwise to reactor II in 2 hours, after dropwising, control temperature of reaction and continue reaction 2 hours at 75 DEG C, be finally down to room temperature discharging, be i.e. obtained modification aliphatic cyclic amine solidifying agent.
After tested, the viscosity of the modification aliphatic cyclic amine solidifying agent that the present embodiment obtains is (25 DEG C, mPa.s) 371, and amine value is (mgKOH/g) 263, and active hydrogen equivalent weight is 115; By obtained modification aliphatic cyclic amine solidifying agent and epoxy-based lacquers in mass ratio 1:2 join paint, the coating surface after solidification is smooth, and gloss is high, and without defects such as albefactions.
embodiment 2:
(1) 22 kilograms of different fluorine that ketone diamines, 7 kilograms of CYD128 epoxy resin, 15 kilograms of phenylcarbinols and 9 kilograms of terephthalyl alcohols are taken.
(2) the CYD128 epoxy resin that step (1) takes is poured in reactor I, stir with the rotating speed of 700 revs/min, add step (1) in whipping process to take phenylcarbinol and stir 25 minutes, and heated material to 80 DEG C, stand-by.
(3) different fluorine that ketone diamines step (1) taken and terephthalyl alcohol join in reactor II, 40 minutes are stirred with the rotating speed of 600 revs/min, and heated material to 80 DEG C, then the material that step (2) is obtained was added dropwise to reactor II in 1.5 hours, after dropwising, control temperature of reaction and continue reaction 1.5 hours at 80 DEG C, be finally down to room temperature discharging, be i.e. obtained modification aliphatic cyclic amine solidifying agent.
After tested, the viscosity of the modification aliphatic cyclic amine solidifying agent that the present embodiment obtains is (25 DEG C, mPa.s) 446, and amine value is (mgKOH/g) 284, and active hydrogen equivalent weight is 121; By the solidifying agent of preparation and epoxy-based lacquers in mass ratio 3:5 join paint, the coating surface after solidification is smooth, and gloss is high, and without defects such as albefactions.
Claims (1)
1. a preparation method for modification aliphatic cyclic amine solidifying agent, is characterized in that concrete steps are:
(1) raw material is taken by following mass ratio, solidifying agent: epoxy resin: thinner 1: thinner 2=30 ~ 50:10 ~ 20:25 ~ 35:15 ~ 25;
(2) epoxy resin that step (1) takes is poured in reactor I, stir with the rotating speed of 300 ~ 800 revs/min, add the thinner 1 that step (1) takes in whipping process and stir 20 ~ 30 minutes, and heated material to 80 DEG C, stand-by;
(3) thinner 2 that solidifying agent step (1) taken and step (1) take joins in reactor II, stir 30 ~ 50 minutes with the rotating speed of 300 ~ 800 revs/min, and heated material to 80 DEG C, then the material that step (2) is obtained was added dropwise to reactor II in 1 ~ 2 hour, after dropwising, control temperature of reaction and continue reaction 1 ~ 2 hour at 75 ~ 85 DEG C, be finally down to room temperature discharging, be i.e. obtained modification aliphatic cyclic amine solidifying agent;
Described solidifying agent is the one in alicyclic ring amine curing agent;
Described epoxy resin is one or more of bisphenol A type epoxy resin;
Described thinner 1 and thinner 2 are one or more in aromatic alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410673233.8A CN104356362A (en) | 2014-11-23 | 2014-11-23 | Preparation method of modified alicyclic amine curing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410673233.8A CN104356362A (en) | 2014-11-23 | 2014-11-23 | Preparation method of modified alicyclic amine curing agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104356362A true CN104356362A (en) | 2015-02-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410673233.8A Pending CN104356362A (en) | 2014-11-23 | 2014-11-23 | Preparation method of modified alicyclic amine curing agent |
Country Status (1)
| Country | Link |
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| CN (1) | CN104356362A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017776A (en) * | 2017-12-26 | 2018-05-11 | 湖南神力铃胶粘剂制造有限公司 | A kind of modified alicyclic ring amine hardener and preparation method thereof |
| CN115785867A (en) * | 2022-12-01 | 2023-03-14 | 上海富铭密封材料有限公司 | Epoxy resin pouring sealant with good chemical resistance for water treatment and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1460689A (en) * | 2003-05-16 | 2003-12-10 | 广州秀珀化工有限公司 | Modified alicyclic amine solidifying agent and its preparation method |
| CN101798378A (en) * | 2009-02-05 | 2010-08-11 | 魏庆梅 | Transparent epoxy resin curing agent |
| CN103224611A (en) * | 2013-05-15 | 2013-07-31 | 程梦喜 | Modified alicyclic amine curing agent and preparation method thereof |
| CN103554438A (en) * | 2013-10-12 | 2014-02-05 | 瑞奇化工（松滋）有限公司 | Preparation method of modified epoxy hardener for reducing bleaching |
| CN104151530A (en) * | 2014-08-19 | 2014-11-19 | 湖南神力铃胶粘剂制造有限公司 | Yellowing-resistance epoxy curing agent and preparation method thereof |
-
2014
- 2014-11-23 CN CN201410673233.8A patent/CN104356362A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1460689A (en) * | 2003-05-16 | 2003-12-10 | 广州秀珀化工有限公司 | Modified alicyclic amine solidifying agent and its preparation method |
| CN101798378A (en) * | 2009-02-05 | 2010-08-11 | 魏庆梅 | Transparent epoxy resin curing agent |
| CN103224611A (en) * | 2013-05-15 | 2013-07-31 | 程梦喜 | Modified alicyclic amine curing agent and preparation method thereof |
| CN103554438A (en) * | 2013-10-12 | 2014-02-05 | 瑞奇化工（松滋）有限公司 | Preparation method of modified epoxy hardener for reducing bleaching |
| CN104151530A (en) * | 2014-08-19 | 2014-11-19 | 湖南神力铃胶粘剂制造有限公司 | Yellowing-resistance epoxy curing agent and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017776A (en) * | 2017-12-26 | 2018-05-11 | 湖南神力铃胶粘剂制造有限公司 | A kind of modified alicyclic ring amine hardener and preparation method thereof |
| CN115785867A (en) * | 2022-12-01 | 2023-03-14 | 上海富铭密封材料有限公司 | Epoxy resin pouring sealant with good chemical resistance for water treatment and preparation method thereof |
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Application publication date: 20150218 |
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