CN106279587A - A kind of preparation method of ciclafrine urea formaldehyde - Google Patents
A kind of preparation method of ciclafrine urea formaldehyde Download PDFInfo
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- CN106279587A CN106279587A CN201610700200.7A CN201610700200A CN106279587A CN 106279587 A CN106279587 A CN 106279587A CN 201610700200 A CN201610700200 A CN 201610700200A CN 106279587 A CN106279587 A CN 106279587A
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- ciclafrine
- urea formaldehyde
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
- C08G8/30—Chemically modified polycondensates by unsaturated compounds, e.g. terpenes
Abstract
nullA kind of preparation method of ciclafrine urea formaldehyde，Phenol by 0.1mol molten state、60mL ethanol、8mL NaOH solution is added sequentially in round-bottomed flask，The mixed solvent adding toluene and butanone after reacting 2h under the conditions of water-bath 50 DEG C stirs，Slowly heat up constant to 80 DEG C,The bromo-spiral shell of 10.0mL3-［ 4 is dripped in system,5 ］-three ketenes，Add dibutyl tin laurate，It is cooled to room temperature after being warming up under nitrogen protective condition at 90 DEG C react 4h，Ammonia regulation pH=7.8，Remove liquid under reduced pressure and obtain ciclafrine urea formaldehyde viscous fluid，Add benzyl sodium sulfonate，In vacuum drying oven，With 0.1MPa application of vacuum 2h，Fine and close mixture is poured in the mould of preheating，Precuring 2h，It is placed on 80 DEG C of tablet machine cure under pressure and get final product.Synthesis technique of the present invention is simple, and reaction condition is gentle, and production cost is relatively low, favorable repeatability.
Description
Technical field
The present invention relates to material synthesis method, the preparation method of a kind of ciclafrine urea formaldehyde.
Background technology
Phenolic resin is the polymer synthesized by phenol-based compounds and aldehyde compound polycondensation, due to low in raw material price,
Phenolic resin can get the composite of the different performances such as electrical insulation capability, heat resistance, high burning-point, sound insulation by modification, therefore
It has obtained paying close attention to widely and applying in association areas such as automobile, electronics, building materials.Phenolic hydroxyl group in unmodified phenolic resin
Easily aoxidize with methylene, cause pure phenolic resin impact resistance poor, the most under normal circumstances, need phenolic resin
Modification just can apply in actual production and life to strengthen its toughness.
Spiral shell ［ 4,5 ］ triolefin ketones derivant has stable rigid structure, is widely used in the field of functional material.According to
Report, the substituent group on the C-3 position of halo volution ［ 4,5 ］ three ketenes derivative is passed through further graft reaction, can be obtained
To the material that the intensity of different properties is splendid.Therefore this research is taked to be grafted on the C-3 position of 3-bromo-spiral shell ［ 4,5 ］ three ketenes
The phenolic resin that the degree of polymerization is relatively low, thus generate the phenolic resin material of a kind of spirane structure.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of ciclafrine urea formaldehyde, it is provided that Yi Zhongxin
Synthetic method.
The synthetic method that the present invention uses, comprises the steps:
The phenol of 0.1mol molten state, 60mL ethanol (mass fraction 30%) 8.0mL NaOH solution (mass fraction 5%) are depended on
Secondary join in round-bottomed flask, add after reacting 2h under the conditions of water-bath 50 DEG C toluene and butanone mixed solvent (volume ratio 1:
1.2) 20.0mL stirs, and slowly heats up constant to 80 DEG C, and the dropping bromo-spiral shell of 10.0mL3-［ 4,5 ］ in system-
Three ketenes, instillation speed is 0.5mL/min, and (mass fraction 5%, solvent is to add reaction promoter dibutyl tin laurate
Dichloromethane), it is cooled to room temperature after being warming up under nitrogen protective condition at 90 DEG C react 4h, ammonia regulation pH=7.8, decompression is steamed
Except liquid obtains ciclafrine urea formaldehyde viscous fluid, in ciclafrine urea formaldehyde viscous fluid, add benzyl sodium sulfonate, in vacuum drying
In case, with 0.1MPa application of vacuum 2h, fine and close mixture is poured in the mould of preheating, precuring 2h, it is placed in 80 DEG C of tablettings
On machine, cure under pressure prepares volution class phenolic resin.
The invention has the beneficial effects as follows: synthesis technique is simple, reaction condition is gentle, and production cost is relatively low, favorable repeatability.
Detailed description of the invention
Further illustrating present disclosure below in conjunction with example, as known by the technical knowledge, the present invention also can pass through other
The scheme without departing from the technology of the present invention feature describe, the most all within the scope of the present invention or equivalent the scope of the invention in
Change and be all included in the invention.
Embodiment:
The phenol of 0.1mol molten state, 60mL ethanol (mass fraction 30%) 8.0mL NaOH solution (mass fraction 5%) are depended on
Secondary join in round-bottomed flask, add after reacting 2h under the conditions of water-bath 50 DEG C toluene and butanone mixed solvent (volume ratio 1:
1.2) 20.0mL stirs, and slowly heats up constant to 80 DEG C, and the dropping bromo-spiral shell of 10.0mL3-［ 4,5 ］ in system-
Three ketenes, instillation speed is 0.5mL/min, and (mass fraction 5%, solvent is to add reaction promoter dibutyl tin laurate
Dichloromethane), it is cooled to room temperature after being warming up under nitrogen protective condition at 90 DEG C react 4h, ammonia regulation pH=7.8, decompression is steamed
Except liquid obtains ciclafrine urea formaldehyde viscous fluid, in ciclafrine urea formaldehyde viscous fluid, add benzyl sodium sulfonate, in vacuum drying
In case, with 0.1MPa application of vacuum 2h, fine and close mixture is poured in the mould of 120 DEG C and solidify 2h, be placed in 80 DEG C of tablet machine
Upper cure under pressure prepares volution class phenolic resin.
Volution phenolic resin material being carried out performance test, obtains its heat resistance the most excellent, electrical insulation capability is obvious
It is better than the electrical insulation capability of unmodified phenolic resin material, and the sound in the range of certain frequency is had the most excellent sound insulation
Effect.In sum, the volution phenolic resin material that prepared by the present invention is that one has one in terms of heat-resisting, electric insulation, sound insulation
Determining the material modified of effectiveness function, because of the multiformity of its function, volution phenolic resin material application prospect commercially is by ten
Divide wide.
Claims (1)
1. a preparation method for ciclafrine urea formaldehyde, comprises the steps:
The phenol of 0.1mol molten state, 60mL ethanol (mass fraction 30%) 8.0mL NaOH solution (mass fraction 5%) are depended on
Secondary join in round-bottomed flask, add after reacting 2h under the conditions of water-bath 50 DEG C toluene and butanone mixed solvent (volume ratio 1:
1.2) 20.0mL stirs, and slowly heats up constant to 80 DEG C, and the dropping bromo-spiral shell of 10.0mL3-［ 4,5 ］ in system-
Three ketenes, instillation speed is 0.5mL/min, and (mass fraction 5%, solvent is to add reaction promoter dibutyl tin laurate
Dichloromethane), it is cooled to room temperature after being warming up under nitrogen protective condition at 90 DEG C react 4h, ammonia regulation pH=7.8, decompression is steamed
Except liquid obtains ciclafrine urea formaldehyde viscous fluid, in ciclafrine urea formaldehyde viscous fluid, add benzyl sodium sulfonate, in vacuum drying
In case, with 0.1MPa application of vacuum 2h, fine and close mixture is poured in the mould of preheating, precuring 2h, it is placed in 80 DEG C of tablettings
On machine, cure under pressure prepares volution class phenolic resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610700200.7A CN106279587A (en) | 2016-08-22 | 2016-08-22 | A kind of preparation method of ciclafrine urea formaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610700200.7A CN106279587A (en) | 2016-08-22 | 2016-08-22 | A kind of preparation method of ciclafrine urea formaldehyde |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106279587A true CN106279587A (en) | 2017-01-04 |
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ID=57660968
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610700200.7A Pending CN106279587A (en) | 2016-08-22 | 2016-08-22 | A kind of preparation method of ciclafrine urea formaldehyde |
Country Status (1)
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| CN (1) | CN106279587A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112210058A (en) * | 2020-10-14 | 2021-01-12 | 中国科学院长春应用化学研究所 | Phenolic resin material, preparation method thereof and high-flux gas separation membrane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4120847A (en) * | 1976-01-09 | 1978-10-17 | Monsanto Company | High ortho etherified resole resins |
| CN104788360A (en) * | 2015-03-30 | 2015-07-22 | 王桦 | 3-sulfuryl spirobacillene and preparation method thereof |
-
2016
- 2016-08-22 CN CN201610700200.7A patent/CN106279587A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4120847A (en) * | 1976-01-09 | 1978-10-17 | Monsanto Company | High ortho etherified resole resins |
| CN104788360A (en) * | 2015-03-30 | 2015-07-22 | 王桦 | 3-sulfuryl spirobacillene and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘超等: ""一种新型螺环酚醛树脂的制备及性能研究"", 《化工新型材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112210058A (en) * | 2020-10-14 | 2021-01-12 | 中国科学院长春应用化学研究所 | Phenolic resin material, preparation method thereof and high-flux gas separation membrane |
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Application publication date: 20170104 |