CN109438676A - 一种环氧树脂用低温快速固化的固化剂及其制备方法 - Google Patents
一种环氧树脂用低温快速固化的固化剂及其制备方法 Download PDFInfo
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 16
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- -1 slabstone Substances 0.000 claims abstract description 9
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims abstract description 6
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 5
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical group CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 239000004568 cement Substances 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract description 2
- 230000003014 reinforcing effect Effects 0.000 abstract description 2
- 239000004593 Epoxy Substances 0.000 abstract 1
- 230000009257 reactivity Effects 0.000 abstract 1
- 239000010802 sludge Substances 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 abstract 1
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5006—Amines aliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4207—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
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- Epoxy Resins (AREA)
Abstract
本发明涉及一种环氧树脂用低温快速固化的固化剂及其制备方法，它是一种适用于低温可快速固化的环氧树脂固化剂。本发明主要组份的重量份数是：1,6己二胺50‑57份，丙烯酸异辛酯32‑36份，促进剂10‑17份。本发明没有废水和废渣排放；由于本固化剂反应活性高，且含有促进剂，具有较好的施工性,能在低温环境下快速固化，解决了环氧树脂在常温甚至低温（2℃）固化速度慢的缺点。适用于水泥、石板、玻璃等粘接加固、水利工程等领域。
Description
技术领域
本发明涉及一种环氧树脂用低温快速固化的固化剂及其制备方法。
背景技术
目前能在低温使用的固化剂中，存在聚硫醇粘度大价格高、硫脲改性胺固化剂毒性大价格高、改性酚醛胺固化剂在0-5℃固化慢等不足。本发明能在低温环境下快速固化，解决了环氧树脂在常温甚至低温（2℃）固化速度慢的缺点。适用于水泥、石板、玻璃等粘接加固、水利工程等领域。
发明内容
为解决上述胶粘剂使用性能之不足，一种环氧树脂用低温快速固化的固化剂及其制备方法。
本发明的目的是通过以下技术方案实现的：
本发明是1,6己二胺、丙烯酸酯和促进剂的反应混合物；主要组份的重量份数为：
1,6己二胺 50-57份
丙烯酸酯 32-36份
促进剂 10-17份
所述的丙烯酸酯为甲基丙烯酸酯、甲基丙烯酸丁酯、丙烯酸异辛酯或它们的混合物；
所述的促进剂为DMP-30、苄醇、乙醇或它们的混合物。
本发明的制备方法如下：
（1）在带搅拌的三口烧瓶中，加入加热至45-50℃的1,6-己二胺，调节温度在80-85℃范围，开启搅拌，转速85-100转/分；
（2）在80-85℃温度下，加入促进剂；
（3）调节温度在82-88℃，滴加丙烯酸酯，2小时滴加完毕，继续反应30分钟即可；
（4）降温到45℃左右，出料即可。
本发明的积极效果在于将本发明的产品与环氧树脂配合后，在低温(0-10)环境下作业，能较快的固化并具有强度，便于施工作业、提高工效。本发明与环氧树脂具有在低温环境下使用，克服了一般胶粘剂需要在室温下才能使用的缺陷。
具体实施方式：
[实施例1]
将50克已预热到45℃的1,6己二胺加入到带搅拌的三口烧瓶中，调节温度在46℃，开启搅拌，控制转速约90转/分；调节温度在82℃，加入16克促进剂DMP-30；在82℃时开始滴加甲基丙烯酸酯，共加入34克，滴加温度控制在82-88℃范围，2小时滴加完毕，后继续反应30分钟，降温到45℃左右，出料即可；
将本发明与环氧树脂配合在2℃环境下使用，126分钟固化,180分钟具有一定的粘接强度。
[实施例2]
将57克已预热到45℃的1,6己二胺加入到带搅拌的三口烧瓶中，调节温度在49℃，开启搅拌，控制转速约95转/分；调节温度在85℃，加入10克促进剂DMP-30；在85℃时开始滴加甲基丙烯酸丁酯，共加入33克，滴加温度控制在84-88℃范围，2小时滴加完毕，后继续反应30分钟，降温到45℃左右，出料即可；
将本发明与环氧树脂配合在0℃环境下使用，148分钟固化,210分钟具有一定的粘接强度。
[实施例3]
将53克已预热到45℃的1,6己二胺加入到带搅拌的三口烧瓶中，调节温度在47℃，开启搅拌，控制转速约90转/分；调节温度在86℃，加入11促进剂DMP-30；在85℃时开始滴加甲基丙烯酸酯，共加入36克，滴加温度控制在85-90℃范围，2小时滴加完毕，后继续反应30分钟，降温到45℃左右，出料即可；
将本发明与环氧树脂配合在8℃环境下使用，110分钟固化,145分钟具有一定的粘接强度。
Claims (3)
1.一种环氧树脂用低温快速固化的固化剂，其特征在于其特征在于各组份及其重量份数组成为：
1,6己二胺 50-57份
丙烯酸酯 32-36份
促进剂 10-17份
所述的一种环氧树脂用低温快速固化的固化剂制备方法，是由下列步骤组成：
（1）在带搅拌的三口烧瓶中，加入加热至45-50℃的1,6-己二胺，调节温度在80-85℃范围，开启搅拌，转速85-100转/分；
（2）在80-85℃温度下，加入促进剂；
（3）调节温度在82-88℃，滴加丙烯酸酯，2小时内滴加完毕，继续反应30分钟即可；
（4）降温到45℃左右，出料即可。
2.如权利要求1所述的一种环氧树脂用低温快速固化的固化剂，其特征在于所述丙烯酸酯为甲基丙烯酸酯、甲基丙烯酸丁酯、丙烯酸异辛酯或它们的混合物。
3.如权利要求1所述的一种环氧树脂用低温快速固化的固化剂及其制备方法，其特征在于所述促进剂为DMP-30、苄醇、乙醇或它们的混合物。
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5359123A (en) * | 1991-02-12 | 1994-10-25 | Nippon Paint Co., Ltd. | Polyoxyalkylene polyamines having secondary amino groups |
| JPH08198942A (ja) * | 1995-01-25 | 1996-08-06 | Asahi Denka Kogyo Kk | 湿潤面ないし水中施工用エポキシ樹脂組成物 |
| JPH1180322A (ja) * | 1997-09-02 | 1999-03-26 | Mitsubishi Gas Chem Co Inc | エポキシ樹脂組成物のポットライフの延長方法 |
| US20080287644A1 (en) * | 2007-04-05 | 2008-11-20 | Uppc Ag | Hardener for epoxy resins, method for hardening an epoxy resin and use of the hardener |
| CN103755923A (zh) * | 2013-12-26 | 2014-04-30 | 江苏苏博特新材料股份有限公司 | 一种低温固化型脂肪族酰胺多胺环氧树脂固化剂及其制备方法 |
| CN104927303A (zh) * | 2015-06-04 | 2015-09-23 | 孙仁华 | 一种抗紫外老化的纤维增强聚合物基复合材料 |
| CN107177031A (zh) * | 2017-04-17 | 2017-09-19 | 烟台大学 | 一种甲基丙烯酸缩水甘油酯改性胺固化剂及防流挂涂料 |
-
2018
- 2018-10-30 CN CN201811272977.3A patent/CN109438676A/zh active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5359123A (en) * | 1991-02-12 | 1994-10-25 | Nippon Paint Co., Ltd. | Polyoxyalkylene polyamines having secondary amino groups |
| JPH08198942A (ja) * | 1995-01-25 | 1996-08-06 | Asahi Denka Kogyo Kk | 湿潤面ないし水中施工用エポキシ樹脂組成物 |
| JPH1180322A (ja) * | 1997-09-02 | 1999-03-26 | Mitsubishi Gas Chem Co Inc | エポキシ樹脂組成物のポットライフの延長方法 |
| US20080287644A1 (en) * | 2007-04-05 | 2008-11-20 | Uppc Ag | Hardener for epoxy resins, method for hardening an epoxy resin and use of the hardener |
| CN103755923A (zh) * | 2013-12-26 | 2014-04-30 | 江苏苏博特新材料股份有限公司 | 一种低温固化型脂肪族酰胺多胺环氧树脂固化剂及其制备方法 |
| CN104927303A (zh) * | 2015-06-04 | 2015-09-23 | 孙仁华 | 一种抗紫外老化的纤维增强聚合物基复合材料 |
| CN107177031A (zh) * | 2017-04-17 | 2017-09-19 | 烟台大学 | 一种甲基丙烯酸缩水甘油酯改性胺固化剂及防流挂涂料 |
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Application publication date: 20190308 |