CN103289059B - Low colourity, low viscosity natural phant cardanol solidifying agent of epoxy resin - Google Patents
Low colourity, low viscosity natural phant cardanol solidifying agent of epoxy resin Download PDFInfo
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- CN103289059B CN103289059B CN201210042725.8A CN201210042725A CN103289059B CN 103289059 B CN103289059 B CN 103289059B CN 201210042725 A CN201210042725 A CN 201210042725A CN 103289059 B CN103289059 B CN 103289059B
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- cardanol
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- paraformaldehyde
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Abstract
The present invention is the synthetic method of a kind of low colourity, low viscous natural phant cashew pnenolic aldehyde amine epoxy curing agent, be raw material with natural phant cardanol, tetraethylene pentamine and paraformaldehyde, under tea-polyphenol acid series catalysts participates in, complete ternary polycondensation synthesis, then vacuum hydro-extraction.By iron cobalt colorimeter quantitative measurment colourity, by digital display viscometer quantitative measurment viscosity.The cured article (paint film) that the supporting epoxy resin ink of this solidifying agent and coating are formed, has good adhesive fastness, mechanical property and chemical resistance with base material.
Description
Technical field
The present invention relates to native biopolymer technical field, product application is in ink, coating, binding agent industry, specifically, the ink produced using epoxy resin as filmogen, coating, binding agent, using the cashew pnenolic aldehyde amine of natural phant cardanol synthesis as solidifying agent, the macromolecular solid compound (paint film) that interlinkage reaction is formed, has good adhesive fastness, mechanical property and chemical resistance with substrate surface.
Background technology
Epoxy resin self is the linear structure thing with two or more reactive epoxy groups, a kind of thermoplastic semifinished products, it must be supporting used in combination with solidifying agent, make epoxy ring-opening, with the amino generation interlinkage of solidifying agent, form the macromolecular solid compound that three dimensional stereo is netted, just there is premium properties and embody practical function.Conventional epoxy curing agent has fatty amine curing agent, polyamide curing agent, pnenolic aldehyde amine hardener, polyurethane curing agent etc., inputs cashew nut oil modified amine hardener again in recent years from the U.S..Comparing result shows, the comprehensive result of use of cashew nut oil modified amine hardener is best.Chinese patent CN101508856A, CN101319042A and CN101333286A report title, be raw material with natural phant cardanol, polyamine, formaldehyde, the cashew pnenolic aldehyde amine synthesized, lighter color, denseness is low, it is the phase jljl of the cashew nut oil modified amine hardener of the U.S., but there is no the quantitative assay of colourity and viscosity, the product that actual market is collected, with iron cobalt colorimetric measurements, colourity, all between 10 to 18, is all the red-brown thick liquid that viscosity is high.The invention provides the preparation method of a kind of low colourity, low viscosity natural phant cardanol solidifying agent of epoxy resin, and its colourity of quantitative assay and viscosity, overcome in existing solidifying agent technology cause because colourity is not low finish paint not easily mix colours and not low the causing of viscosity brush not easily levelling two difficult problems, and paint film and substrate surface have good adhesive fastness, mechanical property and chemical resistance.
Summary of the invention
The present invention with natural phant cardanol, tetraethylene pentamine, paraformaldehyde for raw material, with tea-polyphenol acid series catalysts, complete ternary polycondensation, principal product natural phant cashew pnenolic aldehyde amine, by product generates water, through vacuum hydro-extraction, finally obtains pure plant cashew pnenolic aldehyde amine liquid, target product-epoxy curing agent of the present invention just, reaction equation is as follows:
Embodiment:
On a 1000ml tetra-mouthfuls of glass reaction stills (flask), agitator, widely different flow condenser, direct current condenser, thermometer, nitrogen inlet and charging opening are housed.Under the stirring velocity of 80 revs/min, natural phant cardanol is added in molar ratio by charging opening, tetraethylene pentamine, paraformaldehyde, mol ratio is 1.0-1.2: 08-1.0: 0.7-1.0, tea-polyphenol acid series catalysts consumption is the 2-5% of material gross weight, cardanol purity >=99%, tetraethylene pentamine purity >=90%, paraformaldehyde purity >=95%, logical nitrogen deoxygenation in still, widely different flow condenser ice water circulation, 145 ± 1 DEG C are warming up in still, be incubated about 1 hour, until the paraformaldehyde pressed powder completely dissolve in still, in still, liquid is muddy shape, represent that ternary polycondensation completes.Then, implement vacuum hydro-extraction, close nitrogen inlet, close widely different flow condenser, connect direct current condenser, be not less than under the stirring velocity of 1000 revs/min, connecting vacuum pump and vacuumize, until the vacuum tightness in still reaches-0.098MPa, water flows into measuring container through direct current condenser, when aquifer yield reaches 80% of theoretical aquifer yield, in reactor, turbid solution becomes transparent liquid, terminates vacuum hydro-extraction.
Synthetic product after vacuum hydro-extraction is faint yellow transparent liquid, it is target product-epoxy curing agent of the present invention, iron is estimated the colourity that colorimeter records and is only had 2 ~ 3, be applicable to finish paint toning, the viscosity that digital display viscometer records at 25 DEG C only has ~ 800 (cps), is applicable to using with epoxy resin ink and coatings system, is applicable to brushing construction, the cured article (paint film) generated, has good adhesive fastness, mechanical property and chemical resistance with substrate surface.
Claims (1)
1. the synthetic method of a low colourity, low viscous natural phant cardanol solidifying agent of epoxy resin, it is characterized in that with natural phant cardanol, tetraethylene pentamine, paraformaldehyde for raw material, be catalyzer with tea-polyphenol acid, by ternary polycondensation and vacuum hydro-extraction two steps, complete the preparation of target product, be specially on a 1000ml tetra-mouthfuls of glass reaction stills, agitator, widely different flow condenser, direct current condenser, thermometer, nitrogen inlet and charging opening are housed, under the stirring velocity of 80 revs/min, natural phant cardanol is added in molar ratio by charging opening, tetraethylene pentamine, paraformaldehyde, mol ratio is 1.0-1.2: 08-1.0: 0.7-1.0, tea-polyphenol acid series catalysts consumption is the 2-5% of material gross weight, cardanol purity >=99%, tetraethylene pentamine purity >=90%, paraformaldehyde purity >=95%, logical nitrogen deoxygenation in still, widely different flow condenser ice water circulation, 145 ± 1 DEG C are warming up in still, be incubated 1 hour, until the paraformaldehyde pressed powder completely dissolve in still, in still, liquid is muddy shape, represent that ternary polycondensation completes, then, implement vacuum hydro-extraction, close nitrogen inlet, close widely different flow condenser, connect direct current condenser, be not less than under the stirring velocity of 1000 revs/min, connecting vacuum pump and vacuumize, until the vacuum tightness in still reaches-0.098MPa, water flows into measuring container through direct current condenser, when aquifer yield reaches 80% of theoretical aquifer yield, in reactor, turbid solution becomes transparent liquid, terminates vacuum hydro-extraction and obtains product solidified dose.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210042725.8A CN103289059B (en) | 2012-02-24 | 2012-02-24 | Low colourity, low viscosity natural phant cardanol solidifying agent of epoxy resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210042725.8A CN103289059B (en) | 2012-02-24 | 2012-02-24 | Low colourity, low viscosity natural phant cardanol solidifying agent of epoxy resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103289059A CN103289059A (en) | 2013-09-11 |
| CN103289059B true CN103289059B (en) | 2015-12-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210042725.8A Expired - Fee Related CN103289059B (en) | 2012-02-24 | 2012-02-24 | Low colourity, low viscosity natural phant cardanol solidifying agent of epoxy resin |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739828B (en) * | 2013-12-19 | 2015-10-28 | 上海美东生物材料有限公司 | A kind of preparation method of the high-temperature-resistant epoxy resin solidifying agent based on cardanol |
| CN104744407B (en) * | 2014-11-28 | 2016-10-05 | 上海美东生物材料股份有限公司 | A kind of preparation method of low-molecular-weight high epoxy value cardanol epoxy resin |
| CN107365410B (en) * | 2016-05-12 | 2020-11-24 | 常州杰美新高分子科技有限公司 | Resource-saving, efficient and green plant-based catalytic functional material |
| CN106634758B (en) * | 2016-09-23 | 2020-04-10 | 广东省建筑科学研究院集团股份有限公司 | Aging-resistant epoxy adhesive and application thereof |
| CN107488260B (en) * | 2017-07-10 | 2020-11-17 | 中国林业科学研究院林业新技术研究所 | Epoxy resin curing agent based on cardanol and furfural and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333286A (en) * | 2007-06-26 | 2008-12-31 | 上海经天新材料科技有限公司 | Amine epoxy curing agent modified by cardanol |
| CN101508856A (en) * | 2008-02-13 | 2009-08-19 | 上海涂料有限公司上海长风化工厂 | Cashew pnenolic aldehyde amine epoxide resin paint solidifying agent and method for producing the same |
| CN101585906A (en) * | 2008-05-21 | 2009-11-25 | 考格尼斯知识产权管理有限责任公司 | Curing agents for epoxy resins |
| CN101851327A (en) * | 2010-06-02 | 2010-10-06 | 徐州中研科技工业有限公司 | Cashew nut oil modified solid aromatic amine epoxy curing agent |
| CN102134306A (en) * | 2011-03-04 | 2011-07-27 | 广东工业大学 | Cardanol epoxy floor curing agent and preparation method thereof |
| CN102250525A (en) * | 2010-05-18 | 2011-11-23 | 上海市涂料研究所 | Coating used on internal surface of oil pipe for conveying crude oil and petroleum products and preparation method thereof |
-
2012
- 2012-02-24 CN CN201210042725.8A patent/CN103289059B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333286A (en) * | 2007-06-26 | 2008-12-31 | 上海经天新材料科技有限公司 | Amine epoxy curing agent modified by cardanol |
| CN101508856A (en) * | 2008-02-13 | 2009-08-19 | 上海涂料有限公司上海长风化工厂 | Cashew pnenolic aldehyde amine epoxide resin paint solidifying agent and method for producing the same |
| CN101585906A (en) * | 2008-05-21 | 2009-11-25 | 考格尼斯知识产权管理有限责任公司 | Curing agents for epoxy resins |
| CN102250525A (en) * | 2010-05-18 | 2011-11-23 | 上海市涂料研究所 | Coating used on internal surface of oil pipe for conveying crude oil and petroleum products and preparation method thereof |
| CN101851327A (en) * | 2010-06-02 | 2010-10-06 | 徐州中研科技工业有限公司 | Cashew nut oil modified solid aromatic amine epoxy curing agent |
| 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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| CN103289059A (en) | 2013-09-11 |
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Granted publication date: 20151216 Termination date: 20180224 |