CN104327250A - Preparation method of alicyclic resin 4221 (ERL-4221) - Google Patents
Preparation method of alicyclic resin 4221 (ERL-4221) Download PDFInfo
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- CN104327250A CN104327250A CN201410503717.8A CN201410503717A CN104327250A CN 104327250 A CN104327250 A CN 104327250A CN 201410503717 A CN201410503717 A CN 201410503717A CN 104327250 A CN104327250 A CN 104327250A
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- tetrahydrobenzene
- epoxy resin
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- trichloromethane
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Abstract
The invention discloses a preparation method of alicyclic resin 4221 (ERL-4221). The preparation method is low in processing cost. The alicyclic resin 4221 (ERL-4221) is prepared with trichloromethane as a solvent and hydrogen peroxide and CMCC as main raw materials and through a reaction with a catalyst. The preparation method is simple in processes, is less in equipment investment and is free of safety potential risk generated by enrichment of peroxides. The alicyclic resin 4221 is wide in application, can be applied in an optical adhesive and a photocuring product, electrical pouring and electronic encapsulation of outdoor electronic and electric products, and outdoor coatings and solvent-free coatings. The alicyclic resin 4221 is better than an acrylic acid-polyethane coating and an epoxy resin active diluent in weather-resistance. The alicyclic resin 4221 can be applied in the fields of electronic and electric products, civil constructions and anticorrosive coatings of general bisphenol A epoxy resin and the fields of oil additives and the like, wherein the oil additives includes lubricant oils, cylinder oils and transformer oils.
Description
Technical field
the present invention relates generally to a kind of preparation method of resin, especially designs a kind of alicyclic ring resin 4221(ERL-4221) preparation method.
Background technology
alicyclic ring resin 4221 has another name called 3,4-expoxycyclohexyl formic acid-3 ‵, 4 ‵-expoxycyclohexyl methyl esters, industrial trade mark ERL-4221.Colourless or light yellow transparent liquid is a kind of important meticulous organic intermediate.
Alicyclic ring resin 4221(ERL-4221) be a kind of novel cycloaliphatic products, its chemistry 3,4-epoxyhexyl formic acid-3 by name ', 4 '-epoxycyclohexyl formicester.Unsaturated double-bond is not had in its molecular structure, compared with other type of epoxy resin system, and tool viscosity is very low, reactive behavior is high, cured article physical and mechanical properties is good, cohesive strength is large, and the features such as weathering resistance, voltage ageing excellent property answer scope extremely extensive: can be applicable to optical adhesive and photocuring product, the electrician's cast being applied to outdoor electronic electrical apparatus product and electronics embedding, be applied to outdoor coating and solventless coatings; Excellent weather resistance and hard in acrylic acid-polyurethane coating, be applied to epoxide resin reactive dilution, be applied to the Application Areas of the universal bisphenol A epoxide resins such as electronic apparatus, civil construction, protective system, be applied to the stability of polyvinyl chloride, polycarbonate, the fields such as oil product (lubricating oil, cylinder stock oil, transformer oil) additive.
Summary of the invention
The object of the invention is just to provide a kind of alicyclic ring resin 4221(ERL-4221) preparation method.
The present invention is achieved by the following technical solutions:
A preparation method of aliphatic epoxy resin ERL-4221, comprises the following steps:
Trichloromethane is pumped in reactor, drop into catalyzer hexadecylpyridinium chloride, potassium primary phosphate, stir 18-22min, be warming up to 30-50 DEG C, temperature control is in 30-50 DEG C, by in 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters instillation reactor, drip and finish, slowly drip hydrogen peroxide again, drip and finish, stir, temperature control 30-50 DEG C, synthesis under normal pressure 18-19h, after reaction terminates, be down to room temperature, leave standstill 8-10min, layering, organic layer is proceeded in all turn troughs, after question response still water discharges, organic layer is pushed back reactor, add tap water and stir 4-6min, leave standstill 8-10min layering, organic layer is proceeded in concentration kettle, combining water layer is to wastewater treatment place, it is 100 DEG C in temperature, concentration and recovery trichloromethane is started to trichloromethane accumulator tank under condition of normal pressure, obtain aliphatic epoxy resin ERL-4221 work in-process, the work in-process obtained are put in rectifying still, rectifying is carried out at-0.08Mpa, 100-150 DEG C, foreshot is 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters, collect, when the content of aliphatic epoxy resin ERL-4221 reaches 99%, start extraction finished product, then finished product is proceeded in mixture still to be packaged.
A preparation method of aliphatic epoxy resin ERL-4221, the mass ratio of described trichloromethane, hexadecylpyridinium chloride, potassium primary phosphate, 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters, hydrogen peroxide, tap water is 3-3.1:0.008-0.01:0.004:0.98-1:0.96-1:1.
Advantage of the present invention is:
Preparation method's processing cost of the present invention is low, and adopt trichloromethane as solvent, hydrogen peroxide, CMCC are main raw material, generate through catalyst reaction.The feature of this method is that technique is simple, and facility investment is few, and there is not the potential safety hazard of superoxide enrichment generation.Finished product is widely used, and can be applicable to optical adhesive and photocuring product, electrician's cast of outdoor electronic electrical apparatus product and electronics embedding, outdoor coating and solventless coatings; Excellent weather resistance and hard is in the field such as Application Areas, oil product (lubricating oil, cylinder stock oil, transformer oil) additive of the universal bisphenol A epoxide resin such as acrylic acid-polyurethane coating, epoxide resin reactive diluent, electronic apparatus, civil construction, protective system.
Embodiment
Embodiment 1
A preparation method of aliphatic epoxy resin ERL-4221, comprises the following steps:
Trichloromethane is pumped in reactor, drop into catalyzer hexadecylpyridinium chloride, potassium primary phosphate, stir 18-22min, be warming up to 30-50 DEG C, temperature control is in 30-50 DEG C, by in 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters instillation reactor, drip and finish, slowly drip hydrogen peroxide again, drip and finish, stir, temperature control 30-50 DEG C, synthesis under normal pressure 18-19h, after reaction terminates, be down to room temperature, leave standstill 8-10min, layering, organic layer is proceeded in all turn troughs, after question response still water discharges, organic layer is pushed back reactor, add tap water and stir 4-6min, leave standstill 8-10min layering, organic layer is proceeded in concentration kettle, combining water layer is to wastewater treatment place, it is 100 DEG C in temperature, concentration and recovery trichloromethane is started to trichloromethane accumulator tank under condition of normal pressure, obtain aliphatic epoxy resin ERL-4221 work in-process, the work in-process obtained are put in rectifying still, rectifying is carried out at-0.08Mpa, 100-150 DEG C, foreshot is 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters, collect, when the content of aliphatic epoxy resin ERL-4221 reaches 99%, start extraction finished product, then finished product is proceeded in mixture still to be packaged.Kettle base solution is high boiling point refuse, collects and transfers to useless processed in units of endangering.
A preparation method of aliphatic epoxy resin ERL-4221, the mass ratio of described trichloromethane, hexadecylpyridinium chloride, potassium primary phosphate, 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters, hydrogen peroxide, tap water is 3:0.008:0.004:1:1:1.
Use method of the present invention, the yield of aliphatic epoxy resin ERL-4221 is 97%.
Performance test:
Viscosity (25 DEG C): 200-450cp
Epoxy equivalent (weight) 128-145 g/mol
Solvability: water insoluble.
Claims (2)
1. a preparation method of aliphatic epoxy resin ERL-4221, is characterized in that comprising the following steps:
Trichloromethane is pumped in reactor, drop into catalyzer hexadecylpyridinium chloride, potassium primary phosphate, stir 18-22min, be warming up to 30-50 DEG C, temperature control is in 30-50 DEG C, by in 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters instillation reactor, drip and finish, slowly drip hydrogen peroxide again, drip and finish, stir, temperature control 30-50 DEG C, synthesis under normal pressure 18-19h, after reaction terminates, be down to room temperature, leave standstill 8-10min, layering, organic layer is proceeded in all turn troughs, after question response still water discharges, organic layer is pushed back reactor, add tap water and stir 4-6min, leave standstill 8-10min layering, organic layer is proceeded in concentration kettle, combining water layer is to wastewater treatment place, it is 100 DEG C in temperature, concentration and recovery trichloromethane is started to trichloromethane accumulator tank under condition of normal pressure, obtain aliphatic epoxy resin ERL-4221 work in-process, the work in-process obtained are put in rectifying still, rectifying is carried out at-0.08Mpa, 100-150 DEG C, foreshot is 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters, collect, when the content of aliphatic epoxy resin ERL-4221 reaches 99%, start extraction finished product, then finished product is proceeded in mixture still to be packaged.
2. the preparation method of a kind of aliphatic epoxy resin ERL-4221 according to claim 1, is characterized in that the mass ratio of described trichloromethane, hexadecylpyridinium chloride, potassium primary phosphate, 3-tetrahydrobenzene-1-formic acid 3-tetrahydrobenzene methyl esters, hydrogen peroxide, tap water is 3-3.1:0.008-0.01:0.004:0.98-1:0.96-1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410503717.8A CN104327250A (en) | 2014-09-27 | 2014-09-27 | Preparation method of alicyclic resin 4221 (ERL-4221) |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410503717.8A CN104327250A (en) | 2014-09-27 | 2014-09-27 | Preparation method of alicyclic resin 4221 (ERL-4221) |
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| CN104327250A true CN104327250A (en) | 2015-02-04 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01165542A (en) * | 1987-12-23 | 1989-06-29 | Mitsubishi Petrochem Co Ltd | Production of carboxylic acids |
| CN101143919A (en) * | 2007-09-05 | 2008-03-19 | 中国科学院大连化学物理研究所 | Method for synthesizing alicyclic epoxy resin by catalyzing unsaturated alicyclic compound |
| CN101250169A (en) * | 2008-04-08 | 2008-08-27 | 大连天源基化学有限公司 | Method for synthesizing aliphatic diepoxides |
| CN101671318A (en) * | 2008-09-10 | 2010-03-17 | 山东鲁抗立科药物化学有限公司 | Cycloaliphatic epoxy resin and preparation method thereof |
-
2014
- 2014-09-27 CN CN201410503717.8A patent/CN104327250A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01165542A (en) * | 1987-12-23 | 1989-06-29 | Mitsubishi Petrochem Co Ltd | Production of carboxylic acids |
| CN101143919A (en) * | 2007-09-05 | 2008-03-19 | 中国科学院大连化学物理研究所 | Method for synthesizing alicyclic epoxy resin by catalyzing unsaturated alicyclic compound |
| CN101250169A (en) * | 2008-04-08 | 2008-08-27 | 大连天源基化学有限公司 | Method for synthesizing aliphatic diepoxides |
| CN101671318A (en) * | 2008-09-10 | 2010-03-17 | 山东鲁抗立科药物化学有限公司 | Cycloaliphatic epoxy resin and preparation method thereof |
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Application publication date: 20150204 |
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