CN103044659A - Preparation of novel epoxy hardener - Google Patents
Preparation of novel epoxy hardener Download PDFInfo
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- CN103044659A CN103044659A CN2012104558183A CN201210455818A CN103044659A CN 103044659 A CN103044659 A CN 103044659A CN 2012104558183 A CN2012104558183 A CN 2012104558183A CN 201210455818 A CN201210455818 A CN 201210455818A CN 103044659 A CN103044659 A CN 103044659A
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Abstract
The invention discloses the preparation of novel epoxy hardener B77. The preparation of the novel epoxy hardener B77 comprises the following main preparation steps: adding 4,4'-diaminodiphenylmethane to a reaction kettle, heating, starting to add formaldehyde solution and phenol in a dropwise manner when the temperature is 80-130 DEG C (preferably 90-105 DEG C), keeping the temperature after finishing charging, heating and carrying out vacuum dehydration at 130-200 DEG C (preferably 150-175 DEG C), and analyzing that the content of phenol is smaller than 2%; cooling down and controlling after an analyzed result is qualified, starting to add benzyl alcohol in a dropwise manner when the temperature is 60-150 DEG C (preferably 75-115 DEG C) till an amine value is 240-280 and is qualified, cooling down to 60 DEG C after the amine value is qualified, keeping the temperature for half an hour, and discharging to obtain black viscous liquid as the epoxy hardener B77, wherein the moisture of the black viscous liquid is analyzed to be smaller than 0.2%, and the viscosity of the black viscous liquid at 23 DEG C is 386mPas. The preparation of the novel epoxy hardener, disclosed by the invention, has the advantages of simple and clear process, high yield, small emission of three wastes, strong practicability and wide application range, and is worth of being promoted and recommended; and the prepared epoxy hardener has corrosion and heat resistances, and has a large application value and a certain remarkable economic benefit when being taken as a modified epoxy coating.
Description
Technical field
The preparation of a kind of Novel Curing Agents for Epoxy Resins B77 of the present invention, aromatic amine curing agent belongs to the fine chemicals industry, is subdivided into the coatings additive(s) classification, specifically adds as modified epoxy coating.
Background technology
The organic polyamine class compound of epoxy curing agent.Single polyamines is arranged, mix polyamines, modified polyamine and congruent melting mixing polyamines four classes.Single polyamines mainly is four kinds of aliphatic amide, aliphatic cyclic amine, aromatic amine and polymeric amide.Aliphatic amide and polymeric amide are the self-vulcanizing agent; And aromatic amine need be heating and curing, and its cured article thermotolerance, physical strength and erosion resistance are much better than aliphatic amide.With regard to thermotolerance, best is aromatic amine curing agent, secondly is aliphatic cyclic amine, and the poorest is polymeric amide.Aliphatic amide has larger toxicity and pungency, and the aromatic amine solidification value is higher, all need give modification, so multiple modified polyamine occurred, such as epoxide addition polyamines, Michael addition polyamines, arylamine blend etc.The invention reside in the preparation a kind of thermotolerance preferably aromatic amine curing agent solve the heat-resisting problem of modified epoxy coating.
Summary of the invention
The preparation of a kind of epoxy hardener B77 of the present invention mainly is that preparation one black thick liquid epoxy hardener B77 is that structural formula is as follows:
Main component be and than row as described in the following table:
Its preparation process is as follows: with 4, begin to drip formalin and phenol at 80 ~ 130 ℃ (preferred 90-105 ℃) behind the heat temperature raising in the 4'-diaminodiphenylmethane adding reactor, insulation behind reinforced the end, then heat up in 130 ~ 200 ℃ (preferred 150-175 ℃) lower vacuum hydro-extraction, analysis of Phenol content should be less than 2%; Analyze qualified rear cooling control 60 ~ 150 ℃ (preferred 75-115 ℃) and begin to drip phenylcarbinol, until the amine value reaches 240 ~ 280 qualified, be cooled to 60 ℃ after qualified, insulation half an hour, it is product that blowing obtains the black thick liquid.Its reaction process schema as shown in Figure 1.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
The below elaborates with regard to implementation.
Embodiment
As shown in Figure 1, with kilogram 4, the 4'-diaminodiphenylmethane drops into reactor, and first steam heats up, and rear thermal oil is warming up to 80 ~ 110 ℃, makes its dissolving.Be cooled to 90 ℃, drip kilogram phenol, dripped off in 1 hour, the reaction process heat release need be opened water coolant.Be incubated 1 hour, temperature is controlled at temperature and is controlled at 95 ~ 105 ℃.Be warming up to 150 ℃, dewatered 1 hour, drive vacuum pump, vacuum tightness is 0.08 ~ 0.09MPa, and dehydration temperaturre is take 165 ~ 170 ℃ as good.Open the nitrogen pressurize, sampling, analysis of Phenol content should less than 2%, be cooled to 100 ℃ during sampling.
Analyzing and be cooled to 80 ℃ after qualified, drip phenylcarbinol, should divide 2 dropping, be 1580kg for the first time, is that 80kg(also can divide 2 times the second time for the second time).Open the nitrogen pressurize, sampling analysis, the amine value is qualified 240 ~ 280, as surpasses, and can continue in accordance with regulations to drip phenylcarbinol.Analyze and be cooled to 60 ℃ after qualified, insulation half an hour, blowing obtains a kilogram black thick liquid, moisture during less than 0.2%, 23 ℃ viscosity be 386mPas.
Claims (4)
1. the preparation of a Novel Curing Agents for Epoxy Resins B77 is primarily characterized in that: epoxy hardener B77 is a black thick liquid, and structural formula is as follows:
Main component be and than row as described in the following table:
2. the according to claim 1 preparation of described Novel Curing Agents for Epoxy Resins B77, be primarily characterized in that its preparation process is as follows: with 4, begin to drip formalin and phenol behind the heat temperature raising in the 4'-diaminodiphenylmethane adding reactor, insulation behind reinforced the end, the dehydration that then heats up is analyzed and is cooled to certain temperature after qualified and begins to drip phenylcarbinol, until the amine value is qualified, be cooled to 60 ℃ after qualified, be incubated half an hour, it is product that blowing obtains the black thick liquid.
3. the according to claim 1 and 2 preparation of described Novel Curing Agents for Epoxy Resins B77 is primarily characterized in that: the temperature that drips formalin and phenol and insulation is 80 ~ 130 ℃ (preferred 90-105 ℃); The temperature of vacuum hydro-extraction is 130 ~ 200 ℃ (preferred 150-175 ℃); The temperature that begins to drip phenylcarbinol is 60 ~ 150 ℃ (preferred 75-115 ℃).
4. be primarily characterized in that according to claim 1 and 2 or the preparation of 3 described Novel Curing Agents for Epoxy Resins B77: analyze be cooled to after qualified certain temperature begin to drip phenylcarbinol wherein analyze the qualified analysis of Phenol content that refers to should be less than 2%; Drip phenylcarbinol until the amine value is qualified, wherein the qualified amine value that refers to of amine value is 240 ~ 280.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210455818.3A CN103044659B (en) | 2012-11-14 | 2012-11-14 | Preparation of novel epoxy hardener |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210455818.3A CN103044659B (en) | 2012-11-14 | 2012-11-14 | Preparation of novel epoxy hardener |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103044659A true CN103044659A (en) | 2013-04-17 |
| CN103044659B CN103044659B (en) | 2015-04-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210455818.3A Expired - Fee Related CN103044659B (en) | 2012-11-14 | 2012-11-14 | Preparation of novel epoxy hardener |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101096411A (en) * | 2006-06-29 | 2008-01-02 | 气体产品与化学公司 | Curing agent for epoxy resin and coating composition |
| CN101508764A (en) * | 2009-03-13 | 2009-08-19 | 胡高平 | High-performance pnenolic aldehyde amine hardener for epoxy resin and preparation thereof |
| CN102134306A (en) * | 2011-03-04 | 2011-07-27 | 广东工业大学 | Cardanol epoxy floor curing agent and preparation method thereof |
| JP2011168671A (en) * | 2010-02-17 | 2011-09-01 | Jfe Chemical Corp | Thermosetting resin composition and cured product thereof |
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2012
- 2012-11-14 CN CN201210455818.3A patent/CN103044659B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101096411A (en) * | 2006-06-29 | 2008-01-02 | 气体产品与化学公司 | Curing agent for epoxy resin and coating composition |
| CN101508764A (en) * | 2009-03-13 | 2009-08-19 | 胡高平 | High-performance pnenolic aldehyde amine hardener for epoxy resin and preparation thereof |
| JP2011168671A (en) * | 2010-02-17 | 2011-09-01 | Jfe Chemical Corp | Thermosetting resin composition and cured product thereof |
| CN102134306A (en) * | 2011-03-04 | 2011-07-27 | 广东工业大学 | Cardanol epoxy floor curing agent and preparation method thereof |
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| CN103044659B (en) | 2015-04-15 |
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Granted publication date: 20150415 Termination date: 20181114 |