CN107163019A - A kind of rectificating method of piperonal - Google Patents
A kind of rectificating method of piperonal Download PDFInfo
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- CN107163019A CN107163019A CN201710530236.XA CN201710530236A CN107163019A CN 107163019 A CN107163019 A CN 107163019A CN 201710530236 A CN201710530236 A CN 201710530236A CN 107163019 A CN107163019 A CN 107163019A
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- piperonal
- product
- vacuum
- rectifying
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/44—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D317/46—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 ortho- or peri-condensed with carbocyclic rings or ring systems condensed with one six-membered ring
- C07D317/48—Methylenedioxybenzenes or hydrogenated methylenedioxybenzenes, unsubstituted on the hetero ring
- C07D317/50—Methylenedioxybenzenes or hydrogenated methylenedioxybenzenes, unsubstituted on the hetero ring with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to atoms of the carbocyclic ring
- C07D317/54—Radicals substituted by oxygen atoms
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- Organic Chemistry (AREA)
- Hydrogenated Pyridines (AREA)
Abstract
The present invention relates to a kind of rectificating method of piperonal, concretely comprise the following steps：500g piperonals crude product (wherein raw material piperonyl cyclonene contains 10%) is added in 1000ml single-necked flasks, 200ml atent solvents connect 10cm rectifying columns, fractionating device, receiving flask；Vacuum is opened, survey vacuum is 30Pa, starts to warm up, infinite reflux is carried out during beginning, infinite reflux half an hour starts to receive front-end volatiles, and front-end volatiles receive temperature for 100 150 DEG C, higher than 150 DEG C, it is product piperonal less than 180 DEG C, obtains piperonal rectifying product 445g, content is higher than 98%.The addition of atent solvent, layer protective layer is formd on piperonal surface, has been completely cut off oxidation and polymerisation of the trace oxygen to piperonal, has been served a kind of protective effect, while also reducing the danger of blast, improve rectification yield.
Description
Technical field
The present invention relates to a kind of rectificating method of piperonal, belong to field of medicine and chemical technology.
Background technology
Piperonal, also known as heliotropin, are widely used in all kinds of daily cosmetics essence, flavoring essence, and in doctor
The industries such as medicine, agricultural chemicals, plating are also widely used.
Due to the easily oxidizable of aldehyde in the distillation process of piperonal, due to the liter of temperature in the distillation process of piperonal
Height, micro oxygen can promote piperonal oxidation polymerization, in some instances it may even be possible to can occur explosion danger.In the preparation text of current piperonal
There is no the document report of this respect in offering.
The content of the invention
It is an object of the invention to provide a kind of rectificating method of piperonal, the side of piperonal and air exclusion is made during rectifying
Method, it is to avoid pepper is oxidation of aldehydes, polymerization.
To achieve the above object, the technical scheme is that：
A kind of rectificating method of piperonal, is concretely comprised the following steps：
500g piperonals crude product (wherein raw material piperonyl cyclonene contains 10%) is added in 1000ml single-necked flasks, 200ml inertia is molten
Agent, connects 10cm rectifying columns, fractionating device, receiving flask；
Vacuum is opened, survey vacuum is 30Pa, starts to warm up, infinite reflux is carried out during beginning, infinite reflux half an hour starts to connect
By front-end volatiles, front-end volatiles receive temperature for 100-150 DEG C, higher than 150 DEG C, are product piperonal less than 180 DEG C, obtain piperonal essence
Product 445g is evaporated, content is higher than 98%.
Described atent solvent is the combination of one or both of white oil, atoleine.
To prevent oxidation and polymerization of the trace oxygen to piperonal, the surface of piperonal is compared plus proportion in rectifying still
Light higher boiling atent solvent white oil, atoleine or other atent solvents, preferably white oil, due to the addition of atent solvent,
Piperonal surface forms layer protective layer, has completely cut off oxidation and polymerisation of the trace oxygen to piperonal, has served one kind
Protective effect, while also reducing the danger of blast, improves rectification yield, rectification yield is can reach 98%, be suitable for work
Industry is produced.
Embodiment
Following embodiment, is merely illustrative of, and is not only, so, all within the scope of the present invention or make with
The similar change of the present invention is both contained within the present invention.
Embodiment 1：
A kind of rectificating method of piperonal, is concretely comprised the following steps：
500g piperonals crude product (wherein raw material piperonyl cyclonene contains 10%) is added in 1000ml single-necked flasks, 200ml white oils connect
10cm rectifying columns, fractionating device, receiving flask；
Vacuum is opened, survey vacuum is 30Pa, starts to warm up, infinite reflux is carried out during beginning, infinite reflux half an hour starts to connect
By front-end volatiles, front-end volatiles receive temperature for 100-150 DEG C, higher than 150 DEG C, are product piperonal less than 180 DEG C, obtain piperonal essence
Product 445g is evaporated, content is higher than 98%.
Distillation operation is carried out using high vacuum system, vacuum is≤30PA.
Heated up using conduction oil, oil temperature is up to 250 DEG C.
Rectifying collecting temperature is 100-180 DEG C, and front-end volatiles collecting temperature is≤150 DEG C, and principal component collecting temperature is 150-
180℃。
Claims (2)
1. a kind of rectificating method of piperonal, is concretely comprised the following steps：
500g piperonals crude product (wherein raw material piperonyl cyclonene contains 10%) is added in 1000ml single-necked flasks, 200ml atent solvents connect
10cm rectifying columns, fractionating device, receiving flask；
Vacuum is opened, survey vacuum is 30Pa, starts to warm up, infinite reflux is carried out during beginning, infinite reflux half an hour starts before receiving
Cut, front-end volatiles receive temperature for 100-150 DEG C, higher than 150 DEG C, are product piperonal less than 180 DEG C, obtain piperonal rectifying production
Product 445g, content is higher than 98%.
2. a kind of rectificating method of piperonal according to claim 1, it is characterised in that：Described atent solvent is white
The combination of one or both of oil, atoleine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710530236.XA CN107163019A (en) | 2017-06-24 | 2017-06-24 | A kind of rectificating method of piperonal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710530236.XA CN107163019A (en) | 2017-06-24 | 2017-06-24 | A kind of rectificating method of piperonal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107163019A true CN107163019A (en) | 2017-09-15 |
Family
ID=59826948
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710530236.XA Pending CN107163019A (en) | 2017-06-24 | 2017-06-24 | A kind of rectificating method of piperonal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107163019A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110590732A (en) * | 2019-09-26 | 2019-12-20 | 河北海力香料股份有限公司 | Preparation method of piper nigrum rings |
| CN112979444A (en) * | 2021-03-01 | 2021-06-18 | 黑龙江省科学院石油化学研究院 | Refining method and rectifying device of 2-hydroxy-1-naphthaldehyde |
| CN114477666A (en) * | 2022-04-19 | 2022-05-13 | 河北海力香料股份有限公司 | Treatment method of piperonal production wastewater |
-
2017
- 2017-06-24 CN CN201710530236.XA patent/CN107163019A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110590732A (en) * | 2019-09-26 | 2019-12-20 | 河北海力香料股份有限公司 | Preparation method of piper nigrum rings |
| CN112979444A (en) * | 2021-03-01 | 2021-06-18 | 黑龙江省科学院石油化学研究院 | Refining method and rectifying device of 2-hydroxy-1-naphthaldehyde |
| CN114477666A (en) * | 2022-04-19 | 2022-05-13 | 河北海力香料股份有限公司 | Treatment method of piperonal production wastewater |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170915 |
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| WD01 | Invention patent application deemed withdrawn after publication |