CN101508856A - Cashew pnenolic aldehyde amine epoxide resin paint solidifying agent and method for producing the same - Google Patents
Cashew pnenolic aldehyde amine epoxide resin paint solidifying agent and method for producing the same Download PDFInfo
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- CN101508856A CN101508856A CNA2008100335921A CN200810033592A CN101508856A CN 101508856 A CN101508856 A CN 101508856A CN A2008100335921 A CNA2008100335921 A CN A2008100335921A CN 200810033592 A CN200810033592 A CN 200810033592A CN 101508856 A CN101508856 A CN 101508856A
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- solidifying agent
- aldehyde amine
- polyamine
- cardanol
- formaldehyde
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- Phenolic Resins Or Amino Resins (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to a curing agent used for epoxy resin coating and a preparation method thereof. The curing agent has the main component of cardanol-aldehyde amine, and is characterized in that the synthetic formulation of the cardanol-aldehyde amine comprises the following components based on the weight percentage: 60-70% of cardanol, 20-30% of polyamine, 10-20% of formaldehyde or paraformal-dehyde and 1-5% of 2, 4, 6ternary (dimethylamino methyl) phenol. Compared with common phenolic aldehyde amine curing agent, the curing agent has better water resisting property and flexility when being used for the epoxy resin coating, and generally does not affect the color mixing of finishing coat.
Description
Technical field
The present invention relates to synthetic resins and coating industry in the chemical industry field, specifically, relating to a kind of is the Synergist S-421 95 that based coating is used with Resins, epoxy, promptly a kind of cashew pnenolic aldehyde amine hardener.
Background technology
Resins, epoxy is a kind of application synthetic resins very widely, especially uses more general in fields such as coating, tackiness agent.In order to obtain to have the performance of practical value, Resins, epoxy need use solidifying agent to make it crosslinking curing, and at this moment Resins, epoxy has excellent adhesivity, mechanical property, electrical property and resistance to corrosive chemicals.The performance of solidifying agent after to epoxy resin cure has important effect.
What China's present stage use was more is polyamide-based solidifying agent, but the relatively poor shortcomings of mechanical property such as the snappiness of resin, shock-resistance after existing low temperature to be difficult to solidify, solidify.
Domestic also have by Mannich (Mannich) reaction synthetic epoxy resin solidifying agent, but use phenol on raw material mostly, and the disadvantage of its product is that the snappiness after solidifying is relatively poor, more crisp.
In this field, Chinese patent CN 1374292A once reported with cashew shell liquid as reaction phenol, the synthetic epoxy resin solidifying agent, but because the color of raw material is dark excessively, can't in finish paint cooperates, use basically.
Summary of the invention
In view of good with cashew phenol modified solidifying agent low-temperature curing performance, curing speed is fast, and 5 ℃ still can solidify, and has overcome low-molecular-weight polyamide resin and has been difficult to curing below 10 ℃, can not the solidified shortcoming below 5 ℃.Have good snappiness and hypotoxicity, the solidification brittleness problem that has existed when having overcome polyamine and derivative cured epoxy resin thereof, have excellent in water resistance and chemical resistant properties simultaneously, the present inventor improves with keen determination to synthetic work of cashew phenol class solidifying agent, makes it to have better water tolerance and snappiness than general pnenolic aldehyde amine hardener.And do not influence the toning of finish paint substantially.
The present invention is achieved in that its main component is a cashew pnenolic aldehyde amine, it is characterized in that the synthesizing formula of described cashew pnenolic aldehyde amine comprises following component in weight percent:
Cardanol 60～70%;
Polyamine 20～30%;
Formaldehyde or Paraformaldehyde 96 10～20%;
2,4,6 three (dimethylamino methyl) phenol 1～5%.
That is to say, in solidifying agent of the present invention, polyamine can with the epoxy group(ing) generation crosslinking reaction in the Resins, epoxy.Phenolic hydroxyl group has obvious katalysis to curing reaction, and is still like this under low temperature (below 5 ℃).Long chain hydrocarbon groups substituting group on the phenyl ring has good hydrophobic nature and snappiness, has better water tolerance and snappiness than general pnenolic aldehyde amine hardener.And improve the toning that the color that makes product does not influence finish paint substantially by purification, and aspect of performance more is better than the former to raw material.
In above-mentioned cooperation, described polyamine is an aliphatic polyamine, is selected from quadrol, hexanediamine, diethylenetriamine, triethylene tetramine, a kind of in the m-xylene diamine.
According to the present invention, concrete synthetic method is: with cardanol, formaldehyde or Paraformaldehyde 96, polyamine is raw material, makes cashew pnenolic aldehyde amine by Mannich (Mannich) reaction, and building-up process is as follows:
Get cardanol by proportioning, polyamine is after mixing, add the 37 weight % aqueous solution or Paraformaldehyde 96s of formaldehyde, temperature is controlled at 55～60 ℃ in batches, and the time of adding is 0.5～1.0 hour, add 2,4 subsequently, 6-three (dimethylamino methyl) phenol, be warming up to 70～80 ℃, be incubated 3～5 hours, vacuum hydro-extraction, 70～80 ℃ of temperature, the highlyest be no more than 90 ℃, vacuum degree control is more than 720～740mmHg, and dehydration is till anhydrous the steaming.
The specific performance index of the cashew pnenolic aldehyde amine hardener that makes by the present invention is as follows:
Outward appearance: light viscous liquid;
Solid content: 95～99%;
Amine value: 250～500mgKOH/g;
Reactive hydrogen number: 3;
Viscosity: 3000～12000mPas;
Purity: 〉=99%.
This cashew pnenolic aldehyde amine hardener is used to prepare epoxy anti-rust paint, obtains good result, its shock strength 50kgcm, 1 grade of sticking power, in salt solution, soak a few hours non-foaming, do not expand, nonbleeding, hardness 1H～2H.
Embodiment
With embodiment the present invention is further described in detail below, but the present invention is in no way limited to these embodiment.
Embodiment 1
On a 500ml reaction flask, equipment agitator, condenser, water trap, thermometer add cardanol 150 grams, quadrol 30 grams from charging opening, stir, add Paraformaldehyde 96 15 grams in batches, temperature is controlled at below 60 ℃, 0.5 hour joining day, add 2,4, be warmed up to 70～80 ℃ behind 6-three (dimethylamino methyl) phenol 2 grams, be incubated 4 hours, carry out vacuum (more than the vacuum tightness 740mmHg) dehydration then, the highlyest be no more than 90 ℃, dehydration is till anhydrous the steaming.Product is that faint yellow viscous liquid, solid content are 96%, amine value 300mgKOH/g, 3 of reactive hydrogen numbers, viscosity 7000mPas, purity 99%.
Embodiment 2
Device adds cardanol 150 grams, diethylenetriamine 41.2 grams with embodiment 1, stirs, add 37 weight % formalins, 32.8 grams in batches, temperature is controlled at below 60 ℃, 0.5 hour joining day, adds 2,4, be warmed up to 70～80 ℃ behind 6-three (dimethylamino methyl) phenol 2.5 grams, be incubated 3 hours, carry out vacuum (more than the vacuum tightness 740mmHg) dehydration then, dehydration temperaturre is 70～80 ℃, and dehydration is till anhydrous the steaming.Product is that dark yellow viscous liquid, solid content are 96%, amine value 380mgKOH/g, 3 of reactive hydrogen numbers, viscosity 5000mPas, purity 99.5%.
Embodiment 3
Device adds cardanol 150 grams, m-xylene diamine 47.6 grams with embodiment 1, stirs, add 37 weight % formalins, 28.7 grams, temperature is controlled at below 60 ℃, 0.5 hour joining day in batches, add 2,4, be warmed up to 70～80 ℃ behind 6-three (dimethylamino methyl) phenol 2.8 grams, be incubated 3 hours, carry out vacuum hydro-extraction then, dehydration temperaturre is 70～80 ℃, and more than the vacuum tightness 740mmHg, dehydration is till anhydrous the steaming.Product is that yellow viscous liquid, solid content 97.7 are %, amine value 250mgKOH/g, 3 of reactive hydrogen numbers, viscosity 10000mPas, purity 99.2%.
Embodiment 4
Device adds cardanol 150 grams, hexanediamine 52.2 grams with embodiment 1, stirs, add Paraformaldehyde 96 13.5 grams, temperature is controlled at below 60 ℃, 0.5 hour joining day in batches, add 2,4, be warmed up to 70～80 ℃ again behind 6-three (dimethylamino methyl) phenol 3 grams, be incubated 4 hours, carry out vacuum hydro-extraction then, dehydration temperaturre is 70～80 ℃, and more than the vacuum tightness 740mmHg, dehydration is till anhydrous the steaming.Product is that garnet viscous liquid, solid content are 95%, amine value 280mgKOH/g, 3 of reactive hydrogen numbers, viscosity 8000mPas, purity 99.4%.
Embodiment 5
Device adds cardanol 150 grams, triethylene tetramine 65.7 grams with embodiment 1, stirs, add 37 weight % formalins, 72.9 grams, temperature is controlled at below 60 ℃, 0.5 hour joining day in batches, add 2,4, be warmed up to 70～80 ℃ behind 6-three (dimethylamino methyl) phenol 3.5 grams, be incubated 3 hours, carry out vacuum hydro-extraction then, dehydration temperaturre is 70～80 ℃, and more than the vacuum tightness 740mmHg, dehydration is till anhydrous the steaming.Product is that filbert viscous liquid, solid content are 96%, amine value 500mgKOH/g, 3 of reactive hydrogen numbers, viscosity 3000mPa, purity 99.9%.
Claims (3)
1, a kind of epoxide resin paint solidifying agent that is used for, main component is a cashew pnenolic aldehyde amine, it is characterized in that, the synthesizing formula of described cashew pnenolic aldehyde amine comprises following component in weight percent:
Cardanol 60～70%;
Polyamine 20～30%;
Formaldehyde or Paraformaldehyde 96 10～20%;
2,4,6 three (dimethylamino methyl) phenol 1～5%.
2, epoxypaint solidifying agent according to claim 1 is characterized in that described polyamine is an aliphatic polyamine, is selected from quadrol, hexanediamine, diethylenetriamine, triethylene tetramine, a kind of in the m-xylene diamine.
3, a kind of according to the preparation method of the described epoxypaint of claim 1 with solidifying agent, it is characterized in that whole preparation manipulation process is as follows:
Get cardanol by proportioning, polyamine after mixing, adds formaldehyde or Paraformaldehyde 96 in batches, and described here formaldehyde is the 37 weight % aqueous solution of formaldehyde, and temperature is controlled at 55～60 ℃, and the time of adding is 0.5～1.0 hour; Add 2,4 subsequently, 6-three (dimethylamino methyl) phenol is warming up to 70～80 ℃, is incubated 3～5 hours, vacuum hydro-extraction, and 70～80 ℃ of temperature the highlyest are no more than 90 ℃, and vacuum degree control is 720～740mmHg, and dehydration is till anhydrous the steaming.
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| CN2008100335921A CN101508856B (en) | 2008-02-13 | 2008-02-13 | Cashew pnenolic aldehyde amine epoxide resin paint solidifying agent and method for producing the same |
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| CN101508856B CN101508856B (en) | 2011-04-13 |
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