CN101676248A - Methods for synthesizing hydroxy benzaldehyde - Google Patents
Methods for synthesizing hydroxy benzaldehyde Download PDFInfo
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- CN101676248A CN101676248A CN200810157172A CN200810157172A CN101676248A CN 101676248 A CN101676248 A CN 101676248A CN 200810157172 A CN200810157172 A CN 200810157172A CN 200810157172 A CN200810157172 A CN 200810157172A CN 101676248 A CN101676248 A CN 101676248A
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- China
- Prior art keywords
- hydroxy benzaldehyde
- reaction
- bubble
- iodine
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for synthesizing hydroxy benzaldehyde, namely a reaction method of TFE, I2 and IF5, which has the advantages of short process, simple operation, high purity and yield,less threewastes and the like and is a more mature synthesis method. The synthesis method can be used by most factories and is continuously improved on technology.
Description
Technical field
The present invention relates to a kind of making method of hydroxy benzaldehyde.
Technical background
Hydroxy benzaldehyde has another name called perfluoro ethyl iodide, molecular formula C
2F
5I, molecular weight 246,12.5 ℃ of boiling points are colourless gas under the room temperature.See that light easily decomposes, iodine dissociates.Hydroxy benzaldehyde can be used for preparing five fluorine monochlorethanes.Hydroxy benzaldehyde is mixed with excessive chlorine, be enclosed in the reaction tubes, use the UV-light Continuous irradiation.Product is washed with aqueous sodium hydroxide washes, obtains the C2ClF5 product after the vacuum separation.Hydroxy benzaldehyde also is the important source material of synthesizing perfluoroalkyl iodide, is mainly used in the initial telogen of producing perfluoroalkyl iodides, also can be used for producing fluorine-containing fine chemicals such as fluorine-containing medicines intermediate.The fluorine surfactant of producing with hydroxy benzaldehyde derived product full-fluorine alkyl iodide, fluorine finishing composition etc., kind is a lot, uses very wide.Along with the increasing of industrialization, raw-material pulling function is strengthened day by day.Therefore the research of hydroxy benzaldehyde synthetic method has certain realistic meaning.
Summary of the invention
The making method that the objective of the invention is hydroxy benzaldehyde.
Technical scheme of the present invention is: iodine is dissolved in the iodine pentafluoride, send into to gained solution continuity upright bubble-column reactor, bubble-plate column is equipped with iodine pentafluoride, in its bottom the tetrafluoroethylene feed-pipe is arranged, temperature of reaction is controlled at 85～95 ℃, the hydroxy benzaldehyde that generates is discharged by the bubble-plate column top with gas form, and liquefying in the condenser in downstream is stored in the container.Its optimal reaction temperature is controlled at 90 ℃.
Embodiment
In autoclave, adopt intermittent reaction.Iodine adds with iodine pentafluoride or introduces with the form of hot tetrafluoroethylene steam carrier band.Control certain temperature and pressure, when reaction pressure no longer descended, reaction finished.Product is through gasification, condensation is collected, iodine is dissolved in the iodine pentafluoride, send into to gained solution continuity upright bubble-column reactor, bubble-plate column is equipped with iodine pentafluoride, in its bottom the tetrafluoroethylene feed-pipe is arranged, and temperature of reaction is controlled at 85～95 ℃, the hydroxy benzaldehyde that generates is discharged by the bubble-plate column top with gas form, and liquefying in the condenser in downstream is stored in the container.Its optimal reaction temperature is controlled at 90 ℃.
With IF
5In the technology for fluorizating agent, the difficult control of the quality of iodine pentafluoride, this directly has influence on the yield of hydroxy benzaldehyde.Guaranteed the stability of technology from raw material.As the 48gICI that packs in shaking bottle, pressurization is cooled to-30 ℃, adds 100g anhydrous HF, 10gBF 3 (catalyzer) and 30g tetrafluoroethylene then, shakes reactor 18h in 20 ℃, obtains hydroxy benzaldehyde.
With pentafluoride ethane (C
2F
5I) and 12 mixed gass of forming, the basic metal of flowing through (alkaline earth salt/carrier) catalyst layer reacts under its catalysis, obtains C
2F
5I, C
2F
3I, C
2F
5H, 12 gaseous mixtures.Can obtain desired product C through the multistep separation
2F
5I and C
2F
3I.Can realize target product C by changing reaction conditions (as catalyst property, temperature of reaction and the residence time etc.)
2F
5I and C
2F
3The adjusting of I proportion of composing.As cyclic part reaction mixture selectively, can make C
2F
5H and 12 reactions are to C
2F
5I or C
2F
3The generation direction of I is carried out, so C
2F
5The selectivity of I can reach 45%.This reacts C
2F
5H and 12 mixed gas feeding temperatures are controlled at 150～160 ℃, and catalyzer is the KF/ gac, reaction pressure: 0.1MPa.
Claims (2)
1, a kind of synthetic method of hydroxy benzaldehyde, it is characterized in that: iodine is dissolved in the iodine pentafluoride, send into to gained solution continuity upright bubble-column reactor, bubble-plate column is equipped with iodine pentafluoride, in its bottom the tetrafluoroethylene feed-pipe is arranged, temperature of reaction is controlled at 85～95 ℃, and the hydroxy benzaldehyde of generation is discharged by the bubble-plate column top with gas form, and liquefying in the condenser in downstream is stored in the container.
2, the synthetic method of a kind of hydroxy benzaldehyde according to claim 1 is characterized in that: temperature of reaction is controlled at 90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810157172A CN101676248A (en) | 2008-09-19 | 2008-09-19 | Methods for synthesizing hydroxy benzaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810157172A CN101676248A (en) | 2008-09-19 | 2008-09-19 | Methods for synthesizing hydroxy benzaldehyde |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101676248A true CN101676248A (en) | 2010-03-24 |
Family
ID=42028984
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810157172A Pending CN101676248A (en) | 2008-09-19 | 2008-09-19 | Methods for synthesizing hydroxy benzaldehyde |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101676248A (en) |
-
2008
- 2008-09-19 CN CN200810157172A patent/CN101676248A/en active Pending
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100324 |