CN104341582A - Preparation method of epoxy resin low temperature fast curing agent - Google Patents
Preparation method of epoxy resin low temperature fast curing agent Download PDFInfo
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- CN104341582A CN104341582A CN201410673173.XA CN201410673173A CN104341582A CN 104341582 A CN104341582 A CN 104341582A CN 201410673173 A CN201410673173 A CN 201410673173A CN 104341582 A CN104341582 A CN 104341582A
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Abstract
The invention discloses a preparation method of an epoxy resin low temperature fast curing agent. The method comprises the steps of pouring an amine curing agent into a reaction kettle; stirring the amine curing agent at 300-800 revolutions per minute (rpm); rising the temperature to 45 DEG C during the stirring process; adding hydroxybenzoic acid and stirring for 50-60 minutes; rising the temperature to 95 DEG C; adding urea; cooling to 50 DEG C to obtain a mixture after isothermally reacting for 1.5-2 hours; pouring diisopropylamine into a second reaction kettle; stirring the diisopropylamine at 300-800 rpm; adding mercaptan slowly; rising the temperature to 100 DEG C and isothermally reacting for 1-1.5 hours; reducing the temperature to 60 DEG C and adding a coupling agent; continuously stirring for 30-40 minutes; taking out the reacting product after cooling to the indoor temperature so as to obtain the epoxy resin low temperature fast curing agent. The method disclosed by the invention is simple to operate and easy to popularize.
Description
Technical field
The invention belongs to epoxy curing agent preparing technical field, particularly the preparation method of low-temperature fast-curing dose of a kind of epoxy resin.
Background technology
In modern technologies, the lower molecular weight polyimide resin being used as bonding is mostly 650 conventional both at home and abroad at present types or 651 type lower molecular weight polyimide resins.Using the tackiness agent of this room temperature curing type epoxy curing agent to have operating procedure simple, without the need to applying external force, the feature such as just can to solidify at normal temperatures.But this kind of tackiness agent can not solidify at low temperatures, and curing reaction speed is slow, be not suitable for sharp work, the quick embedding in electronic enterprises production line cannot be met, the quick-binding of modem architectural ornament industry, the problems such as road surface breakage is repaired in motorway express delivery, the Rapid leakage repairing of building building industry.
Summary of the invention
The object of this invention is to provide the preparation method of low-temperature fast-curing dose of a kind of epoxy resin.
Concrete steps are:
(1) raw material is taken by following mass ratio, amine curing agent: hydroxy-benzoic acid: ureas: mercaptan: Diisopropylamine: coupling agent=15 ~ 30:40 ~ 50:3 ~ 12:5 ~ 10:3 ~ 9:3 ~ 5.
(2) under room temperature, the amine curing agent that step (1) takes is poured in the first reactor, stir with the rotating speed of 300 ~ 800 revs/min, 45 DEG C are warming up in whipping process, then add the hydroxy-benzoic acid that step (1) takes to stir 50 ~ 60 minutes, be warming up to 95 DEG C again, finally add the ureas that step (1) takes, isothermal reaction was cooled to 50 DEG C after 1.5 ~ 2 hours, obtained compound.
(3) pour in the second reactor by the Diisopropylamine that step (1) takes, stir with the rotating speed of 300 ~ 800 revs/min, add mercaptan slowly, after being warming up to 100 DEG C, isothermal reaction 1 hour, is then cooled to room temperature, obtained compound.
(4) compound that step (2) is obtained is joined slowly in the obtained compound of step (3), limit edged stirs, be warming up to 130 DEG C of isothermal reactions 1 ~ 1.5 hour subsequently, then be cooled to 60 DEG C and add the coupling agent that step (1) takes, continue stirring 30 ~ 40 minutes, last cool to room temperature discharging, i.e. obtained low-temperature fast-curing dose of epoxy resin.
Described amine curing agent is one or more in aliphatic amide.
Described ureas is thiocarbamide.
Described mercaptan is THIOGLYCOL.
Described coupling agent is one or more in type siloxane coupling agent.
Advantage of the present invention:
(1) the inventive method is simple to operate, is easy to promote.
(2) low-temperature fast-curing dose of epoxy resin obtaining of the present invention can room temperature fast-curing, good with epoxy resin compatibility, and has good oil resistant water tolerance.
Embodiment
embodiment 1:
(1) 25 kilograms of triethylene tetramines, 45 kilograms of hydroxy-benzoic acids, 8 kilograms of thiocarbamides, 9 kilograms of THIOGLYCOL, 5 kilograms of Diisopropylamines and 4 kilograms of KH550 coupling agents are taken.
(2) under room temperature, the triethylene tetramine that step (1) takes is poured in the first reactor, stir with the rotating speed of 550 revs/min, 45 DEG C are warming up in whipping process, then add the hydroxy-benzoic acid that step (1) takes and stir 55 minutes, be warming up to 95 DEG C again, finally add the thiocarbamide that step (1) takes, isothermal reaction is cooled to 50 DEG C after 1 hour 45 minutes, obtained compound.
(3) step (1) being taken Diisopropylamine pours in the second reactor, and stir with the rotating speed of 550 revs/min, add THIOGLYCOL slowly, after being warming up to 100 DEG C, isothermal reaction 1 hour, is then cooled to room temperature, obtained compound.
(4) compound that step (2) is obtained is joined slowly in the obtained compound of step (3), limit edged stirs, be warming up to 130 DEG C of isothermal reactions subsequently 1 hour 15 minutes, then be cooled to 60 DEG C and add the KH550 coupling agent that step (1) takes, continue stirring 35 minutes, last cool to room temperature discharging, i.e. obtained low-temperature fast-curing dose of epoxy resin.
Quick-setting sizing agent under low-temperature fast-curing dose of the epoxy resin obtained by the present embodiment obtains a kind of room temperature after mixing by the mass ratio of 1:1.2 with epoxy resin, under room temperature, initial setting time is 6 minutes, setting time is 9 minutes, tensile shear strength is 12.3MPa, water soaking back draft half a year shearing resistance is 10.5MPa, and it is 11.7MPa that machine oil soaks back draft half a year shearing resistance.
embodiment 2:
(1) 28 kilograms of diethylenetriamines, 50 kilograms of hydroxy-benzoic acids, 10 kilograms of thiocarbamides, 10 kilograms of THIOGLYCOL, 5 kilograms of Diisopropylamines and 5 kilograms of KH570 coupling agents are taken.
(2) under room temperature, the diethylenetriamine that step (1) takes is poured in the first reactor, stir with the rotating speed of 550 revs/min, 45 DEG C are warming up in whipping process, then add the hydroxy-benzoic acid that step (1) takes to stir 50 ~ 60 minutes, be warming up to 95 DEG C again, finally add the thiocarbamide that step (1) takes, isothermal reaction is cooled to 50 DEG C after 1 hour 45 minutes, obtained compound.
(3) pour in the second reactor by the Diisopropylamine that step (1) takes, stir with the rotating speed of 550 revs/min, add THIOGLYCOL slowly, after being warming up to 100 DEG C, isothermal reaction 1 hour, is then cooled to room temperature, obtained compound.
(4) compound that step (2) is obtained is joined slowly in the obtained compound of step (3), limit edged stirs, be warming up to 130 DEG C of isothermal reactions subsequently 1 hour 15 minutes, then be cooled to 60 DEG C and add the KH570 coupling agent that step (1) takes, continue stirring 35 minutes, last cool to room temperature discharging, i.e. obtained low-temperature fast-curing dose of epoxy resin.
Quick-setting sizing agent under low-temperature fast-curing dose of the epoxy resin obtained by the present embodiment obtains a kind of room temperature after mixing by the mass ratio of 1:1.5 with epoxy resin, under room temperature, initial setting time is 6 minutes, setting time is 7 minutes, tensile shear strength is 11.4MPa, water soaking back draft half a year shearing resistance is 9.9MPa, and it is 10.2MPa that machine oil soaks back draft half a year shearing resistance.
Claims (1)
1. a preparation method for low-temperature fast-curing dose of epoxy resin, is characterized in that concrete steps are:
(1) raw material is taken by following mass ratio, amine curing agent: hydroxy-benzoic acid: ureas: mercaptan: Diisopropylamine: coupling agent=15 ~ 30:40 ~ 50:3 ~ 12:5 ~ 10:3 ~ 9:3 ~ 5;
(2) under room temperature, the amine curing agent that step (1) takes is poured in the first reactor, stir with the rotating speed of 300 ~ 800 revs/min, 45 DEG C are warming up in whipping process, then add the hydroxy-benzoic acid that step (1) takes to stir 50 ~ 60 minutes, be warming up to 95 DEG C again, finally add the ureas that step (1) takes, isothermal reaction was cooled to 50 DEG C after 1.5 ~ 2 hours, obtained compound;
(3) pour in the second reactor by the Diisopropylamine that step (1) takes, stir with the rotating speed of 300 ~ 800 revs/min, add mercaptan slowly, after being warming up to 100 DEG C, isothermal reaction 1 hour, is then cooled to room temperature, obtained compound;
(4) compound that step (2) is obtained is joined slowly in the obtained compound of step (3), limit edged stirs, be warming up to 130 DEG C of isothermal reactions 1 ~ 1.5 hour subsequently, then be cooled to 60 DEG C and add the coupling agent that step (1) takes, continue stirring 30 ~ 40 minutes, last cool to room temperature discharging, i.e. obtained low-temperature fast-curing dose of epoxy resin;
Described amine curing agent is one or more in aliphatic amide;
Described ureas is thiocarbamide;
Described mercaptan is THIOGLYCOL;
Described coupling agent is one or more in type siloxane coupling agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410673173.XA CN104341582A (en) | 2014-11-23 | 2014-11-23 | Preparation method of epoxy resin low temperature fast curing agent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410673173.XA CN104341582A (en) | 2014-11-23 | 2014-11-23 | Preparation method of epoxy resin low temperature fast curing agent |
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| CN104341582A true CN104341582A (en) | 2015-02-11 |
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| CN201410673173.XA Pending CN104341582A (en) | 2014-11-23 | 2014-11-23 | Preparation method of epoxy resin low temperature fast curing agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003445A (en) * | 2019-04-16 | 2019-07-12 | 上海盼逸新材料科技有限公司 | A method of the initiator containing amine, breast milk device and solidification breast milk |
| CN110343495A (en) * | 2019-08-13 | 2019-10-18 | 山东益丰生化环保股份有限公司 | A kind of epoxy resin adhesive and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394892A (en) * | 2002-08-07 | 2003-02-05 | 奚海 | Epoxy resin solidfying agent |
| CN102181042A (en) * | 2011-04-06 | 2011-09-14 | 无锡贝拉克新材料科技有限公司 | Method for preparing epoxy resin curing agent |
-
2014
- 2014-11-23 CN CN201410673173.XA patent/CN104341582A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394892A (en) * | 2002-08-07 | 2003-02-05 | 奚海 | Epoxy resin solidfying agent |
| CN102181042A (en) * | 2011-04-06 | 2011-09-14 | 无锡贝拉克新材料科技有限公司 | Method for preparing epoxy resin curing agent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003445A (en) * | 2019-04-16 | 2019-07-12 | 上海盼逸新材料科技有限公司 | A method of the initiator containing amine, breast milk device and solidification breast milk |
| CN110003445B (en) * | 2019-04-16 | 2021-09-21 | 上海盼逸新材料科技有限公司 | Amine-containing initiator, breast milk device and method for solidifying breast milk |
| CN110343495A (en) * | 2019-08-13 | 2019-10-18 | 山东益丰生化环保股份有限公司 | A kind of epoxy resin adhesive and preparation method thereof |
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Application publication date: 20150211 |