CN104497274A - Modified polyamide epoxy curing agent and preparation method thereof - Google Patents
Modified polyamide epoxy curing agent and preparation method thereof Download PDFInfo
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- CN104497274A CN104497274A CN201410757291.9A CN201410757291A CN104497274A CN 104497274 A CN104497274 A CN 104497274A CN 201410757291 A CN201410757291 A CN 201410757291A CN 104497274 A CN104497274 A CN 104497274A
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- polyamide epoxy
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Abstract
The invention discloses a modified polyamide epoxy curing agent. The modified polyamide epoxy curing agent is prepared from the following raw materials in parts by weight: 20-60 parts of poly-fatty acid, 8-35 parts of vegetable oil acids, 12-38 parts of fatty amine, 15-35 parts of ketones, 0.01-0.02 parts of terminator and 8-30 parts of cardanol. The modified polyamide epoxy curing agent disclosed by the invention is high in viscosity, fast in curing speed, moderate in proportion, capable of reducing cost and greatly improving the defect of incomplete low-temperature curing of the existing polyamide, good in low-temperature resistance, high-humidity resistance and solvent resistance, and capable of improving the adhesion force, and the toughness of the cured object.
Description
Technical field
The present invention relates to solidifying agent preparing technical field, relate to a kind of modified polyamide epoxy hardener and preparation method thereof specifically.
Background technology
Daiamid epoxy curing agent has good physical and chemical performance and physical construction performance compared with other solidifying agent, therefore be widely used in industries such as machinery, electrical equipment, petrochemical complex, aviation, boats and ships, buildings, instrument, semiconducter device and Communication Equipment are also had to the application of wide model.Due to formula and the difference of manufacturing process, there is color and luster, viscosity, curing speed, volatility, toxicity, the toughness of cured article, the deficiency of electric property aspect more in existing daiamid epoxy curing agent product.
Summary of the invention
The technical problem to be solved in the present invention is that to overcome existing daiamid epoxy curing agent transparent color and luster degree lower, the drawback that the toughness of viscosity, curing speed, cured article, sticking power and solvent resistance are poor, and then a kind of modified polyamide epoxy hardener and preparation method thereof is provided.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of modified polyamide epoxy hardener, it comprises the raw material of following weight part: poly lipid acid 20-60 part, vegetable oil acid 8-35 part, aliphatic amide 12-38 part, ketone 15-35 part, terminator 0.01-0.02 part, cardanol 8-30 part.
Preferably, the weight part of each raw material is: poly lipid acid 30-50 part, vegetable oil acid 15-25 part, aliphatic amide 20-30 part, ketone 20-30 part, terminator 0.01-0.02 part, cardanol 15-20 part.
Preferably, the weight part of each raw material is: 40 parts, poly lipid acid, vegetable oil acid 21.5 parts, aliphatic amide 25 parts, ketone 25 parts, terminator 0.015 part, cardanol 19 parts.
Preferably, described poly lipid acid is dimer (fatty acid) yl or trimerized fatty acids.
Preferably, described vegetable oil acid is ricinolic acid or cotton oil acid or vegetable seed oleic acid or behenic acid.
Preferably, described aliphatic amide is quadrol or diethylenetriamine or triethylene tetramine or tetraethylene pentamine or mixed amine.
Preferably, described mixed amine is two or more mixing in N-aminoethyl ethanolamine, aminoethyl piperazine, triethylene tetramine.
Preferably, described ketone is acetone or butanone or pimelinketone or methyl iso-butyl ketone (MIBK) or methyl isopropyl Ketone or methylethylketone or pimelinketone or methyl phenyl ketone.
Preferably, described terminator is quinone or nitro polyol or nitroso-group polyol or aryl polyol or boric acid.
Prepare a method for the modified polyamide epoxy hardener described in above-mentioned any one, it comprises the following steps:
(1) according to described weight raw material;
(2) add poly lipid acid, vegetable oil acid and aliphatic amide in a kettle., then mixture is stirred 30-80 minute;
(3) be then warmed up to dehydration, continue to be heated to 180-300 DEG C, and keep reaction 1.5-5 hour;
(4) reactor is cooled to 100-130 DEG C, and adds ketone, then temperature rising reflux 2-10 hour;
(5) backflow reheats recovery free ketone after terminating, and after keeping 1-2 hour at 150-250 DEG C, be cooled to 180-200 DEG C to add terminator, then vacuumize, vacuum tightness reaches-0.08MPa ~-0.1MPa, and keeps 0.5-3 hour;
(6) reactor is cooled to 80-100 DEG C, adds cardanol mixing and stirring blowing, obtain modified polyamide epoxy hardener.
Adopt technique scheme, the present invention at least comprises following beneficial effect:
1. modified polyamide epoxy hardener of the present invention has that viscosity is strong, curing speed is fast, proportioning is moderate can reduce costs, and substantially improve the incomplete defect of existing polymeric amide low-temperature curing, there is the moist and solvent resistance of good lower temperature resistance, resistance to height, and improve the toughness of its sticking power, cured article.
2. the method for the preparation of modified polyamide epoxy hardener of the present invention temperature of reaction and reaction times in preparation process can effectively control, and operation is simple and reliable, the modified polyamide epoxy hardener reliable in quality produced.
Embodiment
Embodiment one
A kind of modified polyamide epoxy hardener, it comprises following raw material: 20 grams, poly lipid acid, vegetable oil acid 8 grams, aliphatic amide 13 grams, ketone 15 grams, terminator 0.01 gram, cardanol 8 grams.
Wherein, described poly lipid acid is the one in dimer (fatty acid) yl or trimerized fatty acids or other poly lipid acid; Vegetable oil acid is the one in ricinolic acid, cotton oil acid, vegetable seed oleic acid or behenic acid; Aliphatic amide is quadrol, one in diethylenetriamine, triethylene tetramine, tetraethylene pentamine, polyethylene polyamine or mixed amine (described mixed amine is two or more mixing in N-aminoethyl ethanolamine, aminoethyl piperazine, triethylene tetramine or polyethylene polyamine); Ketone is the one in acetone, butanone, pimelinketone, methyl iso-butyl ketone (MIBK), methyl isopropyl Ketone, methylethylketone, pimelinketone or methyl phenyl ketone; Terminator is the one in quinone, nitro polyol, nitroso-group polyol, aryl polyol or boric acid.
Prepare a method for described modified polyamide epoxy hardener, it comprises the following steps:
(1) according to each raw material of above-mentioned weight proportion, the weight unit of above-mentioned each raw material is gram, in actual proportioning process, can change according to the capacity of reactor and the need of production proportion relation according to above-mentioned each raw material, as, all with kilogram or Dun Zuo unit (following embodiment in like manner);
(2) add poly lipid acid, vegetable oil acid and aliphatic amide in a kettle., then mixture is stirred 30-80 minute;
(3) then the temperature of temperature reaction still, to dehydration, continues to be heated to the temperature value between 180-300 DEG C, and keeps reaction 1.5-5 hour;
(4) reactor is cooled to 100-130 DEG C, and adds ketone, then temperature rising reflux 2-10 hour;
(5) backflow reheats recovery free ketone after terminating, and after keeping 1-2 hour at 150-250 DEG C, be cooled to 180-200 DEG C to add terminator, then vacuumize, vacuum tightness reaches-0.08MPa ~-0.1MPa, and keeps 0.5-3 hour;
(6) reactor is cooled to 80-100 DEG C, adds cardanol mixing and stirring blowing, obtain modified polyamide epoxy hardener.
The modified polyamide epoxy hardener of the present embodiment has that viscosity is strong, curing speed is fast, proportioning is moderate can reduce costs, and substantially improve the incomplete defect of existing polymeric amide low-temperature curing, there is the moist and solvent resistance of good lower temperature resistance, resistance to height, and improve the toughness of sticking power and its cured article.
Embodiment two
In the present embodiment, in modified polyamide epoxy hardener, the proportioning of each raw material is: 60 grams, poly lipid acid, vegetable oil acid 8 grams, aliphatic amide 13 grams, ketone 15 grams, terminator 0.015 gram, cardanol 8 grams.
The preparation method of described modified polyamide epoxy hardener is identical with embodiment one.
Embodiment three
In the present embodiment, in modified polyamide epoxy hardener, the proportioning of each raw material is: 45 grams, poly lipid acid, vegetable oil acid 20 grams, aliphatic amide 38 grams, ketone 30 grams, terminator 0.01 gram, cardanol 30 grams.
The preparation method of described modified polyamide epoxy hardener is identical with embodiment one.
Embodiment four
In the present embodiment, in modified polyamide epoxy hardener, the proportioning of each raw material is: 30 grams, poly lipid acid, vegetable oil acid 15 grams, aliphatic amide 30 grams, ketone 28 grams, terminator 0.02 gram, cardanol 15 grams.
The preparation method of described modified polyamide epoxy hardener is identical with embodiment one.
Embodiment five
In the present embodiment, in modified polyamide epoxy hardener, the proportioning of each raw material is: 50 grams, poly lipid acid, vegetable oil acid 25 grams, aliphatic amide 21 grams, ketone 20 grams, terminator 0,015 gram, cardanol 20 grams.
The preparation method of described modified polyamide epoxy hardener is identical with embodiment one.
Embodiment six
In the present embodiment, in modified polyamide epoxy hardener, the proportioning of each raw material is: 40 grams, poly lipid acid, vegetable oil acid 21.5 grams, aliphatic amide 25 parts, ketone 25 parts, terminator 0.015 part, cardanol 19 parts.
The preparation method of described modified polyamide epoxy hardener is identical with embodiment one.
The proportion relation of each raw material in above-described embodiment 1-6 all can produce that viscosity is strong, curing speed is fast, proportioning is moderate can reduce costs, and substantially improve the incomplete defect of existing polymeric amide low-temperature curing, there is the moist and solvent resistance of good lower temperature resistance, resistance to height, and improve the toughness of sticking power and its cured article.
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 (10)
1. a modified polyamide epoxy hardener, is characterized in that, comprises the raw material of following weight part:
Poly lipid acid 20-60 part, vegetable oil acid 8-35 part, aliphatic amide 12-38 part, ketone 15-35 part, terminator 0.01-0.02 part, cardanol 8-30 part.
2. a kind of modified polyamide epoxy hardener according to claim 1, is characterized in that, comprise the raw material of following weight part:
Poly lipid acid 30-50 part, vegetable oil acid 15-25 part, aliphatic amide 20-30 part, ketone 20-30 part, terminator 0.01-0.02 part, cardanol 15-20 part.
3. a kind of modified polyamide epoxy hardener according to claim 2, is characterized in that, comprise the raw material of following weight part:
40 parts, poly lipid acid, vegetable oil acid 21.5 parts, aliphatic amide 25 parts, ketone 25 parts, terminator 0.015 part, cardanol 19 parts.
4. a kind of modified polyamide epoxy hardener according to claim 1, is characterized in that, described poly lipid acid is dimer (fatty acid) yl or trimerized fatty acids.
5. a kind of modified polyamide epoxy hardener according to claim 1, is characterized in that, described vegetable oil acid is ricinolic acid or cotton oil acid or vegetable seed oleic acid or behenic acid.
6. a kind of modified polyamide epoxy hardener according to claim 1, is characterized in that, described aliphatic amide is quadrol or diethylenetriamine or triethylene tetramine or tetraethylene pentamine or mixed amine.
7. a kind of modified polyamide epoxy hardener according to claim 6, is characterized in that, described mixed amine is two or more mixing in N-aminoethyl ethanolamine, aminoethyl piperazine, triethylene tetramine.
8. a kind of modified polyamide epoxy hardener according to claim 1, is characterized in that, described ketone is acetone or butanone or pimelinketone or methyl iso-butyl ketone (MIBK) or methyl isopropyl Ketone or methylethylketone or pimelinketone or methyl phenyl ketone.
9. a kind of modified polyamide epoxy hardener according to claim 1, is characterized in that, described terminator is quinone or nitro polyol or nitroso-group polyol or aryl polyol or boric acid.
10. prepare a method for the modified polyamide epoxy hardener described in any one of claim 1-9, it is characterized in that, comprise the following steps:
(1) according to described weight raw material;
(2) add poly lipid acid, vegetable oil acid and aliphatic amide in a kettle., then mixture is stirred 30-80 minute;
(3) be then warmed up to dehydration, continue to be heated to 180-300 DEG C, and keep reaction 1.5-5 hour;
(4) reactor is cooled to 100-130 DEG C, and adds ketone, then temperature rising reflux 2-10 hour;
(5) backflow reheats recovery free ketone after terminating, and after keeping 1-2 hour at 150-250 DEG C, be cooled to 180-200 DEG C to add terminator, then vacuumize, vacuum tightness reaches-0.08MPa ~-0.1MPa, and keeps 0.5-3 hour;
(6) reactor is cooled to 80-100 DEG C, adds cardanol mixing and stirring blowing, obtain modified polyamide epoxy hardener.
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| CN201410757291.9A CN104497274A (en) | 2014-12-12 | 2014-12-12 | Modified polyamide epoxy curing agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353828A (en) * | 2017-06-13 | 2017-11-17 | 中油佳汇防水科技（深圳）股份有限公司 | The ultralow uncured rubber asphalt waterproof coating of temperature spraying |
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2014
- 2014-12-12 CN CN201410757291.9A patent/CN104497274A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353828A (en) * | 2017-06-13 | 2017-11-17 | 中油佳汇防水科技（深圳）股份有限公司 | The ultralow uncured rubber asphalt waterproof coating of temperature spraying |
| CN107353828B (en) * | 2017-06-13 | 2019-11-29 | 中油佳汇防水科技（深圳）股份有限公司 | The ultralow uncured rubber asphalt waterproof coating of temperature spraying |
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Application publication date: 20150408 |