CN104403089A - High-performance modified epoxy alicyclic amine curing agent and preparation method thereof - Google Patents
High-performance modified epoxy alicyclic amine curing agent and preparation method thereof Download PDFInfo
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- CN104403089A CN104403089A CN201410757205.4A CN201410757205A CN104403089A CN 104403089 A CN104403089 A CN 104403089A CN 201410757205 A CN201410757205 A CN 201410757205A CN 104403089 A CN104403089 A CN 104403089A
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Abstract
The invention discloses a high-performance modified epoxy alicyclic amine curing agent. The high-performance modified epoxy alicyclic amine curing agent has the characteristics of being stable in performance and low in irritability and specifically has the following characteristics: the color is transparent, the temperature tolerance can reach 120-150 DEG C, the shore hardness reaches 80-85D, the adhesive force reaches the class A, the alcohol tolerance can have no change in color for 15 days, and the shearing strength is 12-16 MPa; the high-performance modified epoxy alicyclic amine curing agent can be widely applied to the fields of high-temperature baking type anti-yellowing glass paint, normal-temperature self-drying glass paint, solvent-resistant high-adhesion wine bottle paint, adhesives and transparent anti-yellowing electronic potting. The invention also provides a preparation method of the high-performance modified epoxy alicyclic amine curing agent; the raw material components are scientific and reasonable in ratio; the preparation method is scientific and reasonable; the temperature and the time of reaction in the preparation process can be effectively controlled; the curing agent with moderate viscosity, rate and ratio can be prepared; the self moisture absorption property and brittleness of the alicyclic amine can be greatly improved; the adhesive force, the adhesive performance and the solvent resistance of the alicyclic amine are improved.
Description
Technical field
The present invention relates to solidifying agent preparing technical field, relate to a kind of modified epoxy aliphatic cyclic amine high-performance solidifying agent and preparation method thereof specifically.
Background technology
Epoxy resin is a kind of important thermosetting resin, it has a series of excellent performance, and its cohesive strength is high, shrinks little, the advantages such as good dielectric properties and resistance toheat, so be widely used in many production fields such as electronics, sizing agent, coating, building, national defence.
Epoxy resin is given epoxy resin paint and is had excellent performance, epoxy resin and solidifying agent must be carried out the molecule of cross-linked structure.Epoxy curing agent is of a great variety, for isophorone diamine, isophorone diamine is called for short IPDA, it is a kind of alicyclic diamine made by isophorone chemical reaction, by 3-aminomethyl 3,5, the mixture of two kinds of isomer formation of 5-trimethylcyclohexyl amine, as a kind of alicyclic diamine, IPDA can be used in all common amine reactions, be widely used in glass baking varnish, in some matrix materials such as bottle paint, but to have amine value high due to aliphatic cyclic amine, and proportioning is large, the defect such as moisture absorption and fragility, is not easy to operation and uses.
Summary of the invention
The present invention aims to provide a kind of modified epoxy aliphatic cyclic amine high-performance solidifying agent and preparation method thereof, it can obtain a kind of viscosity, speed, solidifying agent that proportioning is moderate, substantially improve moisture absorption and the fragility of aliphatic cyclic amine self, improve the performance of its sticking power, adhesive property and solvent resistance etc.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of modified epoxy aliphatic cyclic amine high-performance solidifying agent, comprises the raw material of following weight part:
20-40 part isophorone diamine, 30-45 part phenylcarbinol, 8-15 part 1,3-hexamethylene dimethylamine, 30-38 part N-aminoethyl piperazine, 10-20 part Amino Terminated polyether(ATPE), 10-35 part epoxy resin.
A preparation method for modified epoxy aliphatic cyclic amine high-performance solidifying agent, comprises the steps:
S1: add 20-40 part isophorone diamine successively at reactor, 30-45 part phenylcarbinol, 8-15 part 1,3-hexamethylene dimethylamine, 30-38 part N-aminoethyl piperazine, 10-20 part Amino Terminated polyether(ATPE), stirs after mixing;
S2: the vacuum pipe of access band negative pressure in described reactor, 10-35 part epoxy resin is at the uniform velocity added drop-wise in described reactor by control valve and concentrates reaction, temperature of reaction controls between 75-85 DEG C by ON cycle water coolant simultaneously, and time for adding controls between 30-40 minute;
S3: the material in described reactor is concentrated reaction maintenance 3 hours, close described recirculated cooling water, until temperature is cooled to vacuum pumping blowing between 45-55 DEG C.
The pressure of the vacuum pipe further in described step S2 is-0.08Mpa.
Temperature of reaction further in described step S2 is 80 DEG C.
Temperature further in described step S3 is cooled to 50 DEG C of vacuum pumping blowings.
Further in described step S2 and step S3 with thermometer.
Stirred by agitator in described step S1 further.
The stirring velocity of described agitator is 150 revs/min further.
Adopt technique scheme, the present invention at least comprises following beneficial effect:
1. modified epoxy aliphatic cyclic amine high-performance solidifying agent of the present invention, has stable performance, bland feature, is embodied in: transparent color and luster, heat resistance can reach 120-150 DEG C, shore hardness reaches 80-85D, adhesion 1 grade, alcohol resistance nondiscoloration in 15 days, shearing resistance 12-16Mpa etc., it can be widely used in high bake type color inhibition glass lacquer, normal temperature self-drying type glass lacquer, solvent-resisting, high adhesive force bottle paint, sizing agent, the fields such as transparent yellowing-resistant electronics embedding.
2. the preparation method of modified epoxy aliphatic cyclic amine high-performance solidifying agent of the present invention, feed composition proportioning and the preparation method of employing are scientific and reasonable, in preparation process, temperature of reaction and time can effectively control, viscosity, speed, solidifying agent that proportioning is moderate can be obtained, substantially improve moisture absorption and the fragility of aliphatic cyclic amine self, improve its sticking power, adhesive property and solvent resistance etc.
Embodiment
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
A kind of modified epoxy aliphatic cyclic amine high-performance solidifying agent, comprises the raw material of following weight part:
20-40 part isophorone diamine, 30-45 part phenylcarbinol, 8-15 part 1,3-hexamethylene dimethylamine (1,3BAC), 30-38 part N-aminoethyl piperazine (N-AEP), 10-20 part Amino Terminated polyether(ATPE) (D-230), 10-35 part epoxy resin (E-51).Described Amino Terminated polyether(ATPE) viscosity is low, colourless, and good with epoxy resin compatibility, working life is long, and bonding strength is high.Isophorone diamine described above, phenylcarbinol, 1,3-hexamethylene dimethylamine, N-aminoethyl piperazine, Amino Terminated polyether(ATPE), epoxy resin are raw material conventional on market, and those skilled in the art should know, so place repeats no more.
Modified epoxy aliphatic cyclic amine high-performance solidifying agent of the present invention, has stable performance, bland feature, is embodied in: transparent color and luster, heat resistance can reach 120-150 DEG C, shore hardness reaches 80-85D, adhesion 1 grade, alcohol resistance nondiscoloration in 15 days, shearing resistance 12-16Mpa etc., it can be widely used in high bake type color inhibition glass lacquer, normal temperature self-drying type glass lacquer, solvent-resisting, high adhesive force bottle paint, sizing agent, the fields such as transparent yellowing-resistant electronics embedding.
In order to understand the present invention further, below in conjunction with embodiment, the preparation method to modified epoxy aliphatic cyclic amine high-performance solidifying agent provided by the invention is described, and protection scope of the present invention is not limited by the following examples.
Embodiment one
The preparation method of a kind of modified epoxy aliphatic cyclic amine high-performance solidifying agent described in the present embodiment, comprises the steps:
S1: add 20 grams of isophorone diamines successively at reactor, 40 grams of phenylcarbinols, 15 gram of 1,3-hexamethylene dimethylamine, 30 grams of N-aminoethyl piperazines, 15 grams of Amino Terminated polyether(ATPE)s, stir after mixing;
S2: the vacuum pipe of access band negative pressure in described reactor, be at the uniform velocity added drop-wise in described reactor by control valve by 35 grams of epoxy resin and concentrate reaction, temperature of reaction controls at 75 DEG C by ON cycle water coolant simultaneously, and time for adding controls at 35 minutes;
S3: the material in described reactor is concentrated reaction maintenance 3 hours, close described recirculated cooling water, until temperature is cooled to 55 DEG C of vacuum pumping blowings.
The pressure of the vacuum pipe in described step S2 is-0.08Mpa.
With thermometer in described step S2 and step S3.The temperature in described reactor can be observed by thermometer intuitively, be convenient to the operation that staff carries out next step.
Stirred by agitator in described step S1.Preferably the stirring velocity of described agitator is 150 revs/min.
In the present embodiment, when proportioning each raw material, employing gram is unit, in actual production or experimentation, the measure units such as the amount of each raw material can also adopt kilogram weigh, specifically can determine according to the demand of the capacity of reactor and reality, as long as meet the weight ratio relation between each raw material, following examples in like manner to adopt gram as unit.
Embodiment two
The preparation method of a kind of modified epoxy aliphatic cyclic amine high-performance solidifying agent described in the present embodiment, comprises the steps:
S1: add 30 grams of isophorone diamines successively at reactor, 45 grams of phenylcarbinols, 8 gram of 1,3-hexamethylene dimethylamine, 35 grams of N-aminoethyl piperazines, 20 grams of Amino Terminated polyether(ATPE)s, stir after mixing;
S2: the vacuum pipe of access band negative pressure in described reactor, be at the uniform velocity added drop-wise in described reactor by control valve by 10 grams of epoxy resin and concentrate reaction, temperature of reaction controls at 80 DEG C by ON cycle water coolant simultaneously, and time for adding controls at 40 minutes;
S3: the material in described reactor is concentrated reaction maintenance 3 hours, close described recirculated cooling water, until temperature is cooled to 50 DEG C of vacuum pumping blowings.
Valve tube pressure in described step S2 is-0.08Mpa.
With thermometer in described step S2 and step S3.The temperature in described reactor can be observed by thermometer intuitively, be convenient to the operation that staff carries out next step.
Stirred by agitator in described step S1.Preferably the stirring velocity of described agitator is 150 revs/min.
Embodiment three
The preparation method of a kind of modified epoxy aliphatic cyclic amine high-performance solidifying agent described in the present embodiment, comprises the steps:
S1: add 40 grams of isophorone diamines successively at reactor, 30 grams of phenylcarbinols, 11 gram of 1,3-hexamethylene dimethylamine, 38 grams of N-aminoethyl piperazines, 10 grams of Amino Terminated polyether(ATPE)s, stir after mixing;
S2: the vacuum pipe of access band negative pressure in described reactor, be at the uniform velocity added drop-wise in described reactor by control valve by 21 grams of epoxy resin and concentrate reaction, temperature of reaction controls at 85 DEG C by ON cycle water coolant simultaneously, and time for adding controls at 30 minutes;
S3: the material in described reactor is concentrated reaction maintenance 3 hours, close described recirculated cooling water, until temperature is cooled to 45 DEG C of vacuum pumping blowings.
The pressure of the vacuum pipe in described step S2 is-0.08Mpa.
With thermometer in described step S2 and step S3.The temperature in described reactor can be observed by thermometer intuitively, be convenient to the operation that staff carries out next step.
Stirred by agitator in described step S1.Preferably the stirring velocity of described agitator is 150 revs/min.
By the preparation method of the arbitrary described modified epoxy aliphatic cyclic amine high-performance solidifying agent of embodiment 1-3, a kind of stable performance, bland solidifying agent can be obtained, owing to having transparent color and luster, heat resistance can reach 120-150 DEG C, and shore hardness reaches 80-85D, adhesion 1 grade, alcohol resistance nondiscoloration in 15 days, the features such as shearing resistance 12-16Mpa, make it at two-pack glass lacquer, bottle paint coating, sizing agent, there is good performance in the fields such as electronics embedding.
The preparation method of modified epoxy aliphatic cyclic amine high-performance solidifying agent of the present invention, feed composition proportioning and the preparation method of employing are scientific and reasonable, in preparation process, temperature of reaction and time can effectively control, viscosity, speed, solidifying agent that proportioning is moderate can be obtained, substantially improve moisture absorption and the fragility of aliphatic cyclic amine self, improve its sticking power, adhesive property and solvent resistance etc.
Above-mentioned embodiment is just explained in detail technical scheme of the present invention; the present invention has more than and is only confined to above-described embodiment; those skilled in the art should be understood that; every improvement on basis of the present invention according to above-mentioned principle and spirit, substitute, all should within protection scope of the present invention.
Claims (8)
1. a modified epoxy aliphatic cyclic amine high-performance solidifying agent, is characterized in that, comprises the raw material of following weight part:
20-40 part isophorone diamine, 30-45 part phenylcarbinol, 8-15 part 1,3-hexamethylene dimethylamine, 30-38 part N-aminoethyl piperazine, 10-20 part Amino Terminated polyether(ATPE), 10-35 part epoxy resin.
2. a preparation method for modified epoxy aliphatic cyclic amine high-performance solidifying agent, is characterized in that, comprise the steps:
S1: add 20-40 part isophorone diamine successively at reactor, 30-45 part phenylcarbinol, 8-15 part 1,3-hexamethylene dimethylamine, 30-38 part N-aminoethyl piperazine, 10-20 part Amino Terminated polyether(ATPE), stirs after mixing;
S2: the vacuum pipe of access band negative pressure in described reactor, 10-35 part epoxy resin is at the uniform velocity added drop-wise in described reactor by control valve and concentrates reaction, temperature of reaction controls between 75-85 DEG C by ON cycle water coolant simultaneously, and time for adding controls between 30-40 minute;
S3: the material in described reactor is concentrated reaction maintenance 3 hours, close described recirculated cooling water, until temperature is cooled to vacuum pumping blowing between 45-55 DEG C.
3. the preparation method of modified epoxy aliphatic cyclic amine high-performance solidifying agent as claimed in claim 2, is characterized in that: the pressure of the vacuum pipe in described step S2 is-0.08Mpa.
4. the preparation method of modified epoxy aliphatic cyclic amine high-performance solidifying agent as claimed in claim 3, is characterized in that: the temperature of reaction in described step S2 is 80 DEG C.
5. the preparation method of the modified epoxy aliphatic cyclic amine high-performance solidifying agent as described in as arbitrary in claim 2-4, is characterized in that: the temperature in described step S3 is cooled to 50 DEG C of vacuum pumping blowings.
6. the preparation method of the modified epoxy aliphatic cyclic amine high-performance solidifying agent as described in as arbitrary in claim 2-5, is characterized in that: with thermometer in described step S2 and step S3.
7. the preparation method of the modified epoxy aliphatic cyclic amine high-performance solidifying agent as described in as arbitrary in claim 2-6, be is characterized in that: stirred by agitator in described step S1.
8. the preparation method of modified epoxy aliphatic cyclic amine high-performance solidifying agent as claimed in claim 7, is characterized in that: the stirring velocity of described agitator is 150 revs/min.
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Cited By (10)
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| CN105037297A (en) * | 2015-06-23 | 2015-11-11 | 广东博兴新材料科技有限公司 | Carbonyl-containing modified heterocyclic amine, preparation method and application in multifunctional acrylic ester thereof |
| CN105294996A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105294998A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105294999A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105294994A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105295003A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105295004A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High viscosity curing agent composition |
| CN107602819A (en) * | 2017-08-17 | 2018-01-19 | 湖北绿色家园材料技术股份有限公司 | A kind of low cost, high rigidity, the preparation method of high glaze epoxy stone material surface adhesive curing agent |
| CN108299624A (en) * | 2018-03-12 | 2018-07-20 | 雅安市弘利展化工有限公司 | A kind of epoxy curing agent, composition epoxy resin and preparation method thereof |
| CN111748306A (en) * | 2020-06-17 | 2020-10-09 | 雅安市弘利展化工有限公司 | Curing agent for medical material pouring sealant and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105037297A (en) * | 2015-06-23 | 2015-11-11 | 广东博兴新材料科技有限公司 | Carbonyl-containing modified heterocyclic amine, preparation method and application in multifunctional acrylic ester thereof |
| CN105037297B (en) * | 2015-06-23 | 2017-10-10 | 广东博兴新材料科技有限公司 | It is a kind of containing carboxy-modified polycyclic amines and preparation method thereof and its application in polyfunctional acrylic ester |
| CN105294996A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105294998A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105294999A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105294994A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105295003A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High-viscosity curing agent composition |
| CN105295004A (en) * | 2015-11-14 | 2016-02-03 | 华玉叶 | High viscosity curing agent composition |
| CN107602819A (en) * | 2017-08-17 | 2018-01-19 | 湖北绿色家园材料技术股份有限公司 | A kind of low cost, high rigidity, the preparation method of high glaze epoxy stone material surface adhesive curing agent |
| CN108299624A (en) * | 2018-03-12 | 2018-07-20 | 雅安市弘利展化工有限公司 | A kind of epoxy curing agent, composition epoxy resin and preparation method thereof |
| CN111748306A (en) * | 2020-06-17 | 2020-10-09 | 雅安市弘利展化工有限公司 | Curing agent for medical material pouring sealant and preparation method thereof |
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Application publication date: 20150311 |