CN102786663A - Epoxy resin latent curing agent, preparation method thereof and method for preparing insulated paint by using epoxy resin latent curing agent - Google Patents

Epoxy resin latent curing agent, preparation method thereof and method for preparing insulated paint by using epoxy resin latent curing agent Download PDF

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Publication number
CN102786663A
CN102786663A CN2012103097160A CN201210309716A CN102786663A CN 102786663 A CN102786663 A CN 102786663A CN 2012103097160 A CN2012103097160 A CN 2012103097160A CN 201210309716 A CN201210309716 A CN 201210309716A CN 102786663 A CN102786663 A CN 102786663A
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epoxy resin
curing agent
latent curing
resin latent
preparation
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焦丕玉
朱宏
王晓梅
杜灵根
石磊
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712th Research Institute of CSIC
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712th Research Institute of CSIC
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Priority to CN2012103097160A priority Critical patent/CN102786663A/en
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Abstract

The invention relates to an epoxy resin latent curing agent for an insulated paint, a preparation method of the epoxy resin latent curing agent, and a method for preparing the insulated paint by using the epoxy resin latent curing agent. The epoxy resin latent curing agent is formed by complexion of tertiary amine epoxy curing agent and metal organic carboxylate, wherein the ertiary amine epoxy curing agent mainly comprises one or the combination of more of triethanolamine, tetramethylguanidine, N, N'-lupetazin, trimethylene diamine and benzyl dimethylamine; and the metal organic carboxylate mainly comprises one or the combination of two of zinc isoocatanoate and cobalt naphthenate. The preparation method of the curing agent comprises two steps of preparing materials and complexing. The step of preparing insulated paint includes the step of collocating the epoxy resin latent curing agent and the epoxy resin, and the step of mixing. The epoxy resin latent curing agent has the advantages of simplicity and convenience in preparation, long storage period after being mixed with the epoxy resin, and stability in storage; and the epoxy resin latent curing agent has fast reaction speed at high temperature, and short gelation time; and the curing substance has an excellent electrical property.

Description

A kind of epoxy resin latent curing agent and preparation method thereof and with its preparation insullac method
Technical field
The present invention relates to epoxy resin latent curing agent that a kind of insullac uses and preparation method thereof and with the method for its preparation insullac.
Background technology
Epoxy resin is widely used in electrical isolation and handles with its excellent comprehensive performance, and wherein epoxy-resin systems insullac is being widely used aspect the electrical machine insulation processing.Insullac mainly contains three kinds with epoxy curing agent, and a kind of is the hot setting type; A kind of is normal temperature cured type; A kind of is the intermediate temperature setting type.Electrical machine insulation lacquer requires to try one's best low temperature-curable, and in order to enhance productivity, curing speed should be as quickly as possible on the basis of performance requriements reaching.Epoxy curing agent is used in insulation at present; Two kinds of problems of ubiquity: the one,,, often use high-temperature curing agent in order to improve product shelf life; This situation causes energy consumption to increase, and some equipment of motor or specific type of electric machine parts can not stand the problem of high bake.The 2nd,, in order to reduce solidification value and set time, gentle low temperature curing agent perhaps adds curing catalyst in the use; This situation causes the insullac normal temperature storage time short; Need in time use up after requiring insullac to prepare, otherwise waste is bigger, has limited the use of product.
The most economical, the epoxy curing agent used of insullac should have following characteristics efficiently: 1, solidification value is moderate; 2, should lack set time as far as possible; 3, the insullac normal temperature storage phase is long as far as possible; 4, electrical insulation capability is excellent.
Summary of the invention
An object of the present invention is: epoxy resin latent curing agent that a kind of insullac efficiently uses and preparation method thereof is provided, and the insullac normal temperature storage phase of this solidifying agent and epoxy resin preparation is long, solidification value is moderate, set time is short, cured article electrical insulation capability excellence; Solidifying agent preparation method technology is simple and easy, easy master, stable and reliable product quality.
Another object of the present invention is: the method that a kind of epoxy resin latent curing agent preparation insullac is provided; This method technology is simple and easy, easy master, stable and reliable product quality, can obtain the product in different viscosity, setting time and storage time as required.
The technical scheme of epoxy resin latent curing agent of the present invention is:
A kind of epoxy resin latent curing agent, it is formed by tertiary amines epoxy hardener and the complexing of metal organic carboxylate; The tertiary amines epoxy hardener is mainly: the combination of one or more among trolamine, tetramethyl guanidine, the N, five kinds of N '-lupetazin, trimethylene diamines and benzyldimethylamines; The metal organic carboxylate is mainly: the combination of one or both in isocaprylic acid zinc and the cobalt naphthenate.
Further technical scheme is:
Described epoxy resin latent curing agent, its tertiary amines epoxy hardener and metal organic carboxylate proportioning by weight are 1:2~3;
Described epoxy resin latent curing agent is formed by trolamine and the complexing of isocaprylic acid zinc.
Described epoxy resin latent curing agent is formed by trolamine and isocaprylic acid zinc and cobalt naphthenate complexing.
Described epoxy resin latent curing agent, by tetramethyl guanidine, N, N '-lupetazin and isocaprylic acid zinc and cobalt naphthenate complexing form.
Described epoxy resin latent curing agent is formed by trimethylene diamines and the complexing of isocaprylic acid zinc.
Described epoxy resin latent curing agent is formed by benzyldimethylamine and cobalt naphthenate complexing.
Preparing method's technical scheme of epoxy resin latent curing agent of the present invention the steps include:
A, batching: take by weighing tertiary amines epoxy hardener and metal organic carboxylate;
B, complex reaction: with confected materials complex reaction 20~40 minutes under 100 ℃ ± 2 ℃ temperature; Obtain the epoxy resin latent curing agent at last; Said complex reaction, its reaction formula is:
Figure 66520DEST_PATH_IMAGE001
Further technical scheme is:
The preparation method of described epoxy resin latent curing agent the steps include:
A, batching: trolamine and isocaprylic acid zinc proportioning by weight are 1:2.5;
B, complex reaction: confected materials complex reaction 30 minutes under 100 ℃ ± 2 ℃ temperature.
Method and technology scheme with epoxy resin latent curing agent preparation insullac of the present invention the steps include:
A, batching: take by weighing epoxy resin and epoxy resin latent curing agent, both weight ratios are 1:10~15; Described epoxy resin is a kind of epoxy resin or several kinds the mixture wherein among E-44, E-51, F-44, the F-51;
B, mixing: in mixing vessel, earlier epoxy resin is heated to 80 ℃ ± 10 ℃, adds the epoxy resin latent curing agent then, it is even with above-mentioned two types of mixing of materials to restart whisking appliance, obtains thick insullac at last.
The principle of technical scheme that the present invention adopts is:
Tertiary amines epoxy hardener and the complexing under certain condition of metal organic carboxylate, thus the activity of tertiary amine under the room temperature reduced.Complex compound decomposes and makes solidifying agent produce activity at a certain temperature.Like this, not only guaranteed the stability in use under the system low temperature but also can make system PhastGel at high temperature.In fact this complex compound has become a kind of latent epoxy resin curing agent.It is long that such latent epoxy resin curing agent can be good at being suitable for insullac requirement ambient stable, working life, and the request for utilization of high temperature rapid curing.
Obvious technical effects of the present invention: 1) with after epoxy resin mixes, the normal temperature storage phase is long; 2) with after epoxy resin mixes, HTG is fast; 3) with after epoxy resin mixes, the time that reaches best state of cure is short; 4) with after epoxy resin fully solidifies, superior electrical property.
Embodiment
In conjunction with embodiment the present invention is described further as follows:
Embodiment 1:Be a basic embodiment of epoxy resin latent curing agent of the present invention.Said epoxy resin latent curing agent, it is formed by tertiary amines epoxy hardener and the complexing of metal organic carboxylate; The tertiary amines epoxy hardener is mainly: the combination of one or more among trolamine, tetramethyl guanidine, the N, five kinds of N '-lupetazin, trimethylene diamines and benzyldimethylamines; The metal organic carboxylate is mainly: the combination of one or both in isocaprylic acid zinc and the cobalt naphthenate.
Embodiment 2:Different with embodiment 1 is, described epoxy resin latent curing agent, and its tertiary amines epoxy hardener and metal organic carboxylate proportioning by weight are 1:2~3.
Embodiment 3:Be a preferred embodiment, different with embodiment 1 is that described epoxy resin latent curing agent is formed by trolamine and the complexing of isocaprylic acid zinc.
Embodiment 4:Be an embodiment preferably, different with embodiment 1 is, described epoxy resin latent curing agent is formed by trolamine and isocaprylic acid zinc and cobalt naphthenate complexing.
Embodiment 5:Be an embodiment preferably, different with embodiment 1 is, described epoxy resin latent curing agent, and by tetramethyl guanidine, N, N '-lupetazin and isocaprylic acid zinc and cobalt naphthenate complexing form.
Embodiment 6:Be an embodiment preferably, different with embodiment 1 is that described epoxy resin latent curing agent is formed by trimethylene diamines and the complexing of isocaprylic acid zinc.
Embodiment 7:Be an embodiment preferably, different with embodiment 1 is that described epoxy resin latent curing agent is formed by benzyldimethylamine and cobalt naphthenate complexing.
Embodiment 8: beThe basic embodiment of the preparation method of epoxy resin latent curing agent of the present invention the steps include:
A, batching: take by weighing tertiary amines epoxy hardener and metal organic carboxylate;
B, complex reaction: with confected materials complex reaction 20~40 minutes under 100 ℃ ± 3 ℃ temperature; Obtain the epoxy resin latent curing agent at last; Said complex reaction, its reaction formula is:
Figure 721624DEST_PATH_IMAGE002
Embodiment 9:Be a more excellent embodiment on the basis of embodiment 8 basic embodiment.The preparation method of described epoxy resin latent curing agent the steps include:
A, batching: the proportioning that takes by weighing trolamine and isocaprylic acid zinc weight meter is 1:2.5.
B, complex reaction: confected materials complex reaction 30 minutes under 100 ℃ ± 2 ℃ temperature.
Embodiment 10:Be with the basic embodiment of method of epoxy resin latent curing agent preparation insullac of the present invention, the steps include:
A, batching: take by weighing epoxy resin and epoxy resin latent curing agent, both weight ratios are 1:10~15; Described epoxy resin is a kind of epoxy resin or several kinds the mixture wherein among E-44, E-51, F-44, the F-51;
B, mixing: in mixing vessel, earlier epoxy resin is heated to 80 ± 10 ℃, adds the epoxy resin latent curing agent then, it is even with above-mentioned two types of mixing of materials to restart whisking appliance, obtains thick insullac at last.
Embodiment 11:Be a more excellent embodiment on the basis of embodiment 10 basic embodiment.The epoxy resin latent curing agent that is adopted is: trolamine and isocaprylic acid zinc weight ratio are 1:2, at the product of 100 ℃ ± 2 ℃ complex reactions after 35 minutes; The epoxy resin latent curing agent is mixed with epoxy resin.Its technique effect of the insullac that is mixed with is: the viscosity of testing under 20 ℃ of conditions is 45 seconds, 50 ℃ of condition held after 96 hours viscosity increase by 0.5 times, the gel time of testing under 140 ℃ of conditions is 4 minutes and 35 seconds, the tested media loss is 3.5% under 155 ℃ of conditions.
Embodiment 12:Be another embodiment on the basis of embodiment 10 basic embodiment.The epoxy resin latent curing agent that is adopted is: benzyldimethylamine and cobalt naphthenate weight ratio were 1:2,100 ℃ ± 2 ℃ complex reactions 30 minutes; The epoxy resin latent curing agent is mixed with epoxy resin.Its technique effect of the insullac that is mixed with is: the viscosity of testing under 20 ℃ of conditions is 46 seconds, 50 ℃ of condition held after 96 hours viscosity increase by 0.6 times, the gel time of testing under 140 ℃ of conditions is 4 minutes and 44 seconds, the tested media loss is 4.2% under 155 ℃ of conditions.
Insullac obvious technical effects with epoxy resin latent curing agent of the present invention and epoxy resin preparation: 1, the shelf lives can reach 6 months at normal temperatures; 2, under 140 ℃ probe temperature gel time less than 8 minutes; 3, under 140 ℃ solidification value, can reach best state of cure with interior in 4 hours; 4, under 155 ℃ temperature condition the tested media loss less than 5%.
Claim protection domain of the present invention is not limited to the foregoing description.

Claims (10)

1. an epoxy resin latent curing agent is characterized in that, it is formed by tertiary amines epoxy hardener and the complexing of metal organic carboxylate; The tertiary amines epoxy hardener is mainly: the combination of one or more among trolamine, tetramethyl guanidine, the N, five kinds of N '-lupetazin, trimethylene diamines and benzyldimethylamines; The metal organic carboxylate is mainly: the combination of one or both in isocaprylic acid zinc and the cobalt naphthenate.
2. epoxy resin latent curing agent according to claim 1 is characterized in that, tertiary amines epoxy hardener and metal organic carboxylate proportioning by weight are 1:2~3.
3. epoxy resin latent curing agent according to claim 1 and 2 is characterized in that, is formed by trolamine and the complexing of isocaprylic acid zinc.
4. epoxy resin latent curing agent according to claim 1 and 2 is characterized in that, is formed by trolamine and isocaprylic acid zinc and cobalt naphthenate complexing.
5. epoxy resin latent curing agent according to claim 1 and 2 is characterized in that, by tetramethyl guanidine, N, N '-lupetazin and isocaprylic acid zinc and cobalt naphthenate complexing form.
6. epoxy resin latent curing agent according to claim 1 and 2 is characterized in that, is formed by trimethylene diamines and the complexing of isocaprylic acid zinc.
7. epoxy resin latent curing agent according to claim 1 and 2 is characterized in that, is formed by benzyldimethylamine and cobalt naphthenate complexing.
8. the preparation method of the said epoxy resin latent curing agent of claim 1 is characterized in that, step is:
A, batching: take by weighing tertiary amines epoxy hardener and metal organic carboxylate;
B, complex reaction: with confected materials complex reaction 20~40 minutes under 100 ℃ ± 3 ℃ temperature; Obtain the epoxy resin latent curing agent at last; Said complex reaction, its reaction formula is:
9. the preparation method of epoxy resin latent curing agent according to claim 8 is characterized in that, step is:
A, batching: take by weighing trolamine and isocaprylic acid zinc proportioning by weight is 1:2.5;
B, complex reaction: confected materials complex reaction 30 minutes under 100 ℃ ± 2 ℃ temperature.
10. method with claim 1 epoxy resin latent curing agent preparation insullac is characterized in that step is:
A, batching: take by weighing epoxy resin and epoxy resin latent curing agent, both weight ratios are 1:10~15; Described epoxy resin is a kind of epoxy resin or several kinds the mixture wherein among E-44, E-51, F-44, the F-51;
B, mixing: in mixing vessel, earlier epoxy resin is heated to 80 ± 10 ℃, adds the epoxy resin latent curing agent then, it is even with above-mentioned two types of mixing of materials to restart whisking appliance, obtains thick insullac at last.
CN2012103097160A 2012-08-28 2012-08-28 Epoxy resin latent curing agent, preparation method thereof and method for preparing insulated paint by using epoxy resin latent curing agent Pending CN102786663A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3804799A (en) * 1972-09-01 1974-04-16 Air Prod & Chem Metal-amine complex accelerator for polyester resin curing
US4814391A (en) * 1988-05-09 1989-03-21 General Electric Company Heat curable epoxy compositions, and amine adducts of cobalt (II) complexes
JP2005154304A (en) * 2003-11-21 2005-06-16 Nof Corp Radically polymerizable hemiacetal ester derivative and its use
CN102181043A (en) * 2011-03-23 2011-09-14 吴江固德电材系统有限公司 latent curing agent with multiple storage stability

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3804799A (en) * 1972-09-01 1974-04-16 Air Prod & Chem Metal-amine complex accelerator for polyester resin curing
US4814391A (en) * 1988-05-09 1989-03-21 General Electric Company Heat curable epoxy compositions, and amine adducts of cobalt (II) complexes
JP2005154304A (en) * 2003-11-21 2005-06-16 Nof Corp Radically polymerizable hemiacetal ester derivative and its use
CN102181043A (en) * 2011-03-23 2011-09-14 吴江固德电材系统有限公司 latent curing agent with multiple storage stability

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Application publication date: 20121121