CN1460689A - Modified alicyclic amine solidifying agent and its preparation method - Google Patents
Modified alicyclic amine solidifying agent and its preparation method Download PDFInfo
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- CN1460689A CN1460689A CN 03126625 CN03126625A CN1460689A CN 1460689 A CN1460689 A CN 1460689A CN 03126625 CN03126625 CN 03126625 CN 03126625 A CN03126625 A CN 03126625A CN 1460689 A CN1460689 A CN 1460689A
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Abstract
The present invention relates to a modified alicyclic amine solidifying agent and its preparation method. It is formed from (wt%) 38-45% of isophorone diamine, 12-18% of epoxy resin and 37-50% of benzyl alcohol, and its preparation method includes the following steps: adding epoxy resin and proper quantity of benzyl alcohol into a three-mouth flask, heating to 70 deg.C for stand-by; adding isophorone diamine and residual benzyl alcohol into another four-mouth flask, heating to 70 deg.c, then drop-adding material of three-mouth flask into four-mouth flask to make reaction, controlling drop-adding speed to make reaction at 70-80 deg.C for 1-2 hr. after the drop-addition continuously reacting for 1 hr. at 70-80 deg.C, cooling and discharging material so as to obtain the invented product.
Description
Technical field:
The present invention relates to a kind of epoxy curing agent, particularly a kind of modification aliphatic cyclic amine solidifying agent and preparation method thereof.
Prior art:
Resins, epoxy is an important kind in the synthetic resins field, because it has a series of good performances, strong as cohesiveness, shrinking percentage is little, mechanical property, dielectric properties and fine heat-resisting performance, good chemical stability is so be widely used in electronics, electrical equipment, machinery, chemical industry, civil engineering work, national defence and other the many production fields.Adopt Resins, epoxy can make numerous high-performance coatings, as cathode electrodeposition priming paint, powder coating, food cans and soft drink can inner-wall paint, boats and ships and heavy duty system, industry ground slab coating, insullac etc.
Resins, epoxy itself is thermoplastic work piece, make epoxy resin-based paint have premium properties, Resins, epoxy and solidifying agent must be carried out crosslinking reaction and form cancellated macromole.Curing agent for epoxy resin is of a great variety, and commonly used have alicyclic polyamines such as aliphatic polyamine and isophorone diamines, 1 such as quadrol, diethylenetriamine, triethylene tetramine, 2-diamino-cyclohexane.These aliphatics or alicyclic polyamine solidifying agent have very high reactive behavior, but normal temperature and low-temperature curing, and it is low to have viscosity, advantages such as chemical resistance is good, but they have following weak point: thermal discharge is big when 1. solidifying, and once joining lacquer can not be too many, and the construction time limit is short.2. the reactive hydrogen equivalent is very low, and joining the lacquer weighing must be accurately, and excessive or not enough meeting influence performance.3. volatile, frowziness and pungency influence operator's health.4. moisture absorption is arranged, under the situation of low temperature and high relative humidity, easily form carbaminate, separate out in coating surface and undermine outward appearance, and influence ply adhesion with airborne moisture and carbon dioxide reaction.5. height polarity, they are not good enough with the compatibility of Resins, epoxy, easily cause disadvantages such as paint film shrinkage cavity, tangerine peel, whiting, so will wait moments later just application of slaking during construction.
Summary of the invention
The purpose of this invention is to provide a kind of modification aliphatic cyclic amine solidifying agent that is used for the epoxies terrace paint and preparation method thereof, it has overcome the shortcoming of above-mentioned aliphatic amide and aliphatic cyclic amine solidifying agent, has the advantage that color and luster is light, tint retention good, viscosity is low, during with its cured epoxy resin, gloss of film degree height is difficult for moisture absorption whiting, and stink is little, can directly use without slaking, can be in envrionment temperature and low-temperature curing.
The object of the present invention is achieved like this: modification aliphatic cyclic amine solidifying agent is by isophorone diamine, Resins, epoxy, and phenylcarbinol is formed.Each constituent content is isophorone diamine 38～45% by weight percentage, Resins, epoxy 12～18%, phenylcarbinol 37～50%.
A kind of modification aliphatic cyclic amine solidifying agent preparation method is characterized in that realizing by following step:
The first step: in the there-necked flask of band whipping appts and thermometer, add 12～18 parts Resins, epoxy and 24～36 parts phenylcarbinol.Start stirring, with material be heated to 70 ℃ stand-by.
Second step: in the four-hole bottle of band whipping appts, thermometer and constant pressure funnel, add 38～45 parts isophorone diamine and 13～24 parts phenylcarbinol, start stirring, material is heated to 70 ℃.The material of the first step gained dripped into by constant pressure funnel react, the control rate of addition makes and is reflected at 70～80 ℃ and carries out, and dropwises in 1～2 hour.
The 3rd step: continue at 70～80 ℃ of reactions 1 hour, cooling discharge.
Modification aliphatic cyclic amine solidifying agent of the present invention is by carrying out addition reaction with Resins, epoxy and excessive aliphatic cyclic amine isophorone diamine, obtain the affixture of aliphatic cyclic amine, thereby reduced the toxicity of solidifying agent, improved the consistency with Resins, epoxy, improved the performance of the anti-albefaction of paint film.Add phenylcarbinol and play the effect that reduces viscosity as non-activated thinner and softening agent.Because it has the aliphatic cyclic amine lighter color, tint retention is good, and the advantage that gloss is high is especially suitable for use as the solidifying agent of epoxies terrace paint.Its main performance index is: and viscosity (25 ℃, mPa.s) 100～700, amine value (mgKOH/g) 250～300.The reactive hydrogen equivalent is 100～125, and hectogram standard epoxy (EEW=190) consumption is 53～66.
Specific embodiment:
Below in conjunction with embodiment the present invention is described in further detail.% embodiment 1
In the there-necked flask of band whipping appts and thermometer, add 15 parts E-51 Resins, epoxy and 30 parts phenylcarbinol, start stirring, with material be heated to 70 ℃ stand-by.In the four-hole bottle of another band whipping appts, thermometer and constant pressure funnel, add 41 parts isophorone diamine and 14 parts phenylcarbinol, start stirring, material is heated to 70 ℃.Then the material in the aforementioned there-necked flask is dripped into by constant pressure funnel and react, the control rate of addition makes and is reflected at 70～80 ℃ and carries out, and dropwises in 1～2 hour.Continuation is at 70～80 ℃ of reactions 1 hour, cooling discharge.Products therefrom is colourless or the light yellow clarifying liquid body, and (25 ℃ is 350～420 mPa.s) to viscosity, and amine value (mgKOH/g) is 262～272.The reactive hydrogen equivalent is 113, and hectogram standard epoxy (EEW=190) consumption is 60.
Join lacquer to scale with the foregoing description 1 gained solidifying agent and epoxy self-leveling colored paint and solidify, the gained coating surface is smooth solid, color homogeneous, gloss height, no albefaction, loose colour film defect such as grow dim.
Embodiment 2
In the there-necked flask of band whipping appts and thermometer, add 14 parts E-51 Resins, epoxy and 28 parts phenylcarbinol, start stirring, with material be heated to 70 ℃ stand-by.In the four-hole bottle of another band whipping appts, thermometer and constant pressure funnel, add 45 parts isophorone diamine and 13 parts phenylcarbinol, start stirring, material is heated to 70 ℃.Then the material in the aforementioned there-necked flask is dripped into by constant pressure funnel and react, the control rate of addition makes and is reflected at 70～80 ℃ and carries out, and dropwises in 1～2 hour.Continuation is at 70～80 ℃ of reactions 1 hour, cooling discharge.Products therefrom is colourless or the light yellow clarifying liquid body, and (25 ℃ is 250～320 mPa.s) to viscosity, and amine value (mgKOH/g) is 292～300.The reactive hydrogen equivalent is 102, and hectogram standard epoxy (EEW=190) consumption is 54.
Join lacquer with the foregoing description 2 gained solidifying agent and epoxy anti-electrostatic to scale from the levelling colored paint and solidify, the gained coating surface is smooth solid, color homogeneous, gloss height, no albefaction, loose colour film defect such as grow dim.
Claims (3)
1. a modification aliphatic cyclic amine solidifying agent is characterized in that by isophorone diamine, Resins, epoxy, and phenylcarbinol is formed, and the weight percent of each constituent content is an isophorone diamine 38～45%, Resins, epoxy 12～18%, phenylcarbinol 37～50%.
2. modification aliphatic cyclic amine solidifying agent as claimed in claim 1 is characterized in that Resins, epoxy is bisphenol-A liquid epoxy resin, and its standard epoxy equivalent (weight) is 190.
3. modification aliphatic cyclic amine solidifying agent preparation method is characterized in that realizing by following step:
The first step: in the there-necked flask of band whipping appts and thermometer, add 12～18 parts Resins, epoxy and 24～36 parts phenylcarbinol.Start stirring, with material be heated to 70 ℃ stand-by.
Second step: in the four-hole bottle of band whipping appts, thermometer and constant pressure funnel, add 38～45 parts isophorone diamine and 13～24 parts phenylcarbinol, start stirring, material is heated to 70 ℃.The material of the first step gained dripped into by constant pressure funnel react, the control rate of addition makes and is reflected at 70～80 ℃ and carries out, and dropwises in 1～2 hour.
The 3rd step: continue at 70～80 ℃ of reactions 1 hour, cooling discharge.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03126625 CN1220714C (en) | 2003-05-16 | 2003-05-16 | Modified alicyclic amine solidifying agent and its preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03126625 CN1220714C (en) | 2003-05-16 | 2003-05-16 | Modified alicyclic amine solidifying agent and its preparation method |
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| CN1460689A true CN1460689A (en) | 2003-12-10 |
| CN1220714C CN1220714C (en) | 2005-09-28 |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100368495C (en) * | 2004-11-10 | 2008-02-13 | 上海市涂料研究所 | Water epoxy resin paint and its making process |
| CN101338018B (en) * | 2007-07-06 | 2010-09-08 | 上海树脂厂有限公司 | Epoxy curing agent and method for preparing same |
| 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 |
| 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 |
| 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 |
| CN104356362A (en) * | 2014-11-23 | 2015-02-18 | 桂林理工大学 | Preparation method of modified alicyclic amine curing agent |
| CN104725783A (en) * | 2014-12-25 | 2015-06-24 | 上海康达新能源材料有限公司 | Anti-sagging and anti-crystallizing wind power hand lay-up resin system and preparation method thereof |
| CN104837907A (en) * | 2012-12-20 | 2015-08-12 | 陶氏环球技术有限责任公司 | Low emission epoxy curing agents |
| CN107964088A (en) * | 2016-10-18 | 2018-04-27 | 中国石油化工股份有限公司 | A kind of hypotoxicity is modified the preparation method of ethylenediamine curing agent |
| 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 |
| CN108341926A (en) * | 2018-02-06 | 2018-07-31 | 西安天元化工有限责任公司 | A kind of epoxy resin of low-temperature curable and the coating containing it |
| CN109280521A (en) * | 2018-09-30 | 2019-01-29 | 武汉市石代高新建材有限公司 | A kind of epoxy structural rubber curing agent and its preparation method and application |
| 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 |
| CN111961191A (en) * | 2020-08-29 | 2020-11-20 | 江苏三木化工股份有限公司 | Epoxy curing agent for seaming and preparation method thereof |
| CN113150700A (en) * | 2021-03-25 | 2021-07-23 | 湖南神力铃胶粘剂制造有限公司 | Epoxy stone repair face adhesive with yellowing resistance, low viscosity and hydrophilic curing and preparation method thereof |
| CN113652145A (en) * | 2021-07-28 | 2021-11-16 | 上海涂固安高科技有限公司 | Modified high-performance epoxy solvent-free coating |
| CN115491102A (en) * | 2022-10-25 | 2022-12-20 | 湖南彩田新材料有限公司 | Solvent-free epoxy super-wear-resistant coating and preparation method thereof |
-
2003
- 2003-05-16 CN CN 03126625 patent/CN1220714C/en not_active Expired - Lifetime
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100368495C (en) * | 2004-11-10 | 2008-02-13 | 上海市涂料研究所 | Water epoxy resin paint and its making process |
| CN101338018B (en) * | 2007-07-06 | 2010-09-08 | 上海树脂厂有限公司 | Epoxy curing agent and method for preparing same |
| CN104837907A (en) * | 2012-12-20 | 2015-08-12 | 陶氏环球技术有限责任公司 | Low emission epoxy curing agents |
| 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 |
| 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 |
| 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 |
| CN104356362A (en) * | 2014-11-23 | 2015-02-18 | 桂林理工大学 | Preparation method of modified alicyclic amine curing agent |
| CN104725783A (en) * | 2014-12-25 | 2015-06-24 | 上海康达新能源材料有限公司 | Anti-sagging and anti-crystallizing wind power hand lay-up resin system and preparation method thereof |
| CN104725783B (en) * | 2014-12-25 | 2017-09-19 | 上海康达新能源材料有限公司 | A kind of resist sagging and the brilliant wind-powered electricity generation level hand paste resin system of resistive connection and preparation method thereof |
| CN107964088A (en) * | 2016-10-18 | 2018-04-27 | 中国石油化工股份有限公司 | A kind of hypotoxicity is modified the preparation method of ethylenediamine curing agent |
| 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 |
| CN108341926A (en) * | 2018-02-06 | 2018-07-31 | 西安天元化工有限责任公司 | A kind of epoxy resin of low-temperature curable and the coating containing it |
| CN108341926B (en) * | 2018-02-06 | 2020-06-16 | 西安天元化工有限责任公司 | Low-temperature curable epoxy resin and coating containing same |
| CN109280521A (en) * | 2018-09-30 | 2019-01-29 | 武汉市石代高新建材有限公司 | A kind of epoxy structural rubber curing agent and its preparation method and application |
| CN109280521B (en) * | 2018-09-30 | 2021-06-01 | 武汉市石代高新建材有限公司 | Epoxy structural adhesive curing agent and preparation method and application thereof |
| 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 |
| CN111961191A (en) * | 2020-08-29 | 2020-11-20 | 江苏三木化工股份有限公司 | Epoxy curing agent for seaming and preparation method thereof |
| CN111961191B (en) * | 2020-08-29 | 2023-05-30 | 江苏三木化工股份有限公司 | Epoxy curing agent for joint king and preparation method thereof |
| CN113150700A (en) * | 2021-03-25 | 2021-07-23 | 湖南神力铃胶粘剂制造有限公司 | Epoxy stone repair face adhesive with yellowing resistance, low viscosity and hydrophilic curing and preparation method thereof |
| CN113652145A (en) * | 2021-07-28 | 2021-11-16 | 上海涂固安高科技有限公司 | Modified high-performance epoxy solvent-free coating |
| CN115491102A (en) * | 2022-10-25 | 2022-12-20 | 湖南彩田新材料有限公司 | Solvent-free epoxy super-wear-resistant coating and preparation method thereof |
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| CN1220714C (en) | 2005-09-28 |
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Owner name: GUANGZHOU XIUPO CHEMICAL ENGINEERING CO., LTD. Free format text: FORMER NAME OR ADDRESS: GUANGZHOU XIUBO CHEMICAL CO., LTD. |
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Address after: No. 72, Xie Shi Road, clock Town, Panyu District, Guangdong, Guangzhou Patentee after: GUANGZHOU SUPE CHEMICAL Co.,Ltd. Address before: No. 72, Xie Shi Road, clock Town, Panyu District, Guangdong, Guangzhou Patentee before: GUANGZHOU XIUBO CHEMICAL Co.,Ltd. |
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Address after: Supe Industrial Park, No. 72 Panyu District Zhong villages of Guangzhou city in Guangdong province 511495 Xie Shi Lu Patentee after: GUANGZHOU SUPE CHEMICAL COATING CO.,LTD. Address before: Panyu District zhongcunzhen Guangzhou city in Guangdong province 511495 Xie Shi Road No. 72 Patentee before: GUANGZHOU SUPE CHEMICAL Co.,Ltd. |
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Granted publication date: 20050928 |